Science.gov

Sample records for chemical spray pyrolysis

  1. Fabrication of ZnO nanorod using spray-pyrolysis and chemical bath deposition method

    SciTech Connect

    Ramadhani, Muhammad F. Pasaribu, Maruli A. H. Yuliarto, Brian Nugraha

    2014-02-24

    ZnO thin films with nanorod structure were deposited using Ultrasonic Spray Pyrolysis method for seed growth, and Chemical Bath Deposition (CBD) for nanorod growth. High purity Zn-hydrate and Urea are used to control Ph were dissolved in ethanol and aqua bidest in Ultrasonic Spray Pyrolysis process. Glass substrate was placed above the heater plate of reaction chamber, and subsequently sprayed with the range duration of 5, 10 and 20 minutes at the temperatures of 3500 C. As for the Chemical Bath Deposition, the glass substrate with ZnO seed on the surface was immerse to Zn-hydrate, HMTA (Hexa Methylene Tetra Amine) and deionized water solution for duration of 3, 5 and 7 hour and temperatures of 600 C, washed in distilled water, dried, and annealed at 3500 C for an hour. The characterization of samples was carried out to reveal the surface morphology using Scanning Electron Microscopy (SEM). From the data, the combination of 5 minutes of Ultrasonic Spray Pyrolysis process and 3 hour of CBD has showed the best structure of nanorod. Meanwhile the longer Spraying process and CBD yield the bigger nanorod structure that have been made, and it makes the films more dense which make the nanorod collide each other and as a result produce unsymetric nanorod structure.

  2. Nonlinear optical characterization of ZnS thin film synthesized by chemical spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    G, Sreeja V.; V, Sabitha P.; Anila, E. I.; R, Reshmi; John, Manu Punnan; Radhakrishnan, P.

    2014-10-01

    ZnS thin film was prepared by Chemical Spray Pyrolysis (CSP) method. The sample was characterized by X-ray diffraction method and Z scan technique. XRD pattern showed that ZnS thin film has hexagonal structure with an average size of about 5.6nm. The nonlinear optical properties of ZnS thin film was studied by open aperture Z-Scan technique using Q-switched Nd-Yag Laser at 532nm. The Z-scan plot showed that the investigated ZnS thin film has saturable absorption behavior. The nonlinear absorption coefficient and saturation intensity were also estimated.

  3. Nonlinear optical characterization of ZnS thin film synthesized by chemical spray pyrolysis method

    SciTech Connect

    G, Sreeja V; Anila, E. I. R, Reshmi John, Manu Punnan; V, Sabitha P; Radhakrishnan, P.

    2014-10-15

    ZnS thin film was prepared by Chemical Spray Pyrolysis (CSP) method. The sample was characterized by X-ray diffraction method and Z scan technique. XRD pattern showed that ZnS thin film has hexagonal structure with an average size of about 5.6nm. The nonlinear optical properties of ZnS thin film was studied by open aperture Z-Scan technique using Q-switched Nd-Yag Laser at 532nm. The Z-scan plot showed that the investigated ZnS thin film has saturable absorption behavior. The nonlinear absorption coefficient and saturation intensity were also estimated.

  4. Low-cost plasmonic solar cells prepared by chemical spray pyrolysis

    PubMed Central

    Katerski, Atanas; Oja Acik, Ilona; Mikli, Valdek; Mere, Arvo; Sildos, Ilmo; Krunks, Malle

    2014-01-01

    Summary Solar cells consisting of an extremely thin In2S3/CuInS2 buffer/absorber layer uniformly covering planar ZnO were prepared entirely by chemical spray pyrolysis. Au nanoparticles (Au-NPs) were formed via thermal decomposition of a gold(III) chloride trihydrate (HAuCl4·3H2O) precursor by spraying 2 mmol/L of the aqueous precursor solution onto a substrate held at 260 °C. Current–voltage scans and external quantum efficiency spectra were used to evaluate the solar cell performance. This work investigates the effect of the location of the Au-NP layer deposition (front side vs rear side) in the solar cell and the effect of varying the volume (2.5–10 mL) of the sprayed Au precursor solution. A 63% increase (from 4.6 to 7.5 mA/cm2) of the short-circuit current density was observed when 2.5 mL of the precursor solution was deposited onto the rear side of the solar cell. PMID:25551068

  5. Low-cost plasmonic solar cells prepared by chemical spray pyrolysis.

    PubMed

    Kärber, Erki; Katerski, Atanas; Oja Acik, Ilona; Mikli, Valdek; Mere, Arvo; Sildos, Ilmo; Krunks, Malle

    2014-01-01

    Solar cells consisting of an extremely thin In2S3/CuInS2 buffer/absorber layer uniformly covering planar ZnO were prepared entirely by chemical spray pyrolysis. Au nanoparticles (Au-NPs) were formed via thermal decomposition of a gold(III) chloride trihydrate (HAuCl4·3H2O) precursor by spraying 2 mmol/L of the aqueous precursor solution onto a substrate held at 260 °C. Current-voltage scans and external quantum efficiency spectra were used to evaluate the solar cell performance. This work investigates the effect of the location of the Au-NP layer deposition (front side vs rear side) in the solar cell and the effect of varying the volume (2.5-10 mL) of the sprayed Au precursor solution. A 63% increase (from 4.6 to 7.5 mA/cm(2)) of the short-circuit current density was observed when 2.5 mL of the precursor solution was deposited onto the rear side of the solar cell.

  6. Chemical spray pyrolysis of copper indium diselenide/cadmium sulfide solar cells

    SciTech Connect

    Brown, B.J.

    1989-01-01

    This dissertation concentrates on Chemical Spray Pyrolysis (CSP) of CuInSe{sub 2} and CdS thin films and solar cells. The primary goal is to gain an understanding of the chemistry and physics of CSP, and apply this knowledge to the fabrication of CuInSe{sub 2}/CdS solar cells. It provide an extensive review of the literature on the properties of CuInSe{sub 2} an CdS produced by CSP and other techniques. The films are characterized by x-ray diffractometry, scanning electron microscopy, electron microprobe, van der Pauw-Hall measurements, and optical absorption spectroscopy, and the devices are characterized electrically in the dark and under illumination. A model for the chemical mechanisms involved in CSP of CdS an CuInSe{sub 2} thin films is developed which is used to point out similarities between the two systems and explain the correlation between spray solution pH and second phases in CuInSe{sub 2} thin films. Structural investigations show that the CuInSe{sub 2} films can be produced in either the ordered or disordered crystal structure, while different substrates radically change the morphology of the films. By taking into account the effect of second phases, the electrical and optical properties of the sprayed films agree with published results for CuInSe{sub 2} produced by other techniques. The properties of the sprayed CdS films in this work are shown to agree with those sprayed by others. The device properties of cells fabricated in both the backwall and reverse backwall configuration are compared with each other and related to the materials properties of the semiconductor layers. The highest efficiency cell employing sprayed CuInSe{sub 2} is reported; however, the efficiency of the cells still need improvement before becoming practical. The dissertation concludes with recommendations for increasing the efficiency of completely sprayed CuInSe{sub 2}/CdS solar cells.

  7. Chemical spray pyrolysis of β-In2S3 thin films deposited at different temperatures

    NASA Astrophysics Data System (ADS)

    Sall, Thierno; Marí Soucase, Bernabé; Mollar, Miguel; Hartitti, Bouchaib; Fahoume, Mounir

    2015-01-01

    In2S3 thin films were deposited onto indium tin oxide-coated glass substrates by chemical spray pyrolysis while keeping the substrates at different temperatures. The structures of the sprayed In2S3 thin films were characterized by X-ray diffraction (XFD). The quality of the thin films was determined by Raman spectroscopy. Scanning electron microscopy (SEM) and atomic force microscopy were used to explore the surface morphology and topography of the thin films, respectively. The optical band gap was determined based on optical transmission measurements. The indium sulfide phase exhibited a preferential orientation in the (0, 0, 12) crystallographic direction according to the XRD analysis. The phonon vibration modes determined by Raman spectroscopy also confirmed the presence of the In2S3 phase in our samples. According to SEM, the surface morphologies of the films were free of defects. The optical band gap energy varied from 2.82 eV to 2.95 eV.

  8. Investigation of discharged aerosol nanoparticles during chemical precipitation and spray pyrolysis for developing safety measures in the nano research laboratory.

    PubMed

    Kolesnikov, Еvgeny; Karunakaran, Gopalu; Godymchuk, Anna; Vera, Levina; Yudin, Andrey Grigorjevich; Gusev, Alexander; Kuznetsov, Denis

    2017-05-01

    Nowadays, the demands for the nanoparticles are increasing due to their tremendous applications in various fields. As a consequence, the discharge of nanoparticles into the atmosphere and environment is also increasing, posing a health threat and environmental damage in terms of pollution. Thus, an extensive research is essential to evaluate the discharge of these nanoparticles into the environment. Keeping this in mind, the present investigation aimed to analyze the discharge of aerosol nanoparticles that are synthesized in the laboratory via chemical precipitation and spray pyrolysis methods. The results indicated that the chemical precipitation method discharges a higher concentration of nanoparticles in the work site when compared to the spray pyrolysis method. The aerosol concentration also varied with the different steps involved during the synthesis of nanoparticles. The average particle's concentration in air for chemical precipitation and spray pyrolysis methods was around 1,037,476 and 883,421particles/cm(3). In addition, the average total discharge of nanoparticles in the entire laboratory was also examined. A significant variation in the concentration of nanoparticles was noticed, during the processing of materials and the concentration of particles (14-723nm) exceeding the daily allowed concentration to about 70-170 times was observed over a period of 6 months. Thus, the results of the present study will be very useful in developing safety measures and would help in organizing the rules for people working in nanotechnology laboratories to minimize the hazardous effects. Copyright © 2017 Elsevier Inc. All rights reserved.

  9. Zirconium doped TiO2 thin films deposited by chemical spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Juma, A.; Oja Acik, I.; Oluwabi, A. T.; Mere, A.; Mikli, V.; Danilson, M.; Krunks, M.

    2016-11-01

    Chemical spray pyrolysis (CSP) is a flexible deposition technique that allows for mixing of the precursor solutions in different proportions suitable for doping thin films. The CSP method was used to dope TiO2 thin films with Zr by adding zirconium(IV) acetylacetonate into a solution of titanium(IV) isopropoxide in ethanol stabilized by acetylacetone at [Zr]/[Ti] of 0, 5, 10 and 20 at%. The Zr-doped TiO2 thin films were uniform and homogeneous showing much smaller grains than the undoped TiO2 films. Zr stabilized the anatase phase to temperatures above 800 °C depending on Zr concentration in the spray solution. The concentration of Zr determined by XPS was 6.4 at% for the thin film deposited from the 20 at% solution. According to AFM studies, Zr doping decreased the root mean square roughness of TiO2 film from 5.9 to 1.1 nm. An XRD study of samples with the highest Zr amount showed the ZrTiO4 phase started forming after annealing at 800 °C. The optical band gap for TiO2 decreased from 3.3 eV to 3.0 eV after annealing at 800 °C but for the TiO2:Zr(20) film it remained at 3.4 eV. The dielectric constant increased by more than four times with Zr-doping and this was associated with the change in the bond formations caused by substitution of Ti by Zr in the lattice.

  10. Properties of NiO thin films deposited by chemical spray pyrolysis using different precursor solutions

    NASA Astrophysics Data System (ADS)

    Cattin, L.; Reguig, B. A.; Khelil, A.; Morsli, M.; Benchouk, K.; Bernède, J. C.

    2008-07-01

    NiO thin films have been deposited by chemical spray pyrolysis using a perfume atomizer to grow the aerosol. The influence of the precursor, nickel chloride hexahydrate (NiCl 2·6H 2O), nickel nitrate hexahydrate (Ni(NO 3) 2·6H 2O), nickel hydroxide hexahydrate (Ni(OH) 2·6H 2O), nickel sulfate tetrahydrate (NiSO 4·4H 2O), on the thin films properties has been studied. In the experimental conditions used (substrate temperature 350 °C, precursor concentration 0.2-0.3 M, etc.), pure NiO thin films crystallized in the cubic phase can be achieved only with NiCl 2 and Ni(NO 3) 2 precursors. These films have been post-annealed at 425 °C for 3 h either in room atmosphere or under vacuum. If all the films are p-type, it is shown that the NiO films conductivity and optical transmittance depend on annealing process. The properties of the NiO thin films annealed under room atmosphere are not significantly modified, which is attributed to the fact that the temperature and the environment of this annealing is not very different from the experimental conditions during spray deposition. The annealing under vacuum is more efficient. This annealing being proceeded in a vacuum no better than 10 -2 Pa, it is supposed that the modifications of the NiO thin film properties, mainly the conductivity and optical transmission, are related to some interaction between residual oxygen and the films.

  11. Gallium doping in transparent conductive ZnO thin films prepared by chemical spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Babar, A. R.; Deshamukh, P. R.; Deokate, R. J.; Haranath, D.; Bhosale, C. H.; Rajpure, K. Y.

    2008-07-01

    Zinc oxide (ZnO) and ZnO : Ga films have been deposited by the spray pyrolysis method onto preheated glass substrates using zinc acetate and gallium nitrate as precursors for Zn and Ga ions, respectively. The effect of Ga doping on the structural, morphological, optical and electrical properties of sprayed ZnO thin films were investigated using x-ray diffraction (XRD), scanning electron microscopy, optical absorption, photoluminescence (PL) and Hall effect techniques. XRD studies reveal that films are polycrystalline with hexagonal (wurtzite) crystal structure. The thin films were oriented along the (0 0 2) plane. Room temperature PL measurements indicate that the deposited films exhibit proper doping of Ga in ZnO lattice. The average transparency in the visible range was around ~85-95% for typical thin film deposited using 2 at% gallium doping. The optical band gap increased from 3.31 to 3.34 eV with Ga doping of 2 at%. The addition of gallium induces a decrease in electrical resistivity of the ZnO : Ga films up to 2 at% gallium doping. The highest figure of merit observed in this present study was 3.09 × 10-3 cm2 Ω-1.

  12. Morphology Study of Prepared Carbon Nanotubes using Palm Oil as Carbon Source in Spray Pyrolysis Chemical Vapor Deposition

    NASA Astrophysics Data System (ADS)

    Azira, A. A.; Rusop, M.

    2010-03-01

    Surface morphology study on the influence of starting carbon materials by using newly developed spray pyrolysis chemical vapor deposition (Spray-CVD) to produced carbon nanotubes (CNTs) is investigated. The CNTs derived from palm oil as carbon sources were synthesized in Argon gas ambient by using Spray-CVD system. The major parameters are also evaluated in order to obtain high-yield and high-quality CNTs. The prepared CNTs are examined using field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscope (HR-TEM) to determine the microstructure of nanocarbons. The FESEM investigation of the CNTs formed on the support catalysts provides evidence that palm oil can serve as a precursor materials for nanotubes formation. The high-temperature graphitization process induced by the Spray-CVD enables the hydrocarbons to act as carbon sources and changes the aromatic species into the layered graphite structure of CNTs. The palm oil of hydrocarbons not only found acts as the precursors but also enhances the production rate of CNTs.

  13. Substrate temperature dependent studies on properties of chemical spray pyrolysis deposited CdS thin films for solar cell applications

    NASA Astrophysics Data System (ADS)

    Diwate, Kiran; Pawbake, Amit; Rondiya, Sachin; Kulkarni, Rupali; Waykar, Ravi; Jadhavar, Ashok; Rokade, Avinash; Funde, Adinath; Mohite, Kakasaheb; Shinde, Manish; Pathan, Habib; Devan, Rupesh; Jadkar, Sandesh

    2017-02-01

    Thin films of CdS have been prepared by chemical spray pyrolysis by spraying precursor solution directly onto soda lime glass (SLG) substrates. Influence of substrate temperature on structural, optical, morphological and electrical properties have been investigated by using various techniques such as low angle X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), transmission electron microscopy (TEM), UV–visible spectroscopy photoluminescence (PL) spectroscopy etc. Formation of CdS has been confirmed by low angle XRD, Raman spectroscopy and XPS analysis. XRD pattern showed that CdS films are polycrystalline, have hexagonal structure and prefer orientation of crystallites shifts from (101) to (002) with increase in substrate temperature. Raman spectroscopy revealed that exciton-phonon coupling depends on substrate temperature and hence on crystallite size. Optical band gap increased from 2.43 to 2.99 eV when substrate temperature increased from 325 to 475 ^\\circ {{C}}. Transmittance of the film also showed an increasing trend from ∼ 52 % to ∼ 80 % with increase in substrate temperature. Such high band gap and transmittance values of CdS films prepared at 475 ^\\circ {{C}} make it a useful window material in CdS/CdTe and CdS/Cu2S heterojunction solar cells. Project supported by the Department of Science and Technology (DST), Ministry of New and Renewable Energy (MNRE), Government of India, New Delhi.

  14. Chemical composition and temperature dependent performance of ZnO-thin film transistors deposited by pulsed and continuous spray pyrolysis

    SciTech Connect

    Ortel, Marlis; Balster, Torsten; Wagner, Veit

    2013-12-21

    Zinc oxide thin film transistors (TFTs) deposited by continuous and pulsed spray pyrolysis were investigated to analyze process kinetics which make reduction of process temperature possible. Thus, fluid mechanics, chemical composition, electrical performance, and deposition and annealing temperature were systematically analyzed. It was found that ZnO layers continuously deposited at 360 °C contained zinc oxynitrides, CO{sub 3}, and hydro carbonate groups from pyrolysis of basic zinc acetate. Statistically, every second wurtzite ZnO unit cell contained an impurity atom. The purity and performance of the ZnO-TFTs increased systematically with increasing deposition temperature due to an improved oxidation processes. At 500 °C the zinc to oxygen ratio exceeded a high value of 0.96. Additionally, the ZnO film was not found to be in a stabilized state after deposition even at high temperatures. Introducing additional subsequent annealing steps stabilizes the film and allows the reduction of the overall thermal stress to the substrate. Further improvement of device characteristics was obtained by pulsed deposition which allowed a more effective transport of the by-products and oxygen. A significant reduction of the deposition temperature by 140 °C was achieved compared to the same performance as in continuous deposition mode. The trap density close to the Fermi energy could be reduced by a factor of two to 4 × 10{sup 17} eV{sup −1} cm{sup −3} due to the optimized combustion process on the surface. The optimization of the deposition processes made the fabrication of TFTs with excellent performance possible. The mobility was high and exceeded 12 cm{sup 2}/V s, the subthreshold slope was 0.3 V dec{sup −1}, and an on-set close to the ideal value of 0 V was achieved.

  15. SnS Thin Films Prepared by Chemical Spray Pyrolysis at Different Substrate Temperatures for Photovoltaic Applications

    NASA Astrophysics Data System (ADS)

    Sall, Thierno; Soucase, Bernabé Marí; Mollar, Miguel; Sans, Juan Angel

    2017-01-01

    The preparation and analysis of morphological, structural, optical, vibrational and compositional properties of tin monosulfide (SnS) thin films deposited on glass substrate by chemical spray pyrolysis is reported herein. The growth conditions were evaluated to reduce the presence of residual phases different to the SnS orthorhombic phase. X-ray diffraction spectra revealed the polycrystalline nature of the SnS films with orthorhombic structure and a preferential grain orientation along the (111) direction. At high substrate temperature (450°C), a crystalline phase corresponding to the Sn2S3 phase was observed. Raman spectroscopy confirmed the dominance of the SnS phase and the presence of an additional Sn2S3 phase. Scanning electron microscopy (SEM) images reveal that the SnS film morphology depends on the substrate temperature. Between 250°C and 350°C, SnS films were shaped as rounded grains with some cracks between them, while at substrate temperatures above 400°C, films were denser and more compact. Energy-dispersive x-ray spectroscopy (EDS) analysis showed that the stoichiometry of sprayed SnS films improved with the increase of substrate temperature and atomic force microscopy micrographs showed films well covered at 350°C resulting in a rougher and bigger grain size. Optical and electrical measurements showed that the optical bandgap and the resistivity decreased when the substrate temperature increased, and smaller values, 1.46 eV and 60 Ω cm, respectively, were attained at 450°C. These SnS thin films could be used as an absorber layer for the development of tandem solar cell devices due to their high absorbability in the visible region with optimum bandgap energy.

  16. SnS Thin Films Prepared by Chemical Spray Pyrolysis at Different Substrate Temperatures for Photovoltaic Applications

    NASA Astrophysics Data System (ADS)

    Sall, Thierno; Soucase, Bernabé Marí; Mollar, Miguel; Sans, Juan Angel

    2017-03-01

    The preparation and analysis of morphological, structural, optical, vibrational and compositional properties of tin monosulfide (SnS) thin films deposited on glass substrate by chemical spray pyrolysis is reported herein. The growth conditions were evaluated to reduce the presence of residual phases different to the SnS orthorhombic phase. X-ray diffraction spectra revealed the polycrystalline nature of the SnS films with orthorhombic structure and a preferential grain orientation along the (111) direction. At high substrate temperature (450°C), a crystalline phase corresponding to the Sn2S3 phase was observed. Raman spectroscopy confirmed the dominance of the SnS phase and the presence of an additional Sn2S3 phase. Scanning electron microscopy (SEM) images reveal that the SnS film morphology depends on the substrate temperature. Between 250°C and 350°C, SnS films were shaped as rounded grains with some cracks between them, while at substrate temperatures above 400°C, films were denser and more compact. Energy-dispersive x-ray spectroscopy (EDS) analysis showed that the stoichiometry of sprayed SnS films improved with the increase of substrate temperature and atomic force microscopy micrographs showed films well covered at 350°C resulting in a rougher and bigger grain size. Optical and electrical measurements showed that the optical bandgap and the resistivity decreased when the substrate temperature increased, and smaller values, 1.46 eV and 60 Ω cm, respectively, were attained at 450°C. These SnS thin films could be used as an absorber layer for the development of tandem solar cell devices due to their high absorbability in the visible region with optimum bandgap energy.

  17. Effects of drying control chemical additive on properties of Li 4Ti 5O 12 negative powders prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Ju, Seo Hee; Kang, Yun Chan

    High-density Li 4Ti 5O 12 powders comprising spherical particles are prepared by spray pyrolysis from a solution containing dimethylacetamide (drying control chemical additive) and citric acid and ethylene glycol (organic additives). The prepared powders have high discharge capacities and good cycle properties. The optimum concentration of dimethylacetamide is 0.5 M. The addition of dimethylacetamide to the polymeric spray solutions containing citric acid and ethylene glycol helps in the effective control of the morphology of the Li 4Ti 5O 12 powders. At a constant current density of 0.17 mA g -1, the initial discharge capacities of the powders obtained from the spray solution with and without the organic additives are 171 and 167 mAh g -1, respectively.

  18. Producing Quantum Dots by Spray Pyrolysis

    NASA Technical Reports Server (NTRS)

    Banger, Kulbinder; Jin, Michael H.; Hepp, Aloysius

    2006-01-01

    An improved process for making nanocrystallites, commonly denoted quantum dots (QDs), is based on spray pyrolysis. Unlike the process used heretofore, the improved process is amenable to mass production of either passivated or non-passivated QDs, with computer control to ensure near uniformity of size.

  19. Ceramic powder synthesis by spray pyrolysis

    SciTech Connect

    Messing, G.L.; Zhang, Shi Chang; Jayanthi, G.V. . Particulate Materials Center)

    1993-11-01

    A variety of spray pyrolysis (SP) techniques have been developed to directly produce ceramic powders from solutions. This paper reviews the current status of these processes in terms of the process parameters that enable the formation of particles with controlled morphology and composition. A model incorporating solute diffusion in the droplet and solvent evaporation from the droplet surface is presented to establish the critical parameters leading to solid particle formation. The model illustrates that solid particles can be obtained if solutes with high solubility and a large difference between the critical supersaturation and equilibrium concentration are used and if the process is designed to avoid solvent boiling. It is demonstrated that mixed metal oxide, non-oxide, and composite particles that are solid, hollow, porous, or fibrous can be produced by modifying the precursor characteristics, solution properties, and process parameters. The physical and chemical flexibility of SP processes offers numerous opportunities for the controlled synthesis of advanced ceramic powders and films. However, production rates are limited by the need to produce <5-[mu]m-diameter droplets and to avoid subsequent droplet coagulation. Developments in process controls, atomization, and system design are required for wider commercialization of SP-type processes.

  20. Structural, optical and electrical properties of CuInS2 thin films prepared by chemical spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Terasako, Tomoaki; Uno, Yuji; Inoue, Seiki; Kariya, Tetsuya; Shirakata, Sho

    2006-09-01

    Polycrystalline CuInS2 thin films were prepared by chemical spray pyrolisis (CSP) on glass sustrate from the ethanol aqueous solution containing CuCl2, InCl3 and thiourea. Structual, electrical and optical properties were systematically studied in terms of substrate temperature, pH and the ion ratio (Cu/In) of the spray solution. Although the In-rich films were composed of CuInS2 and In2S3, the In2S3 content in the film decreased with Cu/In ratio. Appearance of Raman peaks at 288 and 298 cm-1 indicated that the films contained CuInS2 with chalcopyrite and CuAu phases. Typical grain size in the Cu-rich films was 200 nm. Optical gap energies were approximately 0.1-0.2eV smaller than the bandgap energy of the CuInS2 bulk crystal. Resisitivity of the Cu-rich films without In2S3 secondary phase was 0.2-5 cm.

  1. Effect of variation of tin concentration on the properties of Cu2ZnSnS4 thin films deposited using chemical spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Rajeshmon, V. G.; Kuriakose, Abin; Kartha, C. Sudha; Vijayakumar, K. P.

    2013-02-01

    Cu2ZnSnS4 (CZTS) thin films were prepared using chemical spray pyrolysis technique on soda lime glass (SLG) substrates. The effect of tin concentration on the structural, optical and electrical properties was investigated. We deposited films by varying tin concentration from 0.007 M to 0.013 M in steps of 0.0015 M keeping the concentration of copper, zinc and sulphur at 0.02 M, 0.01 M and 0.12 M respectively. It was found that crystallinity of the film increased up to the tin concentration of 0.01 M and then decreases. Band gap of the films steadily decreased from 1.48 to 1.26 eV with increase in tin concentration. All the samples were observed to be p-type by hot probe method. Resistivity of the films increased with increase in tin concentration. In this work we tuned the optoelectronic properties by varying the tin concentration alone and optimized the concentration of tin which yields samples ideal for photovoltaic applications.

  2. Zinc oxide films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Maciąg, Andrzej; Sagan, Piotr; Kuźma, Marian; Popovych, Volodymyr

    2016-12-01

    In this work we developed and tested spray pyrolysis system for layers deposition. In the system we have used ultrasonic apparatus (nebulizator) as a sprayer. A zinc nitrate aqueous solution has been used as a precursor solution. The idea of the method is the decomposition of nitrate on a hot substrate according to the reaction Zn(NO3)2 → ZnO +2 NO2 +1/2O2. The layers were grown on glass, (001)Si and KCl substrates at the temperatures 300 - 500°C. The thickness of the obtained layers was in the range 50 - 500 nm, depending on the growth time and rate. The influence of substrate temperature on the morphology of the layers has been studied by SEM method. The energy gap of the layers was found to be the range of 3.26-3.3 eV from their absorption spectra.

  3. Zinc oxide films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Maciąg, Andrzej; Sagan, Piotr; Kuźma, Marian; Popovych, Volodymyr

    2017-01-01

    In this work we developed and tested spray pyrolysis system for layers deposition. In the system we have used ultrasonic apparatus (nebulizator) as a sprayer. A zinc nitrate aqueous solution has been used as a precursor solution. The idea of the method is the decomposition of nitrate on a hot substrate according to the reaction Zn(NO3)2 → ZnO +2 NO2 +1/2O2. The layers were grown on glass, (001)Si and KCl substrates at the temperatures 300 - 500°C. The thickness of the obtained layers was in the range 50 - 500 nm, depending on the growth time and rate. The influence of substrate temperature on the morphology of the layers has been studied by SEM method. The energy gap of the layers was found to be the range of 3.26-3.3 eV from their absorption spectra.

  4. Photoluminescence of spray pyrolysis deposited ZnO nanorods

    NASA Astrophysics Data System (ADS)

    Kärber, Erki; Raadik, Taavi; Dedova, Tatjana; Krustok, Jüri; Mere, Arvo; Mikli, Valdek; Krunks, Malle

    2011-04-01

    Photoluminescence of highly structured ZnO layers comprising well-shaped hexagonal rods is presented. The ZnO rods (length 500-1,000 nm, diameter 100-300 nm) were grown in air onto a preheated soda-lime glass (SGL) or ITO/SGL substrate by low-cost chemical spray pyrolysis method using zinc chloride precursor solutions and growth temperatures in the range of 450-550°C. We report the effect of the variation in deposition parameters (substrate type, growth temperature, spray rate, solvent type) on the photoluminescence properties of the spray-deposited ZnO nanorods. A dominant near band edge (NBE) emission is observed at 300 K and at 10 K. High-resolution photoluminescence measurements at 10 K reveal fine structure of the NBE band with the dominant peaks related to the bound exciton transitions. It is found that all studied technological parameters affect the excitonic photoluminescence in ZnO nanorods. PACS: 78.55.Et, 81.15.Rs, 61.46.Km

  5. Photoluminescence of spray pyrolysis deposited ZnO nanorods.

    PubMed

    Kärber, Erki; Raadik, Taavi; Dedova, Tatjana; Krustok, Jüri; Mere, Arvo; Mikli, Valdek; Krunks, Malle

    2011-04-21

    Photoluminescence of highly structured ZnO layers comprising well-shaped hexagonal rods is presented. The ZnO rods (length 500-1,000 nm, diameter 100-300 nm) were grown in air onto a preheated soda-lime glass (SGL) or ITO/SGL substrate by low-cost chemical spray pyrolysis method using zinc chloride precursor solutions and growth temperatures in the range of 450-550°C. We report the effect of the variation in deposition parameters (substrate type, growth temperature, spray rate, solvent type) on the photoluminescence properties of the spray-deposited ZnO nanorods. A dominant near band edge (NBE) emission is observed at 300 K and at 10 K. High-resolution photoluminescence measurements at 10 K reveal fine structure of the NBE band with the dominant peaks related to the bound exciton transitions. It is found that all studied technological parameters affect the excitonic photoluminescence in ZnO nanorods.PACS: 78.55.Et, 81.15.Rs, 61.46.Km.

  6. Photoluminescence of spray pyrolysis deposited ZnO nanorods

    PubMed Central

    2011-01-01

    Photoluminescence of highly structured ZnO layers comprising well-shaped hexagonal rods is presented. The ZnO rods (length 500-1,000 nm, diameter 100-300 nm) were grown in air onto a preheated soda-lime glass (SGL) or ITO/SGL substrate by low-cost chemical spray pyrolysis method using zinc chloride precursor solutions and growth temperatures in the range of 450-550°C. We report the effect of the variation in deposition parameters (substrate type, growth temperature, spray rate, solvent type) on the photoluminescence properties of the spray-deposited ZnO nanorods. A dominant near band edge (NBE) emission is observed at 300 K and at 10 K. High-resolution photoluminescence measurements at 10 K reveal fine structure of the NBE band with the dominant peaks related to the bound exciton transitions. It is found that all studied technological parameters affect the excitonic photoluminescence in ZnO nanorods. PACS: 78.55.Et, 81.15.Rs, 61.46.Km PMID:21711895

  7. Air-assisted ultrasonic spray pyrolysis for nanoparticles synthesis

    NASA Astrophysics Data System (ADS)

    Tsai, Shirley C.; Song, Yu L.; Chen, C. Y.; Tseng, T. K.; Tsai, Chen S.

    2002-11-01

    This paper presents new findings regarding the effects of precursor drop size and concentration on product particle size and morphology in ultrasonic spray pyrolysis of zirconium hydroxyl acetate solutions. Large precursor drops (diameter >30μm) generated by ultrasonic atomization at 120kHz yielded particles with holes. Precursor drops 6-9 μm in diameter, generated by an ultrasonic nebulizer at 1.65MHz and 23.5W electric drive power, yielded uniform spherical particles 150nm in diameter under proper control of heating rate and precursor concentration. Moreover, air-assisted ultrasonic spray pyrolysis at 120kHz and 2.3W yielded spherical particles of which nearly half were smaller than those produced by the ultrasonic spray pyrolysis of the 6-9 μm precursor drops, desprite the much larger precursor drop sizes (28 μm peak diameter versus 7 μm mean diameter). These particles are much smaller than those predicted by the conventional one particle per drop mechanism, suggesting that a vapor condensation mechanism may also be involved in spray pyrolysis. It may be concluded that through this new mechanism air-assisted ultrasonic spray pyrolysis can become a viable process for mass production of nanoparticles.

  8. Thin films of SiO2 and hydroxyapatite on titanium deposited by spray pyrolysis.

    PubMed

    Jokanovic, V; Jokanovic, B; Izvonar, D; Dacic, B

    2008-05-01

    Wet spray pyrolysis of fine, well-dispersed a SiO2 sol was used for the deposition of thin films of silicon dioxide. The sol was obtained by hydrothermal precipitation of silicon acid from a solution at pH = 10. The morphology, roughness, phase composition, chemical homogeneity and the mechanism of the films were investigated by SEM, EDS and IR spectroscopy. The obtained results show a complete covering of the titanium substrate with SiO2 after 3 h of deposition. It was observed that the film thickness increased from 3 to 19 microm, the roughness of the film decreased from 12 to 3 microm, while the morphology of the deposit changed considerably. A hydroxyapatite film was prepared on the so-obtained SiO2 thin film by spray pyrolysis deposition and its morphology and phase composition were investigated.

  9. Porous carbon powders prepared by ultrasonic spray pyrolysis.

    PubMed

    Skrabalak, Sara E; Suslick, Kenneth S

    2006-10-04

    New, thermally robust meso- and macroporous carbon powders were prepared by ultrasonic spray pyrolysis (USP) of aqueous solutions using an inexpensive high-frequency ultrasound generator from a household humidifier. We choose our molecular precursors rationally, so that the expected decomposition pathways produce only remnant carbon atoms. Specifically, our rational design criterion led to halo-organic carboxylate salts, whose pyrolysis yields well-defined carbon solids with a temporary template being generated in situ, simply an inorganic salt, which is easily dissolved during aqueous workup. The materials have been characterized by SEM, TEM, XRD, 13C NMR MAS, XPS, FTIR spectroscopy, and BET surface area measurements. Changing the alkali metal alters the morphology and pore structure of the final material, which can be explained in terms of the observed differences in the DSC and TGA of the various precursors. This preparatory method provides an extremely facile and versatile method for the generation of meso- and macroporous carbons.

  10. Aerosol spray pyrolysis & solution phase synthesis of nanostructures

    NASA Astrophysics Data System (ADS)

    Zhang, Hongwang

    This dissertation focuses on the synthesis of nanomaterials by both solution phase and gas phase methods. By the solution phase method, we demonstrate the synthesis of Au/CdS binary hybrid nanoparticles and the Au-induced growth of CdS nanorods. At higher reaction temperature, extremely uniform CdS nanorods were obtained. The size of the Au seed nanoparticles has an important influence on the length and diameter of the nanorods. In addition, preparation of peanut-like FePt-CdS hybrid nanoparticles by spontaneous epitaxial nucleation and growth of CdS onto FePt-seed nanoparticles in high-temperature organic solution is reported. The FePt-CdS hybrid nanoparticles reported here are an example of a bifunctional nanomaterial that combines size-dependent magnetic and optical properties. In the gas phase method, a spray pyrolysis aerosol synthesis method was used to produce tellurium dioxide nanoparticles and zinc sulfide nanoparticles. Tellurite glasses (amorphous TeO2 based materials) have two useful optical properties, high refractive index and high optical nonlinearity, that make them attractive for a range of applications. In the work presented here, TeO2 nanoparticles were prepared by spray pyrolysis of an aqueous solution of telluric acid, Te(OH)6. This laboratory-scale process is capable of producing up to 80 mg/hr of amorphous TeO2-nanoparticles with primary particle diameters from 10 to 40 nm, and allows their synthesis in significant quantities from an inexpensive and environmentally friendly precursor. Furthermore, both Er3+ doped and Er3+ and Yb3+ co-doped tellurium dioxide nanoparticles were synthesized by spray pyrolysis of an aqueous mixture of telluric acid with erbium/ytterbium salts, which exhibit the infrared to green visible upconversion phenomena. ZnS nanoparticles (NPs) were prepared by spray pyrolysis using zinc diethyldithiocarbamate as a single-source precursor. The home-built scanning mobility particle spectrometer (SMPS) is a useful tool for

  11. Chemical spray pyrolysis of Tl-Ba-Ca-Cu-O high-T(sub c) superconductors for high-field bitter magnets

    NASA Technical Reports Server (NTRS)

    Derochemont, L. Pierre; Zhang, John G.; Squillante, Michael R.; Hermann, A. M.; Duan, H. M.; Andrews, Robert J.; Kelliher, Warren C.

    1991-01-01

    The deposition of Tl-Ba-Ca-Cu-O thick films by spray pyrolyzing a Ba-Ca-Cu-O precursor film and diffusing thallium into the film to form the superconducting phase is examined. This approach was taken to reduce exposure to thallium and its health and safety hazards. The Tl-Ba-Ca-Cu-O system was selected because it has very attractive features which make it appealing to device and manufacturing engineering. Tl-Ba-Ca-Cu-O will accommodate a number of superconducting phases. This attribute makes it very forgiving to stoichiometric fluctuations in the bulk and film. It has excellent thermal and chemical stability, and appears to be relatively insensitive to chemical impurities. Oxygen is tightly bound into the systems, consequently there is no orthorhombic (conductor) to tetragonal (insulator) transition which would affect a component's lifetime. More significantly, the thallium based superconductors appear to have harder magnetic properties than the other high-Tc oxide ceramics. Estimates using magnetoresistance measurements indicate that at 77 K Tl2Ba2CaCu2O10 will have an upper critical field, H(sub c2) fo 26 Tesla for applied fields parallel to the c-axis and approximately 1000 Tesla for fields oriented in the a-b plane. Results to date have shown that superconducting films can be reproducibly deposited on 100 oriented MgO substrates. One film had a zero resistance temperature of 111.5 K. Furthermore, x ray diffraction analysis of the films showed preferential c-axis orientation parallel to the plane of the substrate. These results have now made it possible to consider the manufacture of a superconducting tape wire which can be configured into a topology useful for high-field magnet designs. The research which leads to the preparation of these films and plans for further development are reviewed.

  12. Thin Film CuInS2 Prepared by Spray Pyrolysis with Single-Source Precursors

    NASA Technical Reports Server (NTRS)

    Jin, Michael H.; Banger, Kulinder K.; Harris, Jerry D.; Cowen, Jonathan E.; Hepp, Aloysius F.; Lyons, Valerie (Technical Monitor)

    2002-01-01

    Both horizontal hot-wall and vertical cold-wall atmospheric chemical spray pyrolysis processes deposited near single-phase stoichiometric CuInS2 thin films. Single-source precursors developed for ternary chalcopyrite materials were used for this study, and a new liquid phase single-source precursor was tested with a vertical cold-wall reactor. The depositions were carried out under an argon atmosphere, and the substrate temperature was kept at 400 C. Columnar grain structure was obtained with vapor deposition, and the granular structure was obtained with (liquid) droplet deposition. Conductive films were deposited with planar electrical resistivities ranging from 1 to 30 Omega x cm.

  13. Generation of size-monodisperse metal nanoparticles by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Kim, Jung Hyeun

    2003-10-01

    Size-monodisperse pure copper metal particles were formed from metal salt precursors in a spray pyrolysis process that uses ethanol as a co-solvent, thus avoiding the addition of hydrogen or other reducing gases. In addition, the uniform-size particles were classified using a droplet impactor plate, which eliminates larger droplets at the atomizer prior to entering the reactor furnace. To investigate the role of ethanol co-solvent for the formation of phase pure metal particles in the spray pyrolysis process, the generation of phase pure copper and nickel particles from aqueous solutions of copper acetate, copper nitrate, and nickel nitrates over the temperature range of 450°C to 1000°C was demonstrated. Addition of ethanol as a co-solvent played a crucial role in producing phase pure metal powders. Results of a modeling study of ethanol decomposition kinetics suggested that co-solvent decomposition created a strong reducing atmosphere during spray pyrolysis via in-situ production of hydrogen and carbon monoxide. With the size-classified copper spheres as well as monodisperse polystyrene latex (PSL) spheres, the polarization and intensity of light scattered by those spheres, having diameters ranging from 92 nm to 218 nm, deposited on silicon substrates were measured using 442 nm, 532 nm, and 633 nm light. The results showed that accurate calculation of the scattering of light by a metal sphere requires that the near-field interaction between the sphere and its image is included in a complete manner. The normal incidence approximation did not suffice for this interaction, and the existence of any thin oxide layer on the substrate must be included in the calculation. In order to further examine the effects of light scattering by particles on a silicon substrate having an oxide coating, the polarization and intensity of light scattered by 101 nm polystyrene latex (PSL) and 100 nm copper spheres, deposited on silicon substrates containing various thickness of oxide

  14. Synthesis of Potassium Silicate Nanoparticles from Rice Straw Ash Using a Flame-assisted Spray-pyrolysis Method

    NASA Astrophysics Data System (ADS)

    Nandiyanto, A. B. D.; Permatasari, N.; Sucahya, T. N.; Abdullah, A. G.; Hasanah, L.

    2017-03-01

    The purpose of this study was to synthesize potassium silicate nanoparticles from rice straw ash using a flame-assisted spray-pyrolysis method. Rice straw, as one of the agricultural wastes, was used as a source of silica. In the experimental procedure, rice straw was burned at 700°C for 3 hours to produce rice straw ash. Then, the rice straw ash was extracted using an alkaline method. We used potassium hydroxide (KOH) as an alkaline chemical agent as well as a source of potassium. The solution was then put into the flame-assisted spray-pyrolysis apparatus to produce potassium silicate nanoparticles. The results showed that the spray method can assist the production of spherical potassium silicate nanoparticles with sizes of about 50 nm.

  15. Magnetic and porous nanospheres from ultrasonic spray pyrolysis.

    PubMed

    Suh, Won Hyuk; Suslick, Kenneth S

    2005-08-31

    We have used an inexpensive high-frequency ultrasound generator from a household humidifier to create a useful source for ultrasonic spray pyrolysis and produced submicrometer silica particles that are porous on the nanometer scale. By using two heated zones, we first initiate polymerization of organic monomers in the presence of silica colloid, which creates in situ a composite of silica with an organic polymer, followed by a second heating to pyrolyze and remove the polymer. The morphology and surface area of the final porous silica are controlled by varying the silica-to-organic monomer ratio. In a single flow process, ferromagnetic cobalt nanoparticles can be easily encapsulated in the porous silica, and the resulting nanospheres are extremely resistant to air oxidation. Products were characterized by SEM, (S)TEM, EDS, XPS, and SQUID.

  16. SnS2 Thin Film Deposition by Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Jaber, Abdallah Yahia; Alamri, Saleh Noaiman; Aida, Mohammed Salah

    2012-06-01

    Tin disulfide (SnS2) thin films have been synthesized using a simplified spray pyrolysis technique using a perfume atomizer. The films were deposited using two different solutions prepared by the dilution of SnCl2 and thiourea in distilled water and in methanol. The obtained films have a microcrystalline structure. The film deposited using methanol as the solvent is nearly stochiometric SnS2 with a spinel phase having a (001) preferential orientation. The film prepared with an aqueous solution is Sn-rich. Scanning electronic microscopy (SEM) images reveal that the film deposited with the aqueous solution is rough and is formed with large wires. However, the film deposited with methanol is dense and smooth. Conductivity measurements indicate that the aqueous solution leads to an n-type semiconductor, while methanol leads to a p-type semiconductor.

  17. Titania by spray pyrolysis for photocatalytic destruction of organics in aqueous solutions

    SciTech Connect

    Fotou, G.P.; Himebaugh, L.; Kodas, T.T.; Wu, M.

    1996-12-31

    In this study, the potential of spray pyrolysis and spray calcination for the synthesis of effective titanium dioxide photocatalysts is explored. The product titanium dioxide powders were used in the photoassisted oxidation of salicylic acid in aqueous solutions. Titania particles were produced by spray pyrolysis of dihydroxybis titanium solutions in water at concentrations between 20 to 70% by volume at temperatures from 500 to 1100{degrees}C. Powders were made by spray calcination of titanium hydrolysate solutions at temperatures from 700 to 900 {degrees}C. Spray pyrolysis produced titania particles which were partially hollow. Spray calcination resulted in agglomerates which consisted of 15 nm primary particles that showed high photoactivity in the photooxidation of aqueous salicylic acid solutions. Doping with palladium oxide or ruthenium oxides did not improve the photocatalytic activity of these powders. 6 refs., 3 figs.

  18. ZnO layers prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Messaoudi, C.; Abd-Lefdil, S.; Sayah, D.; Cadene, M.

    1998-02-01

    Highly transparent undoped and indium doped ZnO thin films have been grown on glass substrates by using the spray pyrolysis process. Conditions of preparation have been optimized to get good quality and reproducible films with required properties. Polycrystalline films with an hexagonal Wurtzite-type structure were easily obtained under the optimum spraying conditions. Both of samples have shown high transmission coefficient in the visible and infrared wavelength range with sharp absorption edge around 380 nm which closely corresponds to the intrinsic band-gap of ZnO (3.2 eV). Orientation and crystallites size were remarkably modified by deposition temperature and indium doping. Des couches minces de ZnO, hautement transparentes, non dopées et dopées à l'indium ont été élaborées sur un substrat en verre par le procédé de pulvérisation chimique réactive spray. Les conditions de préparation ont été optimisées pour l'obtention de couches reproductibles, de bonne qualité et ayant les propriétés requises. Des films polycristallins, présentant une structure hexagonale de type Wurtzite, ont été aisément obtenus dans les conditions optimales de pulvérisation. Tous les échantillons ont présenté un coefficient de transmission élevé dans le domaine du visible et du proche infrarouge, avec une absorption brutale au voisinage de 380 nm, correspondant au gap optique du ZnO (3,2 eV). L'orientation et la taille des cristallites ont été remarquablement modifiées par la température du dépôt et par le dopage à l'indium.

  19. Fabrication of functional nanomaterials using flame assisted spray pyrolysis

    SciTech Connect

    Purwanto, Agus

    2014-02-24

    Flame assisted spray pyrolysis (FASP) is a class of synthesis method for nanomaterials fabrication. The ability to control nanomaterials characteristics and easy to be-scaled up are the main features of FASP. The crystallinity and particles size of the prepared nanomaterials can be easily controlled by variation of fuel flow rate. The precursor concentration, carrier gas flow rate, and carrier gas can be also used to control the prepared nanomaterials. Energy related nanomaterials preparation uses as the example case in FASP application. These material are yttrium aluminum garnet (YAG:Ce) and tungsten oxide (WO{sub 3}). It needs strategies to produce these materials into nano-sized order. YAG:Ce nanoparticles only can be synthesized by FASP using the urea addition. The decomposition of urea under high temperature of flame promotes the breakage of YAG:Ce particles into nanoparticles. In the preparation of WO{sub 3}, the high temperature flame can be used to gasify WO{sub 3} solid material. As a result, WO{sub 3} nanoparticles can be prepared easily. Generally, to produce nanoparticles via FASP method, the boiling point of the material is important to determine the strategy which will be used.

  20. Electrical Properties of CZO Films Prepared by Ultrasonic Spray Pyrolysis

    PubMed Central

    Chen, Lung-Chien; Hsieh, Cheng-An; Zhang, Xiuyu

    2014-01-01

    CuZnO (CZO) films have attracted increasing amounts of attention due to their promising potential applications in semiconductor devices. ZnO shows n-type conductivity, and attempts have been made to dope several elements in ZnO to improve the electrical properties. This study investigated the electrical property transitions of CZO films and determined the copper concentration at which the conductivity of CZO films will change from n-type to p-type. In this study, CZO films were fabricated by ultrasonic spray pyrolysis with copper acetate, zinc acetate, and ammonium acetate precursor solution. The concentrations of Cu ions in the CZO films were controlled by the concentration ratios of copper acetate to zinc acetate in the precursor solutions. In addition, these samples were analyzed by Hall effect measurements, X-ray diffraction, transmittance measurements, and photoluminescence measurements. The results show that the conductivity of the CZO film changes from n-type to p-type when the copper ion concentration in the film is 5%. PMID:28788247

  1. Cytotoxicity of gold nanoparticles prepared by ultrasonic spray pyrolysis.

    PubMed

    Rudolf, R; Friedrich, B; Stopić, S; Anžel, I; Tomić, S; Čolić, M

    2012-01-01

    The aim of this work was to study the cytotoxicity of different fractions of gold nanoparticles prepared by ultrasonic spray pyrolysis from gold scrap. The target cells were rat thymocytes, as a type of nonproliferating cells, and L929 mouse fibroblasts, as a type of continuous proliferating cells. Fractions 1 and 2, composed of pure gold nanoparticles, as determined by scanning electron microscopy with a combination of energy dispersive X-ray analysis, were nontoxic for thymocytes, but reduced moderately the proliferative activity of L929 cells. The inhibitory effect of fraction 2, containing particles smaller in size than fraction 1, was stronger. Fraction 3, composed of Au and up to 3% Cu was noncytotoxic for thymocytes, but was cytotoxic for L929 cells. Fraction 4, composed of Au and Ag nanoparticles, and fraction 5, composed of Au together with Cu, Ni, Zn, Fe, and In were cytotoxic for both thymocytes and L929 cells. These results suggest that USP enables the synthesis of pure gold nanoparticles with controlled size, even from gold scrap. However, microstructural analyses and biocompatibility testing are necessary for their proper selection from more cytotoxic gold nanoparticles, contaminated with other elements of gold alloys.

  2. Effect of precursor concentration and spray pyrolysis temperature upon hydroxyapatite particle size and density.

    PubMed

    Cho, Jung Sang; Lee, Jeong-Cheol; Rhee, Sang-Hoon

    2016-02-01

    In the synthesis of hydroxyapatite powders by spray pyrolysis, control of the particle size was investigated by varying the initial concentration of the precursor solution and the pyrolysis temperature. Calcium phosphate solutions (Ca/P ratio of 1.67) with a range of concentrations from 0.1 to 2.0 mol/L were prepared by dissolving calcium nitrate tetrahydrate and diammonium hydrogen phosphate in deionized water and subsequently adding nitric acid. Hydroxyapatite powders were then synthesized by spray pyrolysis at 900°C and at 1500°C, using these calcium phosphate precursor solutions, under the fixed carrier gas flow rate of 10 L/min. The particle size decreased as the precursor concentration decreased and the spray pyrolysis temperature increased. Sinterability tests conducted at 1100°C for 1 h showed that the smaller and denser the particles were, the higher the relative densities were of sintered hydroxyapatite disks formed from these particles. The practical implication of these results is that highly sinterable small and dense hydroxyapatite particles can be synthesized by means of spray pyrolysis using a low-concentration precursor solution and a high pyrolysis temperature under a fixed carrier gas flow rate. © 2015 Wiley Periodicals, Inc.

  3. Formation of CuAlO2 Film by Ultrasonic Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Iping, S.; Lockman, Zainovia; Hutagalung, S. D.; Kamsul, A.; Matsuda, Atsunori

    2011-10-01

    Smooth, crack free and homogenous CuAlO2 film was produced by chemical solution deposition process via spray pyrolysis technique on a cleaned Si substrate. The precursor solution used was comprised of a mixture of 45.87 mmol Cu(NO3)2.3H2O and 90 mmol Al(NO3)3.9H2O at ratio of Cu:Al = 1.2:1. The precursor solution was placed in a mist chamber and was atomized by a nebulizer to produce precursor mist. The precursor mist was then carried out by Ar gas and was sprayed onto a heated Si. Two main parameters were studied: the distance between the nozzle of the precursor mist chamber and the Si and the temperature of the Si substrate. It appears that from the XRD data, CuAlO2 can be detected for samples prepared by spraying the precursor mist at temperature of > 550 °C with distance between the nozzle and the substrate of 3cm. Reaction of the Cu and Al ions in the mist near the substrate may have promoted the crystallisation of CuAlO2.

  4. Study of the influence of substrate temperature on structural, optical, and electrical properties of Zn-doped MnIn2S4 thin films prepared by chemical spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Kennedy, A.; Viswanathan, K.; Pradeev raj, K.

    2016-08-01

    The Zn-doped MnIn2S4 thin films were deposited by chemical spray pyrolysis technique on a heated glass substrate using the aqueous solution of MnCl2, InCl3, (NH2)2CS and ZnCl2. The thin films were grown at different substrate temperatures ranging from 250-400 °C. The synthesized films were characterized by X-ray diffraction (XRD), energy dispersive analysis spectrum (EDS), field emission scanning electron microscope (FESEM), UV-Vis absorption spectroscopy and four probe method. The XRD analysis indicates Zn-doped MnIn2S4 thin films were polycrystalline in nature with a cubic spinel structure having (101) plane as the preferred orientation. The structural parameters like crystalline size (D), dislocation density (δ), strain (ε) and lattice distortion (LD) have been evaluated from XRD results. The energy dispersive analysis spectrum (EDS) predicts the presence of Mn, In, S and Zn in the film grown at 250 °C. The formation of the needle and spherical shaped grains was clearly observed from FE-SEM analysis. From the optical studies, it is analyzed that about (88%) of light transmission occurs in the Vis-IR regions. It is interesting to note that the structural homogeneity and crystallinity of the films has improved due to the decrease in the absorption coefficient (α) and extinction coefficient (K) with an increase in substrate temperature. The calculated optical band gap energies increase (1.51-1.74 eV) with an increase of substrate temperatures. The photoluminescence (PL) spectrum reveals the presence of well-defined band edge (<400 nm) and defect emissions in the wavelength region around 400-650 nm. Moreover, from electrical studies, the electrical resistivity decreases with increase in substrate temperature and a minimum electrical resistivity of 1.20 ×103 Ωm was obtained for the film coated at 400 °C. The high absorption coefficient (α) in the order of 104cm-1 and high transmittance (88%) of the films makes them an efficient absorber and a good window

  5. Fabrication of CIGS thin films by using spray pyrolysis and post-selenization

    NASA Astrophysics Data System (ADS)

    Kim, Seong Yeon; Kim, JunHo

    2012-06-01

    We fabricated Cu(In1- x Ga x )Se2 ( x: 0 ˜ 0.4) thin films by using ultrasonic spray pyrolysis and post-selenization. First, we made Cu(In1- x Ga x )S2 ( x: 0 ˜ 0.4) films by ultrasonic spray pyrolysis under an air environment. Then, we converted as-sprayed Cu(In1- x Ga x )S2 (CIGS) films to Cu-(In1- x Ga x )Se2 (CIGSe) films through post-selenization. For all Ga fractions, the sprayed CIGS films were well recrystallized into poly-crystalline CIGSe films with a dominant (112) texture, which was confirmed by X-ray diffraction, Raman spectroscopy and energy dispersive X-ray analyses. This result indicates that CIGSe films with any amount of Ga substitution can be made by converting sprayed CIGS to CIGSe with post-selenization.

  6. Synthesis of gold nanoparticles with a modified ultrasonic spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Majeric, Peter

    This Doctoral Dissertation presents the studies, experimental work, characterization techniques, results and analyses of synthesis of very pure, spherical, unagglomerated gold nanoparticles (AuNPs), with sizes around 50 nm. In the first part of the research, the AuNPs were synthesized with conventional Ultrasonic Spray Pyrolysis (USP). For the raw material, tetrachloroauric acid HAuCl4(s) was dissolved in water. This precursor solution was then sprayed into droplets with ultrasound, and a carrier gas N2 then transported the droplets into a reaction furnace. In this furnace the AuNP synthesis stages took place: Droplet evaporation, thermal decomposition, reduction with H2 gas and densification. The resulting AuNPs had diverse shapes in sizes up to 300 nm, with a high degree of agglomeration. Because the aim was not achieved with the conventional USP, a hypothesis was proposed where the targeted AuNPs could be synthesized with a modified USP. With this modification, the droplet evaporation zone is separated from the reaction furnace and the reduction gas is introduced directly into the reaction furnace. To confirm this hypothesis we have carried out experiments in order to determine the influential parameters of USP synthesis: The concentration of Au in the precursor solution, evaporation zone temperature, reaction furnace temperature and gas flows of N2 and H2. Characterization of the obtained AuNPs has shown that 2 formation mechanisms take place in USP synthesis (Droplet-to-Particle, DTP and Gas-to-Particle, GTP). With DTP, nanoparticles up to 300 nm are formed, while smaller nanoparticles up to 50 nm are formed with GTP. When both mechanisms occur simultaneously, we obtain a bimodal size distribution of AuNPs. Based on these findings, we have set up an AuNP formation model, explaining how one can control the DTP and GTP mechanisms in USP by changing the most influential parameters, the concentration of Au in the precursor solution and the gas flows. Based on this

  7. Growth of ZnO rods on FTO electrodes by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Dedova, Tatjana; Volobujeva, Olga; Krunks, Malle; Mikli, Valdek; Gromyko, Inga; Katerski, Atanas; Mere, Arvo

    2013-12-01

    ZnO layers comprizing rods were deposited by chemical spray pyrolysis (CSP) method at 520 °C on different FTO (SnO2:F)/glass substrates using zinc chloride aqueous solutions. Substrates were purchased from different manufactures and differ by morphology, grain size and roughness of FTO electrode. FTO/glass substrates and ZnO layers grown on them were characterised with the help of XRD, AFM, high resolution SEM, EDX methods. The relationship between nanorod formation and substrate properties was studied. It was found that substrate roughness and grain size influence the ZnO rods formation. Deposition of rods (d=300 nm, L=1.4 μm) was successful on the FTO layers with grain sizes around 30-50 nm and roughness below 10 nm, whereas large-grained FTO (grain size > 130 nm) resulted in thick, low-aspect ratio crystals with diameter around 400 nm and length of about 400 nm.

  8. Influence of zinc precursor concentration on properties zinc sulphide thin films using spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Veena, E.; Bangera, Kasturi V.; Shivakumar, G. K.

    2017-07-01

    Stoichiometric high transparent n-zinc sulphide thin films were prepared using chemical spray pyrolysis technique. The concentration of the cationic precursor played a major role to obtain stoichiometry, regardless of various deposition parameters. Zinc sulphide films deposited at 450˚C for the ratio 0.33:1 (Zn:S) resulted in well oriented, stoichiometric polycrystalline cubic structure. The variation in crystallite size associated with the cationic precursor concentration provides significant control over the structural, optical and electrical properties of the films. The optical band gap and activation energy of stoichiometric ZnS films were found to be 3.54 ± 0.02eV and 0.82 ± 0.05eV, respectively. The absorption coefficient of the films was found to be 102 cm-1.

  9. A Spray Pyrolysis Method to Grow Carbon Nanotubes on Carbon Fibres, Steel and Ceramic Bricks.

    PubMed

    Vilatela, Juan J; Rabanal, M E; Cervantes-Sodi, Felipe; García-Ruiz, Máximo; Jiménez-Rodríguez, José A; Reiband, Gerd; Terrones, Mauricio

    2015-04-01

    We demonstrate a spray pyrolysis method to grow carbon nanotubes (CNTs) with high degree of crystallinity, aspect ratio and degree of alignment on a variety of different substrates, such as conventional steel, carbon fibres (CF) and ceramics. The process consists in the chemical vapour deposition of both a thin SiO2 layer and CNTs that subsequently grow on this thin layer. After CNT growth, increases in specific surface by factors of 1000 and 30 for the steel and CF samples, respectively, are observed. CNTs growth on ceramic surfaces results in a surface resistance of 37.5 Ohm/sq. When using conventional steel as a rector tube, we observed CNTs growth rates of 0.6 g/min. Details of nanotube morphology and the growth mechanism are discussed. Since the method discussed here is highly versatile, it opens up a wide variety of applications in which specific substrates could be used in combination with CNTs.

  10. Enhanced early osteogenic differentiation by silicon-substituted hydroxyapatite ceramics fabricated via ultrasonic spray pyrolysis route.

    PubMed

    Honda, Michiyo; Kikushima, Koichi; Kawanobe, Yusuke; Konishi, Toshiisa; Mizumoto, Minori; Aizawa, Mamoru

    2012-12-01

    The influence of silicon-substituted hydroxyapatite (Si-HAp) on osteogenic differentiation was assessed by biological analysis. Si-HAp was prepared by ultrasonic spray pyrolysis (USSP) technique using various amounts of Si (0, 0.8, and 1.6 mass%). Chemical analysis revealed that Si was incorporated into the hydroxyapatite (HAp) lattice with no other crystalline phase and which caused the change of crystal structure. Biological analyses showed that the Si contents affected the cell proliferation and morphology, suggesting that there is an optimal Si content for cell culture. As for differentiation, alkaline phosphatase activity and osteocalcin production of Si-HAp were higher than those of HAp. Gene expression profiles also revealed that substitution of Si (0.8 mass%) up-regulated the expression levels of osteocalcin and especially Runx2, a master gene for osteoblast development. These results suggest that incorporating Si into the HAp lattice may enhance the bioactivity, particularly during early osteoblast development.

  11. Catalytic properties of mesoporous Al–La–Mn oxides prepared via spray pyrolysis

    SciTech Connect

    Kim, Goun; Jung, Kyeong Youl; Lee, Choul-Ho; Han, Jeong-Sik; Jeong, Byung-Hun; Park, Young-Kwon; Jeon, Jong-Ki

    2016-10-15

    Highlights: • Al–La–Mn oxides were prepared using spray pyrolysis. • Al–La–Mn oxides exhibit large and uniform pore sizes. • Mesoporous Al–La–Mn oxides were compared with those prepared by conventional precipitation. • Mesoporous Al–La–Mn oxides show superior activity in decomposition of hydrogen peroxide. - Abstract: Mesoporous Al–La–Mn oxides are prepared via spray pyrolysis and are applied to the catalytic decomposition of hydrogen peroxide. The characteristics of the mesoporous Al–La–Mn oxides are examined using N{sub 2} adsorption, X-ray diffraction, and X-ray fluorescence measurements. The surface area and pore size of the Al–La–Mn oxides prepared via spray pyrolysis are larger than those of the Al–La–Mn oxides prepared using a precipitation method. The catalytic performance of the materials during the decomposition of hydrogen peroxide is examined in a pulse-injection reactor. It is confirmed that the mesoporous Al–La–Mn oxides prepared via spray pyrolysis exhibit higher catalytic activity and stability in the decomposition of hydrogen peroxide than Al–La–Mn oxides prepared using a conventional precipitation method.

  12. Preparation of NiO-CuO-MgO fine powders by ultrasonic spray pyrolysis for carbon nanofibers synthesis

    NASA Astrophysics Data System (ADS)

    Krasnikova, Irina V.; Mishakov, Ilya V.; Bauman, Yury I.; Karnaukhov, Timofey M.; Vedyagin, Aleksey A.

    2017-09-01

    Carbon nanofibers with uniform diameter distribution are of great importance to be applied in composite materials production. Characteristics of the final carbon product obtained via catalytic chemical vapour deposition are known to be determined by the catalyst characteristics and the process conditions. In this work, ultrasonic spray pyrolysis was used for the preparation of uniform-sized NiO-CuO-MgO fine powders. Spherical particles of 170-340 nm in diameter were obtained in a temperature range of 400-600 °C. Synthesized powders exhibited high catalytic activity in CCVD of ethylene with the formation of CNF with relatively narrow diameter distribution (60 ± 20 nm).

  13. Method to synthesize and produce thin films by spray pyrolysis

    DOEpatents

    Squillante, Michael R.

    1982-06-22

    Forming a film by spraying onto a heated substrate an atomized solution containing the appropriate salt of a constituent element of the film and a highly soluble (i.e., greater than 1 M) organic acid in sufficient amount to reduce the oxidation state of at least one solute element of the spray solution after contacting the heated substrate.

  14. Corrosion resistance of zirconium oxynitride coatings deposited via DC unbalanced magnetron sputtering and spray pyrolysis-nitriding

    NASA Astrophysics Data System (ADS)

    Cubillos, G. I.; Bethencourt, M.; Olaya, J. J.

    2015-02-01

    ZrOxNy/ZrO2 thin films were deposited on stainless steel using two different methods: ultrasonic spray pyrolysis-nitriding (SPY-N) and the DC unbalanced magnetron sputtering technique (UBMS). Using the first method, ZrO2 was initially deposited and subsequently nitrided in an anhydrous ammonia atmosphere at 1023 K at atmospheric pressure. For UBMS, the film was deposited in an atmosphere of air/argon with a Φair/ΦAr flow ratio of 3.0. Structural analysis was carried out through X-ray diffraction (XRD), and morphological analysis was done through scanning electron microscopy (SEM) and atomic force microscopy (AFM). Chemical analysis was carried out using X-ray photoelectron spectroscopy (XPS). ZrOxNy rhombohedral polycrystalline film was produced with spray pyrolysis-nitriding, whereas using the UBMS technique, the oxynitride films grew with cubic Zr2ON2 crystalline structures preferentially oriented along the (2 2 2) plane. Upon chemical analysis of the surface, the coatings exhibited spectral lines of Zr3d, O1s, and N1s, characteristic of zirconium oxynitride/zirconia. SEM analysis showed the homogeneity of the films, and AFM showed morphological differences according to the deposition technique of the coatings. Zirconium oxynitride films enhanced the stainless steel's resistance to corrosion using both techniques. The protective efficacy was evaluated using electrochemical techniques based on linear polarization (LP). The results indicated that the layers provide good resistance to corrosion when exposed to chloride-containing media.

  15. Effect of solvent composition on oxide morphology during flame spray pyrolysis of metal nitrates.

    PubMed

    Strobel, Reto; Pratsinis, Sotiris E

    2011-05-28

    The effect of solvent composition on particle formation during flame spray pyrolysis of inexpensive metal-nitrates has been investigated for alumina, iron oxide, cobalt oxide, zinc oxide and magnesium oxide. The as-prepared materials were characterized by electron microscopy, nitrogen adsorption, X-ray diffraction (XRD) and disc centrifugation (XDC). The influence of solvent parameters such as boiling point, combustion enthalpy and chemical reactivity on formation of either homogeneous nanoparticles by evaporation/nucleation/coagulation (gas-to-particle conversion) or large particles through precipitation and conversion within the sprayed droplets (droplet-to-particle conversion) is discussed. For Al(2)O(3), Fe(2)O(3), Co(3)O(4) and partly also MgO, the presence of a carboxylic acid in the FSP solution resulted in homogeneous nanoparticles. This is attributed to formation of volatile metal carboxylates in solution as evidenced by attenuated total reflectance spectroscopy (ATR). For ZnO and MgO rather homogeneous nanoparticles were formed regardless of solvent composition. For ZnO this is attributed to its relatively low dissociation temperature compared to other oxides. While for MgO this is traced to the high decomposition temperature of Mg(NO(3))(2) together with Mg(OH)(2)↔MgO transformations. Cobalt oxide (Co(3)O(4)) nanoparticles made by FSP were not aggregated but rather loosely agglomerated as determined by the excellent agreement between XRD- and XDC-derived crystallite and particle sizes, respectively, pointing out the potential of FSP to make non-aggregated particles.

  16. Method to synthesize and produce thin films by spray pyrolysis

    DOEpatents

    Turcotte, Richard L.

    1982-07-06

    Forming a film by spraying onto a heated substrate an atomized solution containing the appropriate salt of a constituent element of the film and a reducing agent at a concentration greater than 1 M and greater than 10 times the stoichiometric amount of reducing agent.

  17. Synthesis of Li₂Ti₃O₇ Anode Materials by Ultrasonic Spray Pyrolysis and Their Electrochemical Properties.

    PubMed

    Ogihara, Takashi; Kodera, Takayuki

    2013-06-03

    Ramsdellite-type lithium titanate (Li₂Ti₃O₇) powders were synthesized by performing ultrasonic spray pyrolysis, and their chemical and physical properties were characterized by performing Scanning Electron Microscope (SEM), powder X-ray Diffraction (XRD), and Inductively Coupled Plasma (ICP) analyses. The as-prepared Li₂Ti₃O₇ precursor powders had spherical morphologies with hollow microstructures, but an irregularly shaped morphology was obtained after calcination above 900 °C. The ramsdellite Li₂Ti₃O₇ crystal phase was obtained after the calcination at 1100 °C under an argon/hydrogen atmosphere. The first rechargeable capacity of the Li₂Ti₃O₇ anode material was 168 mAh/g at 0.1 C and 82 mAh/g at 20 C, and the discharge capacity retention ratio was 99% at 1 C after the 500th cycle. The cycle performance of the Li₂Ti₃O₇ anode was also highly stable at 50 °C, demonstrating the superiority of Li₂Ti₃O₇ anode materials reported previously.

  18. Hydrophilic CdSe thin films by low cost spray pyrolysis technique and annealing effects

    NASA Astrophysics Data System (ADS)

    Logu, T.; Sankarasubramanian, K.; Soundarrajan, P.; Sethuraman, K.

    2015-03-01

    Cadmium selenide (CdSe) thin films were deposited on glass substrates at 200°C by homemade chemical spray pyrolysis technique. The as-deposited films were annealed in air atmosphere for 3 hrs, at two different temperatures (350 and 450°C). The as-deposited film has been observed to possess uniform surface with crystalline sphalerite cubic structure and optical band gap of E g = 2.4 eV. It is worth noting that after annealing, metastable cubic sphalerite phase transforms into stable well crystalline hexagonal wurtzite phase. The optical band gap was found to decrease from 2.4 eV to 1.75 eV. The average surface roughness is 1.5 nm for the as-deposited film which rises to 4.2 nm after annealing the film in air atmosphere. The contact angle was found to vary from 94° ± 1° to 81° ± 1° with annealing temperature. In addition, from Wenzel's relation it is concluded that CdSe thin film is hydrophilic in nature. [Figure not available: see fulltext.

  19. CTAB assisted growth and characterization of nanocrystalline CuO films by ultrasonic spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Singh, Iqbal; Kaur, Gursharan; Bedi, R. K.

    2011-09-01

    An aqueous solution of cupric nitrate trihydrate (Cu(NO 3) 2·3H 2O) modified with cetyltrimetylammonium bromide (CTAB) is used to deposit CuO films on glass substrate by chemical spray pyrolysis technique. The thermal analysis shows that the dried CTAB doped precursor decomposes by an exothermic reaction and suggests that minimum substrate temperature for film deposition should be greater than 270 °C. X-ray diffraction (XRD) studies indicate the formation of monoclinic CuO with preferential orientation along (0 0 2) plane for all film samples. The CTAB used as cationic surfactant in precursor results in the suppression of grain growth in films along the (1 1 0), (0 2 0) and (2 2 0) crystal planes of CuO. Surfactant modified films showed an increase in crystallite size of 14 nm at substrate temperature of 300 °C. The scanning electron micrographs (FESEM) confirm the uniform distribution of facets like grains on the entire area of substrate. CTAB modified films show a significant reduction in the particle agglomeration. Electrical studies of the CuO films deposited at substrate temperature of 300 °C with and without surfactant reveal that the CTAB doping increase the activation energy of conduction by 0.217 eV and room temperature response to ammonia by 9%. The kinetics of the ammonia gas adsorption on the film surface follows the Elovich and Diffusion models.

  20. Additives initiate selective production of chemicals from biomass pyrolysis.

    PubMed

    Leng, Shuai; Wang, Xinde; Wang, Lei; Qiu, Huizhe; Zhuang, Guilin; Zhong, Xing; Wang, Jianguo; Ma, Fengyun; Liu, Jingmei; Wang, Qiang

    2014-03-01

    To improve chemicals selectivity under low temperature, a new method that involves the injection of additives into biomass pyrolysis is introduced. This method allows biomass pyrolysis to achieve high selectivity to chemicals under low temperature (300°C), while nothing was obtained in typical pyrolysis under 300°C. However, by using the new method, the first liquid drop emerged at the interval between 140°C and 240°C. Adding methanol to mushroom scrap pyrolysis obtained high selectivity to acetic acid (98.33%), while adding ethyl acetate gained selectivity to methanol (65.77%) in bagasse pyrolysis and to acetone (72.51%) in corncob pyrolysis. Apart from basic chemicals, one high value-added chemical (2,3-dihydrobenzofuran) was also detected, which obtained the highest selectivity (10.33%) in corncob pyrolysis through the addition of ethyl acetate. Comparison of HZSM-5 and CaCO3 catalysis showed that benzene emerged in the liquid because of the larger degree of cracking and hydrodeoxygenation over HZSM-5.

  1. High-rate production of functional nanostructured films and devices by coupling flame spray pyrolysis with supersonic expansion.

    PubMed

    Wegner, K; Vinati, S; Piseri, P; Antonini, A; Zelioli, A; Barborini, E; Ducati, C; Milani, P

    2012-05-11

    The fabrication of functional thin films and devices by direct deposition of nanoparticles from the gas phase is a promising approach enabling, for instance, the integration of complex analytical and sensing capabilities on microfabricated platforms. Aerosol-based techniques ensure large-scale nanoparticle production and they are potentially suited for this goal. However, they are not adequate in terms of fine control over the lateral resolution of the coatings, mild processing conditions (avoiding high temperature and aggressive chemicals), low contamination and compatibility with microfabrication processes. Here we report the high-rate and efficient production of functional nanostructured films by nanoparticle assembling obtained by the combination of flame spray pyrolysis and supersonic expansion. Our approach merges the advantages of flame spray pyrolysis for bulk nanopowders such as process stability and wide material library availability with those of supersonic cluster beam deposition in terms of lateral resolution and of direct integration of nanomaterials on devices. We efficiently produced nanostructured films and devices (such as gas sensors) using metal oxide, pure noble metal and oxide-supported noble metal nanoparticles.

  2. Macro controlling of copper oxide deposition processes and spray mode by using home-made fully computerized spray pyrolysis system

    NASA Astrophysics Data System (ADS)

    Essa, Mohammed Sh.; Chiad, Bahaa T.; Shafeeq, Omer Sh.

    2017-09-01

    Thin Films of Copper Oxide (CuO) absorption layer have been deposited using home-made Fully Computerized Spray Pyrolysis Deposition system FCSPD on glass substrates, at the nozzle to substrate distance equal to 20,35 cm, and computerized spray mode (continues spray, macro-control spray). The substrate temperature has been kept at 450 °c with the optional user can enter temperature tolerance values ± 5 °C. Also that fixed molar concentration of 0.1 M, and 2D platform speed or deposition platform speed of 4mm/s. more than 1000 instruction program code, and specific design of graphical user interface GUI to fully control the deposition process and real-time monitoring and controlling the deposition temperature at every 200 ms. The changing in the temperature has been recorded during deposition processes, in addition to all deposition parameters. The films have been characterized to evaluate the thermal distribution over the X, Y movable hot plate, the structure and optical energy gap, thermal and temperature distribution exhibited a good and uniform distribution over 20 cm2 hot plate area, X-ray diffraction (XRD) measurement revealed that the films are polycrystalline in nature and can be assigned to monoclinic CuO structure. Optical band gap varies from 1.5-1.66 eV depending on deposition parameter.

  3. Fates of Chemical Elements in Biomass during Its Pyrolysis.

    PubMed

    Liu, Wu-Jun; Li, Wen-Wei; Jiang, Hong; Yu, Han-Qing

    2017-05-10

    Biomass is increasingly perceived as a renewable resource rather than as an organic solid waste today, as it can be converted to various chemicals, biofuels, and solid biochar using modern processes. In the past few years, pyrolysis has attracted growing interest as a promising versatile platform to convert biomass into valuable resources. However, an efficient and selective conversion process is still difficult to be realized due to the complex nature of biomass, which usually makes the products complicated. Furthermore, various contaminants and inorganic elements (e.g., heavy metals, nitrogen, phosphorus, sulfur, and chlorine) embodied in biomass may be transferred into pyrolysis products or released into the environment, arousing environmental pollution concerns. Understanding their behaviors in biomass pyrolysis is essential to optimizing the pyrolysis process for efficient resource recovery and less environmental pollution. However, there is no comprehensive review so far about the fates of chemical elements in biomass during its pyrolysis. Here, we provide a critical review about the fates of main chemical elements (C, H, O, N, P, Cl, S, and metals) in biomass during its pyrolysis. We overview the research advances about the emission, transformation, and distribution of elements in biomass pyrolysis, discuss the present challenges for resource-oriented conversion and pollution abatement, highlight the importance and significance of understanding the fate of elements during pyrolysis, and outlook the future development directions for process control. The review provides useful information for developing sustainable biomass pyrolysis processes with an improved efficiency and selectivity as well as minimized environmental impacts, and encourages more research efforts from the scientific communities of chemistry, the environment, and energy.

  4. A newly designed ultrasonic spray pyrolysis device to fabricate YBCO tapes

    NASA Astrophysics Data System (ADS)

    Liu, M.; Zhou, M. L.; Zhai, L. H.; Liu, D. M.; Gao, X.; Liu, W.

    2003-04-01

    A newly designed ultrasonic spray pyrolysis device has been manufactured to fabricate YBCO tapes. The apparatus is primarily composed of four zones: the ultrasonic generator, the atomization chamber, the pyrolysis chamber and the rotating equipment. Every part of them is designed and fabricated by us. The whole system costs far less than the ready-made equipment facility in which there is always a vacuum apparatus. This apparatus with processing parameters accurately controlled can fabricate short and long YBCO tapes. In this paper, we mainly focused on how to design and manufacture four parts of the ultrasonic spray pyrolysis. We have deposited c-axis aligned short YBCO tapes on biaxially textured Ag {1 1 0}<1 1 0> substrates with Jc=10 3 A/cm 2 using this method with our device. The method is very promising in terms of its precise control of metal compositions, high deposition rate and low cost non-vacuum approach. Improvements of this technique are being carried out to fabricate long YBCO tapes.

  5. Some physical parameters of CuInGaS2 thin films deposited by spray pyrolysis for solar cells

    NASA Astrophysics Data System (ADS)

    Kotbi, Ahmed; Hartiti, Bouchaib; Fadili, Salah; Ridah, Abderraouf; Thevenin, Philippe

    2017-05-01

    Copper-indium-gallium-disulphide (CuInGaS2) is a promising absorber material for thin film photovoltaic. In this paper, CuInGaS2 (CIGS) thin films have been prepared by chemical spray pyrolysis method onto glass substrates at ambient atmosphere. Structural, morphological, optical and electrical properties of CuInGaS2 films were analysed by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), UV-Vis spectrophotometer and Hall Effect measurement, respectively. The films exhibited single phase chalcopyrite structure. The strain and dislocation density decreased with increase of spray time. The grain size of the films increased from 4.45 to 9.01 nm with increase of spray time. The Raman spectrum indicated the presence of the principal chalcopyrite peak at 295 cm^{-1}. The optical properties of the synthesized films have been carried out through the measurement of the absorbance spectrum. The optical band gap was estimated by the absorption spectrum fitting (ASF) method. For each sample, the width of the band tail (E_Tail) of CuInGaS2 thin films was determined. The resistivity (ρ), conductivity (σ), mobility (μ), carrier concentration and conduction type of the films were determined using Hall Effect measurements. The interesting optical properties of CuInGaS2 make them an attractive material for photovoltaic devices.

  6. Sb2S3 grown by ultrasonic spray pyrolysis and its application in a hybrid solar cell

    PubMed Central

    Katerski, Atanas; Oja Acik, Ilona; Mere, Arvo; Mikli, Valdek; Krunks, Malle

    2016-01-01

    Chemical spray pyrolysis (CSP) is a fast wet-chemical deposition method in which an aerosol is guided by carrier gas onto a hot substrate where the decomposition of the precursor chemicals occurs. The aerosol is produced using an ultrasonic oscillator in a bath of precursor solution and guided by compressed air. The use of the ultrasonic CSP resulted in the growth of homogeneous and well-adhered layers that consist of submicron crystals of single-phase Sb2S3 with a bandgap of 1.6 eV if an abundance of sulfur source is present in the precursor solution (SbCl3/SC(NH2)2 = 1:6) sprayed onto the substrate at 250 °C in air. Solar cells with glass-ITO-TiO2-Sb2S3-P3HT-Au structure and an active area of 1 cm2 had an open circuit voltage of 630 mV, short circuit current density of 5 mA/cm2, a fill factor of 42% and a conversion efficiency of 1.3%. Conversion efficiencies up to 1.9% were obtained from solar cells with smaller areas. PMID:28144515

  7. Sb2S3 grown by ultrasonic spray pyrolysis and its application in a hybrid solar cell.

    PubMed

    Kärber, Erki; Katerski, Atanas; Oja Acik, Ilona; Mere, Arvo; Mikli, Valdek; Krunks, Malle

    2016-01-01

    Chemical spray pyrolysis (CSP) is a fast wet-chemical deposition method in which an aerosol is guided by carrier gas onto a hot substrate where the decomposition of the precursor chemicals occurs. The aerosol is produced using an ultrasonic oscillator in a bath of precursor solution and guided by compressed air. The use of the ultrasonic CSP resulted in the growth of homogeneous and well-adhered layers that consist of submicron crystals of single-phase Sb2S3 with a bandgap of 1.6 eV if an abundance of sulfur source is present in the precursor solution (SbCl3/SC(NH2)2 = 1:6) sprayed onto the substrate at 250 °C in air. Solar cells with glass-ITO-TiO2-Sb2S3-P3HT-Au structure and an active area of 1 cm(2) had an open circuit voltage of 630 mV, short circuit current density of 5 mA/cm(2), a fill factor of 42% and a conversion efficiency of 1.3%. Conversion efficiencies up to 1.9% were obtained from solar cells with smaller areas.

  8. Preparation of oxide particles with ordered macropores by colloidal templating and spray pyrolysis

    SciTech Connect

    Abdullah, Mikrajuddin; Iskandar, Ferry; Shibamoto, Shinji; Ogi, Takashi; Okuyama, Kikuo . E-mail: okuyama@hiroshima-u.ac.jp

    2004-10-04

    Silicon dioxide, titanium dioxide, aluminium dioxide, zirconium dioxide, and yttrium dioxide particles containing macropores with ordered, hexagonal closed packing structures were produced by spray pyrolysis. A mixture of a solution of the oxide source (nitrous metal) and a colloid comprised of polystyrene latex (PSL) particles was used. The process involved initial drying at low temperature to evaporate the solvent, followed by drying at high temperature to permit the pyrolysis reaction to occur and to decompose the PSL beads. This takes place in a vertical reactor and requires around 1-2 s. This method can, in principle, be used to produce various types of oxide particles containing ordered pores. It allows easy control of the particle size, pore size and space, and the porosity of particles. Bragg reflection of the powdered material was observed under ultraviolet irradiation.

  9. Selectivity Enhancement by Using Double-Layer MOX-Based Gas Sensors Prepared by Flame Spray Pyrolysis (FSP).

    PubMed

    Rebholz, Julia; Grossmann, Katharina; Pham, David; Pokhrel, Suman; Mädler, Lutz; Weimar, Udo; Barsan, Nicolae

    2016-09-06

    Here we present a novel concept for the selective recognition of different target gases with a multilayer semiconducting metal oxide (SMOX)-based sensor device. Direct current (DC) electrical resistance measurements were performed during exposure to CO and ethanol as single gases and mixtures of highly porous metal oxide double- and single-layer sensors obtained by flame spray pyrolysis. The results show that the calculated resistance ratios of the single- and double-layer sensors are a good indicator for the presence of specific gases in the atmosphere, and can constitute some building blocks for the development of chemical logic devices. Due to the inherent lack of selectivity of SMOX-based gas sensors, such devices could be especially relevant for domestic applications.

  10. Effect of Sm doping on the physical properties of ZnO thin films deposited by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Velusamy, P.; Babu, R. Ramesh; Aparna, K. T.

    2017-05-01

    Undoped and Sm doped ZnO thin films have been prepared by chemical spray pyrolysis method on a glass substrate at 430°C. The physical properties of undoped and Sm doped ZnO thin films are characterized by XRD, FE-SEM, UV-VIS spectroscopy, Hall measurement and PL analysis. XRD pattern reveals that all the films are polycrystalline nature. The FE-SEM study of CdO shows the smooth and uniform surface with the spherical shaped particle. The electrical study reveals the n-type semiconductor and the optical study shows that Sm doped ZnO thin films about 92% transparency and optical band gap vary between 3.266-3.276 eV. Sm doped ZnO thin films have strong green emission behavior.

  11. Selectivity Enhancement by Using Double-Layer MOX-Based Gas Sensors Prepared by Flame Spray Pyrolysis (FSP)

    PubMed Central

    Rebholz, Julia; Grossmann, Katharina; Pham, David; Pokhrel, Suman; Mädler, Lutz; Weimar, Udo; Barsan, Nicolae

    2016-01-01

    Here we present a novel concept for the selective recognition of different target gases with a multilayer semiconducting metal oxide (SMOX)-based sensor device. Direct current (DC) electrical resistance measurements were performed during exposure to CO and ethanol as single gases and mixtures of highly porous metal oxide double- and single-layer sensors obtained by flame spray pyrolysis. The results show that the calculated resistance ratios of the single- and double-layer sensors are a good indicator for the presence of specific gases in the atmosphere, and can constitute some building blocks for the development of chemical logic devices. Due to the inherent lack of selectivity of SMOX-based gas sensors, such devices could be especially relevant for domestic applications. PMID:27608028

  12. Synthesis of In2S3 thin films by spray pyrolysis from precursors with different [S]/[In] ratios

    NASA Astrophysics Data System (ADS)

    Sall, Thierno; Nafidi, A.; Marí Soucase, Bernabé; Mollar, Miguel; Hartitti, Bouchaib; Fahoume, Mounir

    2014-06-01

    Indium sulfide (In2S3) thin films were prepared by chemical spray pyrolysis technique from solutions with different [S]/[In] ratios on glass substrates at a constant temperature of 250 °C. Thin films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-ray spectroscopy (EDS), Raman spectroscopy and optical transmittance spectroscopy. All samples exhibit a polycrystalline structure with a preferential orientation along (0, 0, 12). A good stoichiometry was attained for all samples. The morphology of thin film surfaces, as seen by SEM, was dense and no cracks or pinholes were observed. Raman spectroscopy analysis shows active modes belonging to β-ln2S3 phase. The optical transmittance in the visible range is higher than 60% and the band gap energy slightly increases with the sulfur to indium ratio, attaining a value of 2.63 eV for [S]/[In] = 4.5.

  13. Characterization of Al/Al 2O 3/NiO x solar absorber obtained by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Ienei, Elena; Isac, Luminita; Cazan, Cristina; Duta, Anca

    2010-11-01

    The aim of this paper is to obtain high efficient and inexpensive spectral selective solar absorbers, for solar thermal flat plat collectors using a simple technique - spray pyrolysis deposition (SPD). To achieve maximum solar absorptance and minimum thermal emittance, the following parameters are optimized: the precursor solution concentration and composition, substrate temperature and annealing treatment. The structural and morphological properties of the films were investigated by X-ray diffraction, atomic force microscopy and contact angle measurements. The thermal emittance and solar absorptance of as-deposited films were correlated with the chemical composition, crystalline structure and morphology. The results prove that coatings with excellent spectral selective properties (normal solar absorptance of 0.92 and a normal thermal emittance of 0.03) can be obtained by SPD.

  14. Effect of aluminium doping on zinc oxide thin films grown by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Manouni, A. El; Manjón, F. J.; Mollar, M.; Marí, B.; Gómez, R.; López, M. C.; Ramos-Barrado, J. R.

    2006-01-01

    We report the structural, optical, and electrical characterization of aluminium-doped zinc oxide thin films grown by the spray pyrolysis method. We report the effect of Al concentration on the resistivity and on the X-ray diffraction, transmittance, photoluminescence and Raman scattering spectra of the films. The minimum resistivity is obtained for the sample with nominal Al concentration of 1%. An increase of the Al doping decreases the quality of the films. The loss of short-range order affects the photoluminescence and resistivity, although the optical transmittance is good, and the decrease of the long-range order affects X-ray diffraction and Raman spectra.

  15. Effect of thermal annealing on ZnO:Al thin films grown by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    El Manouni, A.; Manjón, F. J.; Perales, M.; Mollar, M.; Marí, B.; Lopez, M. C.; Ramos Barrado, J. R.

    2007-07-01

    We report the effect of thermal annealing in air on the structural and optical properties of undoped and aluminium-doped (1%-4%) zinc oxide (AZO) thin films, grown by the spray pyrolysis technique on quartz substrates. Films were characterized by X-ray diffraction, low-temperature photoluminescence, electrical resistivity, and Raman spectroscopy after annealing at temperatures between 500 and 900 ∘C. Annealing in air improves the long-range order crystalline quality of the bulk crystals, but promotes a number of point defects in the surface affecting both the resistivity and the photoluminescence.

  16. Atmospheric growth of ZnO films deposited by spray pyrolysis using diethylzinc solution

    NASA Astrophysics Data System (ADS)

    Imai, Masato; Watanabe, Marin; Mochihara, Akiko; Tominaga, Himeka; Yoshino, Kenji; Shen, Qing; Toyoda, Taro; Hayase, Shuzi

    2017-06-01

    Non-doped ZnO thin films are deposited on glass substrates by spray pyrolysis using diethylzinc solution at a range from a room temperature to 150 °C while making N2 gas flow in atmospheric pressure. The morphology, the structural property, the density and the optical band gap are studied. As the deposition temperature is increasing, the overall density and the optical band gap approach to the values of ZnO single crystal. The quality of ZnO thin film deposited at 150 °C becomes near ZnO single crystal.

  17. Study of photoconductivity in Ni doped CdS thin films prepared by spray pyrolysis technique

    SciTech Connect

    Patidar, Manju Mishra Gangrade, Mohan; Nath, R.; Ganesan, V.; Ajay, Akhil; Wala, Arwa Dewas; N, Kiran; Panda, Richa

    2014-04-24

    Ni-doped cadmium sulphide [Cd{sub 1−x}Ni{sub x}S, (x=0, 0.03, 0.05 and 0.20)] thin films were investigated for photoconductive properties. The films were prepared by spray Pyrolysis technique (SPT). AFM and two probe resistivity measurements were carried out to analyze the morphological and electrical properties of the films. AFM shows the note worthy changes in the morphology where the nanorod structures in CdS is changed into nano particles with the Ni doping. The presence of persistence photo current is demonstrated and extensive photoconductivity analysis has been studied on these films.

  18. Achieving Low-Electrical-Resistance WO3:Li Nanostructured Thin Films Using Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Asghari, Zahra; Eshghi, Hosein

    2017-03-01

    We have grown 1 wt.%, 5 wt.%, and 10 wt.% Li-doped tungsten oxide thin films on glass substrate using the spray pyrolysis technique and investigated their morphological, structural, optical, and electrical properties. In addition to formation of nanograin coverage, we found that the doped films grew with polycrystalline monoclinic structure having preferred orientation along (200) plane instead of the amorphous undoped structure. The 10 wt.%-doped sample showed the highest visible transmittance (˜95%) and lowest resistivity (˜7.5 Ω cm), together with relatively high ultraviolet (UV) photoluminescence emission at room temperature.

  19. Electrical properties of transparent conductive ATO coatings obtained by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Zinchenko, T. O.; Kondrashin, V. I.; Pecherskaya, E. A.; Kozlyakov, A. S.; Nikolaev, K. O.; Shepeleva, J. V.

    2017-08-01

    Transparent conductive coatings based on thin films of metal oxides have been widely spread in various optoelectronic devices and appliances. It is necessary to determine the influence of preparation conditions on coatings properties for their use in the solution of certain tasks. Thin films of tin dioxide were obtained by the method of spray pyrolysis on glass substrates. Surface resistance and resistivity, concentration and mobility of charge carriers, the conductivity were measured, and the dependences showing the effect of preparation conditions on electrical properties of optically transparent coatings.

  20. Hydroxyapatite forming ability of electrostatic spray pyrolysis derived calcium phosphate nano powder.

    PubMed

    Hwang, Kyu-Seog; Jeon, Kyung-Ok; Jeon, Young-Sun; Kim, Byung-Hoon

    2007-04-01

    A novel fabrication technique, i.e., electrostatic spray pyrolysis (ESP), has been used in this study to prepare calcium phosphate nano powders. Final annealing was done at 400 degrees C for 30 min in air. The hydroxyapatite-forming ability of the annealed powder has been investigated in Eagle's minimum essential medium solution. X-ray diffracton, field emission scanning electron microscope, energy dispersive X-ray spectroscope, and Fourier transform infrared spectroscope were employed to characterize the annealed powders after immersion. The powder with an amorphous structure induced hydroxyapatite formation on their surfaces after immersion for 15 days.

  1. Structural and optical characterization of InAs nanocrystals deposited by spray pyrolysis

    SciTech Connect

    Mousa, A. M. Mohammed, M. A.; Kadhim, R.

    2015-03-30

    4-5 nm size InAs nanocrystals were prepared by spray pyrolysis technique on glass substrates from alkaline solution containing InCl{sub 3} and As{sub 2}O. X-Ray diffraction and absorption spectra suggested that the deposition conditions (deposition time and temperature) had a profound influence on the structure and thickness of deposited layers. The optical absorption band edges shifted to lower energy when increasing the thickness with respect to the bulk material. The marked blue shift of the optical absorption edge indicated a strong quantum confinement effect in InAs films.

  2. Achieving Low-Electrical-Resistance WO3:Li Nanostructured Thin Films Using Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Asghari, Zahra; Eshghi, Hosein

    2016-12-01

    We have grown 1 wt.%, 5 wt.%, and 10 wt.% Li-doped tungsten oxide thin films on glass substrate using the spray pyrolysis technique and investigated their morphological, structural, optical, and electrical properties. In addition to formation of nanograin coverage, we found that the doped films grew with polycrystalline monoclinic structure having preferred orientation along (200) plane instead of the amorphous undoped structure. The 10 wt.%-doped sample showed the highest visible transmittance (˜95%) and lowest resistivity (˜7.5 Ω cm), together with relatively high ultraviolet (UV) photoluminescence emission at room temperature.

  3. Properties of mixed molybdenum oxide iridium oxide thin films synthesized by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Patil, P. S.; Kawar, R. K.; Sadale, S. B.; Inamdar, A. I.; Deshmukh, H. P.

    2006-09-01

    Molybdenum-doped iridium oxide thin films have been deposited onto corning glass- and fluorine-doped tin oxide coated corning glass substrates at 350 °C by using a pneumatic spray pyrolysis technique. An aqueous solution of 0.01 M ammonium molybdate was mixed with 0.01 M iridium trichloride solution in different volume proportions and the resultant solution was used as a precursor solution for spraying. The as-deposited samples were annealed at 600 °C in air medium for 1 h. The structural, electrical and optical properties of as-deposited and annealed Mo-doped iridium oxide were studied and values of room temperature electrical resistivity, and thermoelectric power were estimated. The as-deposited samples with 2% Mo doping exhibit more pronounced electrochromism than other samples, including pristine Ir oxide.

  4. In-situ fabrication of nanostructured cobalt oxide powders by spray pyrolysis technique.

    PubMed

    Zhao, Z W; Konstantinov, K; Yuan, L; Liu, H K; Dou, S X

    2004-09-01

    Nano-crystalline Co3O4 and CoO powders have been prepared by a spray pyrolysis approach. The effects of the reaction temperature and initial salts on the crystallinity and phase composition have been studied. Based on the TEM and XRD results, the crystal sizes were in the range of 1-10 nm. SEM and TEM observations also reveal that the nano-powders easily create micron-scale spherical agglomerates. The Co3O4 powders obtained by spraying nitrate solution at 500 degrees C show high specific surface area, which according to the BET method is 82.37 m2/g. The time/temperature phase diagram of cobalt oxides developed from XRD and DTA/TGA analyses shows the existence of a CoO phase at low and high temperature ranges when some specific preparation conditions are applied.

  5. Decoration of crumpled rGO sheets with Ag nanoparticles by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Papailias, I.; Giannouri, M.; Trapalis, A.; Todorova, N.; Giannakopoulou, T.; Boukos, N.; Lekakou, C.

    2015-12-01

    In this work, crumpled reduced graphene oxide (rGO) nanostructures were produced using spray pyrolysis technique. Graphite oxide (GtO) prepared through a modified Hummers method was used as starting material. Water dispersions of graphene oxide (GO) were prepared and sprayed in a tube furnace at 300 °C, 500 °C and 700 °C using Argon (Ar) as carrier gas. Also, precursor dispersions with different AgNO3 concentrations were processed at the same conditions. During the treatment, the sprayed droplets underwent rapid heating and then gradual cooling until the exit of the oven, where crumpled rGO and Ag/rGO powders were collected. The prepared materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman and FT-IR spectroscopy. It was established that the crumpling of the nanosheets was slightly affected by the increase of the process temperature. Crumpled morphologies were obtained even at low temperature of 300 °C. In contrast, the degree of GO reduction was temperature dependent and increased with the increase of the temperature. The incorporation of Ag nanoparticles was evidenced by the XRD and TEM analysis with the size of the Ag nanoparticles to grow as the concentration of AgNO3 and/or the process temperature increased. SERS effect in the Raman spectra of the Ag/rGO materials was observed that reached a maximum at 500 °C. Spray pyrolysis was suggested as a simple, controllable and scalable route for the instantaneous crumpling, reduction and decoration of GO nanosheets with metal/metal oxide nanoparticles.

  6. Uniform nanoparticles by flame-assisted spray pyrolysis (FASP) of low cost precursors

    NASA Astrophysics Data System (ADS)

    Rudin, Thomas; Wegner, Karsten; Pratsinis, Sotiris E.

    2011-07-01

    A new flame-assisted spray pyrolysis (FASP) reactor design is presented, which allows the use of inexpensive precursors and solvents (e.g., ethanol) for synthesis of nanoparticles (10-20 nm) with uniform characteristics. In this reactor design, a gas-assisted atomizer generates the precursor solution spray that is mixed and combusted with externally fed inexpensive fuel gases (acetylene or methane) at a defined height above the atomizing nozzle. The gaseous fuel feed can be varied to control the combustion enthalpy content of the flame and onset of particle formation. This way, the enthalpy density of the flame is decoupled from the precursor solution composition. Low enthalpy content precursor solutions are prone to synthesis of non-uniform particles (e.g., bimodal particle size distribution) by standard flame spray pyrolysis (FSP) processes. For example, metal nitrates in ethanol typically produce nanosized particles by gas-to-particle conversion along with larger particles by droplet-to-particle conversion. The present FASP design facilitates the use of such low enthalpy precursor solutions for synthesis of homogeneous nanopowders by increasing the combustion enthalpy density of the flame with low-cost, gaseous fuels. The effect of flame enthalpy density on product properties in the FASP configuration is explored by the example of Bi2O3 nanoparticles produced from bismuth nitrate in ethanol. Product powders were characterized by nitrogen adsorption, X-ray diffraction, X-ray disk centrifuge, and transmission electron microscopy. Homogeneous Bi2O3 nanopowders were produced both by increasing the gaseous fuel content and, most notably, by cutting the air entrainment prior to ignition of the spray.

  7. Uniform nanoparticles by flame-assisted spray pyrolysis (FASP) of low cost precursors.

    PubMed

    Rudin, Thomas; Wegner, Karsten; Pratsinis, Sotiris E

    2011-07-01

    A new flame-assisted spray pyrolysis (FASP) reactor design is presented, which allows the use of inexpensive precursors and solvents (e.g., ethanol) for synthesis of nanoparticles (10-20 nm) with uniform characteristics. In this reactor design, a gas-assisted atomizer generates the precursor solution spray that is mixed and combusted with externally fed inexpensive fuel gases (acetylene or methane) at a defined height above the atomizing nozzle. The gaseous fuel feed can be varied to control the combustion enthalpy content of the flame and onset of particle formation. This way, the enthalpy density of the flame is decoupled from the precursor solution composition. Low enthalpy content precursor solutions are prone to synthesis of non-uniform particles (e.g., bimodal particle size distribution) by standard flame spray pyrolysis (FSP) processes. For example, metal nitrates in ethanol typically produce nanosized particles by gas-to-particle conversion along with larger particles by droplet-to-particle conversion. The present FASP design facilitates the use of such low enthalpy precursor solutions for synthesis of homogeneous nanopowders by increasing the combustion enthalpy density of the flame with low-cost, gaseous fuels. The effect of flame enthalpy density on product properties in the FASP configuration is explored by the example of Bi(2)O(3) nanoparticles produced from bismuth nitrate in ethanol. Product powders were characterized by nitrogen adsorption, X-ray diffraction, X-ray disk centrifuge, and transmission electron microscopy. Homogeneous Bi(2)O(3) nanopowders were produced both by increasing the gaseous fuel content and, most notably, by cutting the air entrainment prior to ignition of the spray.

  8. Uniform nanoparticles by flame-assisted spray pyrolysis (FASP) of low cost precursors

    PubMed Central

    Rudin, Thomas; Wegner, Karsten

    2013-01-01

    A new flame-assisted spray pyrolysis (FASP) reactor design is presented, which allows the use of inexpensive precursors and solvents (e.g., ethanol) for synthesis of nanoparticles (10–20 nm) with uniform characteristics. In this reactor design, a gas-assisted atomizer generates the precursor solution spray that is mixed and combusted with externally fed inexpensive fuel gases (acetylene or methane) at a defined height above the atomizing nozzle. The gaseous fuel feed can be varied to control the combustion enthalpy content of the flame and onset of particle formation. This way, the enthalpy density of the flame is decoupled from the precursor solution composition. Low enthalpy content precursor solutions are prone to synthesis of non-uniform particles (e.g., bimodal particle size distribution) by standard flame spray pyrolysis (FSP) processes. For example, metal nitrates in ethanol typically produce nanosized particles by gas-to-particle conversion along with larger particles by droplet-to-particle conversion. The present FASP design facilitates the use of such low enthalpy precursor solutions for synthesis of homogeneous nanopowders by increasing the combustion enthalpy density of the flame with low-cost, gaseous fuels. The effect of flame enthalpy density on product properties in the FASP configuration is explored by the example of Bi2O3 nanoparticles produced from bismuth nitrate in ethanol. Product powders were characterized by nitrogen adsorption, X-ray diffraction, X-ray disk centrifuge, and transmission electron microscopy. Homogeneous Bi2O3 nanopowders were produced both by increasing the gaseous fuel content and, most notably, by cutting the air entrainment prior to ignition of the spray. PMID:23408113

  9. Surfactant-assisted ultrasonic spray pyrolysis of nickel oxide and lithium-doped nickel oxide thin films, toward electrochromic applications

    NASA Astrophysics Data System (ADS)

    Denayer, Jessica; Bister, Geoffroy; Simonis, Priscilla; Colson, Pierre; Maho, Anthony; Aubry, Philippe; Vertruyen, Bénédicte; Henrist, Catherine; Lardot, Véronique; Cambier, Francis; Cloots, Rudi

    2014-12-01

    Lithium-doped nickel oxide and undoped nickel oxide thin films have been deposited on FTO/glass substrates by a surfactant-assisted ultrasonic spray pyrolysis. The addition of polyethylene glycol in the sprayed solution has led to improved uniformity and reduced light scattering compared to films made without surfactant. Furthermore, the presence of lithium ions in NiO films has resulted in improved electrochromic performances (coloration contrast and efficiency), but with a slight decrease of the electrochromic switching kinetics.

  10. Fabrication of solid oxide fuel cell anode electrode by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Liu, Lin; Kim, Gap-Yong; Chandra, Abhijit

    Large triple phase boundaries (TPBs) and high gas diffusion capability are critical in enhancing the performance of a solid oxide fuel cell (SOFC). In this study, ultrasonic spray pyrolysis has been investigated to assess its capability in controlling the anode microstructure. Deposition of porous anode film of nickel and Ce 0.9Gd 0.1O 1.95 on a dense 8 mol.% yttria stabilized zirconia (YSZ) substrate was carried out. First, an ultrasonic atomization model was utilized to predict the deposited particle size. The model accurately estimated the deposited particle size based on the feed solution condition. Second, effects of various process parameters, which included the precursor solution feed rate, precursor solution concentration and deposition temperature, on the TPB formation and porosity were investigated. The deposition temperature and precursor solution concentration were the most critical parameters that influenced the morphology, porosity and particle size of the anode electrode. Ultrasonic spray pyrolysis achieved homogeneous distribution of constitutive elements within the deposited particles and demonstrated capability to control the particle size and porosity in the range of 2-17 μm and 21-52%, respectively.

  11. Analysis of carrier gas flow rate effect on hydroxyapatite particle formation in ultrasonic spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Widiyastuti, W.; Setiawan, Adhi; Nurtono, Tantular; Winardi, Sugeng

    2016-02-01

    Ultrasonic spray pyrolysis has been well-known process for producing fine particles from single and multicomponent materials. Here, the effect of carrier gas flow rate in ultrasonic spray pyrolysis process was studied in the particle formation of hydroxyapatite using solution precursor of Ca(CH3COO)2 and (NH4)2HPO4 with Ca/P ratio of 1.67. The experimental analysis was accompanied with computational fluid dynamics (CFD) simulation for comparison. In the simulation, the evaporation of the solvent in the droplets, a second evaporation due to crust formation, the decomposition reaction of the precursor involving the transfer of heat and mass transfer from droplet to surrounding were considered. By maintaining temperature at 900 °C, the residence time increased with decreasing the carrier gas flow rate led to the increasing the evaporation rate and the reacted fraction of the precursor. The predicted and experimental results of average particles size were agreed well with discrepancy 6.3%.

  12. Electrochemical properties of tungsten sulfide–carbon composite microspheres prepared by spray pyrolysis

    PubMed Central

    Choi, Seung Ho; Boo, Sung Jin; Lee, Jong-Heun; Kang, Yun Chan

    2014-01-01

    Tungsten sulfide (WS2)–carbon composite powders with superior electrochemical properties are prepared by a two-step process. WO3-carbon composite powders were first prepared by conventional spray pyrolysis, and they were then sulfidated to form WS2-carbon powders. Bare WS2 powders are also prepared by sulfidation of bare WO3 powders obtained by spray pyrolysis. Stacked graphitic layers could not be found in the bare WS2 and WS2–carbon composite powders. The amorphous bare WS2 and WS2–carbon composite powders have Brunauer–Emmett–Teller (BET) surface areas of 2.8 and 4 m2 g−1, respectively. The initial discharge and charge capacities of the WS2–carbon composite powders at a current density of 100 mA g−1 are 1055 and 714 mA h g−1, respectively, and the corresponding initial Coulombic efficiency is 68%. On the other hand, the initial discharge and charge capacities of the bare WS2 powders are 514 and 346 mA h g−1, respectively. The discharge capacities of the WS2–carbon composite powders for the 2nd and 50th cycles are 716 and 555 mA h g−1, respectively, and the corresponding capacity retention measured after first cycle is 78%. PMID:25169439

  13. Antimony-Doped Tin Oxide Thin Films Grown by Home Made Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Yusuf, Gbadebo; Babatola, Babatunde Keji; Ishola, Abdulahi Dimeji; Awodugba, Ayodeji O.; Solar cell Collaboration

    2016-03-01

    Transparent conducting antimony-doped tin oxide (ATO) films have been deposited on glass substrates by home made spray pyrolysis technique. The structural, electrical and optical properties of the ATO films have been investigated as a function of Sb-doping level and annealing temperature. The optimum target composition for high conductivity and low resistivity was found to be 20 wt. % SnSb2 + 90 wt. ATO. Under optimized deposition conditions of 450oC annealing temperature, electrical resistivity of 5.2×10-4 Ω -cm, sheet resistance of 16.4 Ω/sq, average optical transmittance of 86% in the visible range, and average optical band-gap of 3.34eV were obtained. The film deposited at lower annealing temperature shows a relatively rough, loosely bound slightly porous surface morphology while the film deposited at higher annealing temperature shows uniformly distributed grains of greater size. Keywords: Annealing, Doping, Homemade spray pyrolysis, Tin oxide, Resistivity

  14. Electrochemical properties of LiNi0.8Co0.2-xAlxO2 (0≤x≤0.1) cathode particles prepared by spray pyrolysis from the spray solutions with and without organic additives

    NASA Astrophysics Data System (ADS)

    Ju, S. H.; Kim, J. H.; Kang, Y. C.

    2010-04-01

    Fine-sized LiNi0.8Co0.2-xAlxO2 (0≤x≤0.1) cathode particles were prepared by spray pyrolysis from the spray solutions with and without organic additives. Citric acid, ethylene glycol, and Drying Control Chemical Additive (DCCA) were used as organic additives and improved the morphologies and electrochemical properties of the cathode particles. The LiNi0.8Co0.2-xAlxO2 (0≤x≤0.1) cathode particles obtained from the spray solutions with organic additives were of micro size and had slightly aggregated morphologies. The initial discharge capacities of the LiNi0.8Co0.2-xAlxO2 (0≤x≤0.1) cathode particles obtained from the spray solutions without organic additive changed from 169 mAhg-1 to 190 mAhg-1 when the x changed from 0 to 0.1. However, the initial discharge capacities of the cathode particles obtained from the spray solutions with organic additives changed from 196 mAhg-1 to 218 mAhg-1. The initial discharge capacity of the LiNi0.8Co0.15Al0.05O2 cathode particles obtained from the spray solution with organic additives was maintained after the 20th cycle at a current density of 0.1 C.

  15. Yolk-shelled cathode materials with extremely high electrochemical performances prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Choi, Seung Ho; Hong, Young Jun; Kang, Yun Chan

    2013-08-01

    A facile, continuous preparation process of yolk-shell-structured lithium-metal oxide powders without a template for use as cathode materials in lithium ion batteries is introduced for the first time. Single and double-shelled LiNi0.5Mn1.5O4 yolk-shell powders as the first target materials are prepared directly by spray pyrolysis from a spray solution with sucrose, at a short residence time of 4 s. Fast combustion and contraction of a carbon-mixed oxide composite intermediate, formed from a micro-sized droplet inside a hot wall reactor maintained at 700 °C, produces the yolk-shell powders. The yolk-shell structure of the precursor powders directly prepared by spray pyrolysis is well maintained even at a high post-treatment temperature of 750 °C. The yolk-shell LiNi0.5Mn1.5O4 powders delivered a 1000th high discharge capacity of 108 mA h g-1 at 10 C. The discharge capacities are as high as 103, 95, and 91 mA h g-1 at extremely high discharge rates of 100, 200, and 300 C and the corresponding specific energy densities are 420, 370, and 328 W h kg-1. The capacity retention at a constant discharge rate of 200 C is 90% after 500 cycles.A facile, continuous preparation process of yolk-shell-structured lithium-metal oxide powders without a template for use as cathode materials in lithium ion batteries is introduced for the first time. Single and double-shelled LiNi0.5Mn1.5O4 yolk-shell powders as the first target materials are prepared directly by spray pyrolysis from a spray solution with sucrose, at a short residence time of 4 s. Fast combustion and contraction of a carbon-mixed oxide composite intermediate, formed from a micro-sized droplet inside a hot wall reactor maintained at 700 °C, produces the yolk-shell powders. The yolk-shell structure of the precursor powders directly prepared by spray pyrolysis is well maintained even at a high post-treatment temperature of 750 °C. The yolk-shell LiNi0.5Mn1.5O4 powders delivered a 1000th high discharge capacity of 108 m

  16. The destruction of halogenated organic chemicals by plasma pyrolysis.

    PubMed

    Barton, T G; Mordy, J A

    1984-08-01

    Very high destruction efficiencies for halogenated chemicals have been achieved by plasma pyrolysis. Destruction efficiencies exceeded 99.9999999% for tests with polychlorinated biphenyls (PCBs). Preliminary tests with tetrachloromethane have obtained destruction efficiencies exceeding 99.99%. The plasma pyrolysis process involved the creation of a 250-kW plasma with a temperature in excess of 25 000 degrees C. The toxic material was injected into the plasma zone at a rate between 1 and 2 L/min. Thermochemical and photochemical dissociation of the toxic materials produced atoms and ions which recombined to form primarily H2, CO, HCl, and particulate carbon. The HCl was neutralized by NaOH. The flaring of the H2 and CO should destroy to a high degree any trace residuals. The application of plasma pyrolysis for the ultimate disposal of toxicological waste was also investigated. Rat carcasses containing mean lethal dosage of PCB were pyrolyzed.

  17. Optical and electrical properties of thin NiO films deposited by reactive magnetron sputtering and spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Parkhomenko, H. P.; Solovan, M. N.; Mostovoi, A. I.; Orletskii, I. G.; Parfenyuk, O. A.; Maryanchuk, P. D.

    2017-06-01

    Thin NiO films are deposited by reactive magnetron sputtering and spray pyrolysis. The main optical constants, i.e., refractive index n(λ), absorption coefficient α(λ), extinction coefficient k(λ), and thickness d, are determined. The temperature dependence of the resistance of thin films is found, and the activation energy of films deposited by different methods is determined.

  18. Characterization and Electrochromic Properties of Vanadium Oxide Thin Films Prepared via Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M.-M.

    2013-08-01

    Vanadium oxide thin films were grown on glass substrates using spray pyrolysis technique. The effects of substrate temperature, vanadium concentration in the initial solution and the solution spray rate on the nanostructural and the electrochromic properties of deposited films are investigated. Characterization and the electrochromic measurements were carried out using X-ray diffraction, scanning electron microscopy and cyclic voltammogram. XRD patterns showed that the prepared films have polycrystalline structure and are mostly mixed phases of orthorhombic α-V2O5 along with minor β-V2O5 and V4O9 tetragonal structures. The preferred orientation of the deposited films was found to be along [101] plane. The cyclic voltammogram results obtained for different samples showed that only the films with 0.2 M solution concentration, 5 ml/min solution spray rate and 450°C substrate temperature exhibit two-step electrochromic properties. The results show a correlation between cycle voltammogram, morphology and resistance of the films.

  19. Properties of NiO thin films deposited by intermittent spray pyrolysis process

    NASA Astrophysics Data System (ADS)

    Reguig, B. A.; Khelil, A.; Cattin, L.; Morsli, M.; Bernède, J. C.

    2007-02-01

    NiO thin films have been grown on glass substrates by intermittent spray pyrolysis deposition of NiCl 2·6H 2O diluted in distilled water, using a simple "perfume atomizer". The effect of the solution molarity on their properties was studied and compared to those of NiO thin films deposited with a classical spray system. It is shown that NiO thin films crystallized in the NiO structure are achieved after deposition. Whatever the precursor molarity, the grain size is around 25-30 nm. The crystallites are preferentially oriented along the (1 1 1) direction. All the films are p-type. However, the thickness and the conductivity of the NiO films depend on the precursor contraction. By comparison with the properties of films deposited by classical spray technique, it is shown that the critical precursor concentration, which induces strong thin films properties perturbations, is higher when a perfume atomizer is used. This broader stability domain can be attributed to better chlorides decomposition during the rest time used in the perfume atomizer technique.

  20. Characterization of CuO Thin Films Deposition on Porous Silicon by Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Khashan, Khawla S.; Hassan, Azhar I.; Addie, Ali J.

    2016-05-01

    CuO thin films on porous silicon (PSi) substrates were prepared via spray pyrolysis method. The structural, optical and electrical properties of the films and the heterojunctions were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscope (AFM) and UV-Vis spectrophotometer. XRD results show that the film is polycrystalline and have a monoclinic crystal structure. Optical measurement indicates that the films had a low transmittance at the visible range and an optical bandgap of 2.2eV. High rectification was achieved with a maximum photoresponsivity of about 0.59A/W at 400nm, so that the CuO/PSi heterojunction may act as a good candidate for the fabrication of an efficient photodiode.

  1. Controlled crystal phase of TiO2 by spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Aji, B. B.; Shih, S. J.; Pradita, T.

    2017-04-01

    TiO2 in powder form was preferred due to its flexibility and easy handling. TiO2 powders with controlled crystal phase were successfully synthesised by ultrasonic spray pyrolysis from titanium tetraisopropoxide (TTIP) precursor. The effect of various acid solvents (nitric acid, acetic acid and citric acid) in relationship with crystal compositions have been well-studied. This experimental study suggested that the ratio of anatase phase achieved from TiO2 prepared by nitric, acid acetic acid and citric acid solvent are 85%, 39% and 27% respectively. Spurs-Myers equation used to determine the anatase-rutile phase. Crystal sizes were calculated using Scherer equation. Both of ratio and crystal size were estimated from corresponding X-ray diffraction pattern. Precipitation and chelating process were the keys to determine the last composition of TiO2.

  2. Synthesis of MgO powder from magnesium nitrate using spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Pradita, T.; Shih, S. J.; Aji, B. B.; Sudibyo

    2017-03-01

    A variety of advantages such as catalyst, paints, flame retardants, semiconductors, additives in refractory and solid adsorbent can be obtained from Magnesium Oxide (MgO) based material. Ultrasonic spray pyrolysis (SP) process was conducted to synthesize MgO from Mg(NO3)2.6H2O (MgN) precursor. The MgO particles were characterized using Thermogravimetric Analysis (TGA), X-Ray Diffraction analysis (XRD) and Field Emission-Secondary Electron Microscopy (FE-SEM). In this study, Hollow spherical and irregular MgO particles were successfully obtained. It suggests that the particle size will decrease along with the increasing of the SP temperature, the smallest particle size obtained is in the range of 354±104 nm at 900°C SP temperature.

  3. The piezoelectric effect on zinc oxide nano on polyimide substrate by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Idris, A. A. M.; Arsat, R.; Ahmad, M. K.

    2017-03-01

    This paper reports the effect of the deposition conditions crystal quality and film thickness of the Zinc Oxide (ZnO) film on the polyimide substrate. The ZnO film has been deposited by using the spray pyrolysis technique. This technique needs Zinc Nitrate Hexahydrate with the mixture of deionized water. At 350 °C, a higher c-axis preferred orientation at peak 0002 crystal orientation, which is critical for piezoelectric applications in ZnO thin films are obtained with the thickness of thin film is 300ηm. It also produces the 204.8 Hz of frequency which is higher than other frequency obtained by lower growth temperature.

  4. Improvement on droplet production rate of ultrasonic - nebulizer in spray pyrolysis process

    NASA Astrophysics Data System (ADS)

    Panatarani, Camellia; Demen, Tuti Aryati; Men, Liu Kin; Maulana, Dwindra Wilham; Hidayat, Darmawan; Joni, I. Made

    2013-09-01

    Atomization is an important part in Spray Pyrolysis (SP) process which is applied to synthesize submicron or nano sized particles or to deposit thin film. Ultrasonic Nebulizer (UN) is usually use in SP due to its homogeneous droplets production with size between 1-5 μm. The drawback of the UN is low droplets production rate. In this research, we successfully developed a Digital Ultrasonic Nebulizer (DUN) with high droplets production rate using two ultrasonic traducers with applied frequency of 2.4 MHz. The result of DUN atomization was improved 4-6 fold compare to the conventional UN. The DUN also has an additional digital features such as pushbutton, LCD and microcontroller which is allow to set duration and applied voltage.

  5. Synthesis of Single Crystalline ZnO Nanoparticles by Salt-Assisted Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Panatarani, Camellia; Lenggoro, I. Wuled; Okuyama, Kikuo

    2003-04-01

    LiNO3 was used as a shield in the preparation of single crystalline ZnO particles by a spray pyrolysis process in order to prevent agglomeration and enhance the crystallinity of the ZnO. LiNO3 was added to a precursor solution of zinc acetate dihydrate prior to its atomization by means of an ultrasonic transducer. Agglomerate-free particles having a mean particle size of 26 nm were successfully obtained after washing the product. X-ray diffractometry, field-emission scanning electron micrograph and transmission electron micrograph data indicate that the size and morphology of ZnO were strongly influenced by the operating temperature used and the residence time of the particle in the reactor.

  6. Polymetallic citric complexes as precursors for spray-pyrolysis deposition of thin ferrite films

    NASA Astrophysics Data System (ADS)

    Milanova, M.; Koleva, I.; Todorovska, R.; Zaharieva, J.; Кostadinov, M.; Todorovsky, D.

    2011-06-01

    Thin films of ferrites of the type M IIFe 2O 4 (M = Cu, Mg, Zn) are prepared by spray-pyrolysis using ethylene glycol solutions of mixed-metal citric complexes of the respective metals at substrate temperature between 350 °C and 450 °C and post-deposition annealing at 480-750 °C in air. Phase composition, crystal structure, morphology and adhesion of the obtained films (40-400 nm in thickness) are studied by X-ray diffraction, SEM, energy dispersive X-ray microanalysis and AFM. Single phase dense uniform films with grains from 30-100 nm (M = Cu, Mg) to 0.15-2 μm (M = Zn) are obtained.

  7. Ultra-low thermal conductivity of nanogranular indium tin oxide films deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Brinzari, Vladimir I.; Cocemasov, Alexandr I.; Nika, Denis L.; Korotcenkov, Ghenadii S.

    2017-02-01

    The authors have shown that nanogranular indium tin oxide (ITO) films, deposited by spray pyrolysis on a silicon substrate, demonstrate ultralow thermal conductivity κ ˜ 0.84 ± 0.12 Wm-1 K-1 at room temperature. This value is approximately by one order of magnitude lower than that in bulk ITO. The strong drop of thermal conductivity is explained by the nanogranular structure and porosity of ITO films, resulting in enhanced phonon scattering on grain boundaries. The experimental results were interpreted theoretically, employing the Boltzmann transport equation approach for phonon transport and filtering model for electronic transport. The calculated values of thermal conductivity are in reasonable agreement with the experimental findings. The presented results show that ITO films with an optimal nanogranular structure may be prospective for thermoelectric applications.

  8. Optoelectronic characteristics of YAG phosphor-incorporated ZnO films deposited by ultrasonic spray pyrolysis

    PubMed Central

    2012-01-01

    This work presents a novel white light device. An yttrium aluminum garnet (YAG) phosphor-incorporated zinc oxide (ZnO) film is deposited on a slide glass substrate by ultrasonic spray pyrolysis. A nanoflower consisting of a hexagonal nanopetal is formed on the surfaces of the samples, and the sizes of the nanopetal are approximately 200 to 700 nm. Additionally, the nanopetal becomes blunted with an increasing incorporated amount of YAG. As the incorporated amount is 1.5 and 2.5 wt.%, the photoluminescence color of the YAG-incorporated ZnO film is nearly white, possibly contributing to the YAG emission and the band-to-deep level transition in the ZnO film. PMID:23151219

  9. Effect of cobalt on the electrochromic properties of NiO films deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Martinez-Luevanos, A.; Oliva, J.; Garcia, C. R.; Avalos-Belmontes, F.; Garcia-Lobato, M. A.

    2017-05-01

    In this work, the morphological, optical and electrochromic properties of NiO and Ni-Co oxides films are reported. Those films were deposited on FTO glass substrates using a simple spray pyrolysis method. SEM images indicated that the size of particles that formed the Ni-Co oxide films decreased from 18 to 6 nm as the content of Co increases. In addition, the thickness of the films decreased from 378 to 310 nm as the content of cobalt augments from 0 to 10 mol%. This reduction of thickness also produced a diminution of the band gap of the films, which benefited the electrochromic properties. Electrochemical measurements were carried out and found that the diffusion coefficient, reversibility and coloration efficiency were enhanced in samples with cobalt with respect to the sample with pure NiO. Thus, the results suggest that our films could be useful for electrochromic applications.

  10. Computational fluid dynamic modeling of the flame spray pyrolysis process for silica nanopowder synthesis

    NASA Astrophysics Data System (ADS)

    Olivas-Martinez, Miguel; Sohn, Hong Yong; Jang, Hee Dong; Rhee, Kang-In

    2015-07-01

    A computational fluid dynamic model that couples the fluid dynamics with various processes involving precursor droplets and product particles during the flame spray pyrolysis (FSP) synthesis of silica nanopowder from volatile precursors is presented. The synthesis of silica nanopowder from tetraethylorthosilicate and tetramethylorthosilicate in bench- and pilot-scale FSP reactors, with the ultimate purpose of industrial-scale production, was simulated. The transport and evaporation of liquid droplets are simulated from the Lagrangian viewpoint. The quadrature method of moments is used to solve the population balance equation for particles undergoing homogeneous nucleation and Brownian collision. The nucleation rate is computed based on the rates of thermal decomposition and oxidation of the precursor with no adjustable parameters. The computed results show that the model is capable of reproducing the magnitude as well as the variations of the average particle diameter with different experimental conditions using a single value of the collision efficiency factor α for a given reactor size.

  11. Solution-based carbohydrate synthesis of individual solid, hollow, and porous carbon nanospheres using spray pyrolysis.

    PubMed

    Wang, Chengwei; Wang, Yuan; Graser, Jake; Zhao, Ran; Gao, Fei; O'Connell, Michael J

    2013-12-23

    A facile and scalable solution-based, spray pyrolysis synthesis technique was used to synthesize individual carbon nanospheres with specific surface area (SSA) up to 1106 m(2)/g using a novel metal-salt catalyzed reaction. The carbon nanosphere diameters were tunable from 10 nm to several micrometers by varying the precursor concentrations. Solid, hollow, and porous carbon nanospheres were achieved by simply varying the ratio of catalyst and carbon source without using any templates. These hollow carbon nanospheres showed adsorption of to 300 mg of dye per gram of carbon, which is more than 15 times higher than that observed for conventional carbon black particles. When evaluated as supercapacitor electrode materials, specific capacitances of up to 112 F/g at a current density of 0.1 A/g were observed, with no capacitance loss after 20,000 cycles.

  12. Properties of antimony doped ZnO thin films deposited by spray pyrolysis technique

    SciTech Connect

    Sadananda Kumar, N. Bangera, Kasturi V.; Shivakumar, G. K.

    2015-07-15

    Antimony (Sb) doped zinc oxide (ZnO) thin films were deposited on the glass substrate at 450°C using spray pyrolysis technique. Effect of Sb doping on surface morphology structural, optical and electrical properties were studied. X-ray diffraction (XRD) analysis showed that both the undoped and doped ZnO thin films are polycrystalline in nature with (101) preferred orientation. SEM analysis showed a change in surface morphology of Sb doped ZnO thin films. Doping results in a marked increase in conductivity without affecting the transmittance of the films. ZnO films prepared with 3 at % Sb shows the lowest resistivity of 0.185 Ohm cm with a Hall mobility of 54.05 cm{sup 2} V{sup –1} s{sup –1}, and a hole concentration of 6.25 × 10{sup 17} cm{sup –3}.

  13. Synthesis of ZnO Microrods by the Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Ikhmayies, Shadia J.

    2016-08-01

    Zinc oxide (ZnO) microrods were synthesized by the spray pyrolysis technique on aluminum substrates at a substrate temperature of 350 ± 5°C. The samples were characterized by x-ray diffraction (XRD), x-ray fluorescence (XRF), scanning electron microscopy (SEM), and energy dispersion x-ray spectroscopy (EDX). XRD diffractograms presented the wurtzite (hexagonal) structure with (002) as the preferential orientation. The SEM observations showed typical microrods of hexagonal cross sections with lengths in the range 1.0-2.5 μm and diameter in the range 300-400 nm. XRF and EDX analysis revealed that the samples contain chlorine, and other impurities, which are related to the aluminum substrate and the starting material zinc chloride (ZnCl2). It is found that the microrods are rich in oxygen, which make them of potential use in gas sensors, besides solar cells, lithium ion batteries and other electo-optic devices.

  14. Synthesis of ZnO Hexagonal Micro Discs on Glass Substrates Using the Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Ikhmayies, Shadia J.; Zbib, Mohamad B.

    2017-07-01

    Zinc oxide (ZnO) is an important transparent conducting oxide of potential use in solar cells, electronics, photoelectronics, and sensors. In this work ZnO micro discs were synthesized in thin film form on glass substrates using the low cost spray pyrolysis method. The films were prepared from a precursor solution of ZnCl2 in distilled water at a substrate temperature of 300 ± 5°C. The as-synthesized samples were analyzed with x-ray diffraction, scanning electron microscopy, and x-ray energy dispersive spectroscopy (EDS). The morphology of the films showed randomly distributed micro discs of hexagonal shape. The EDS reports showed that the films contained Cl and Fe. Size analysis was performed using ImageJ software, where the average diameter was found to be 4.8 ± 0.9 μm, and the average thickness was found to be 254 ± 43 nm.

  15. Indium oxide thin-film transistors processed at low temperature via ultrasonic spray pyrolysis.

    PubMed

    Faber, Hendrik; Lin, Yen-Hung; Thomas, Stuart R; Zhao, Kui; Pliatsikas, Nikos; McLachlan, Martyn A; Amassian, Aram; Patsalas, Panos A; Anthopoulos, Thomas D

    2015-01-14

    The use of ultrasonic spray pyrolysis is demonstrated for the growth of polycrystalline, highly uniform indium oxide films at temperatures in the range of 200-300 °C in air using an aqueous In(NO3)3 precursor solution. Electrical characterization of as-deposited films by field-effect measurements reveals a strong dependence of the electron mobility on deposition temperature. Transistors fabricated at ∼250 °C exhibit optimum performance with maximum electron mobility values in the range of 15-20 cm(2) V (-1) s(-1) and current on/off ratio in excess of 10(6). Structural and compositional analysis of as-grown films by means of X-ray diffraction, diffuse scattering, and X-ray photoelectron spectroscopy reveal that layers deposited at 250 °C are denser and contain a reduced amount of hydroxyl groups as compared to films grown at either lower or higher temperatures. Microstructural analysis of semiconducting films deposited at 250 °C by high resolution cross-sectional transmission electron microscopy reveals that as-grown layers are extremely thin (∼7 nm) and composed of laterally large (30-60 nm) highly crystalline In2O3 domains. These unique characteristics of the In2O3 films are believed to be responsible for the high electron mobilities obtained from transistors fabricated at 250 °C. Our work demonstrates the ability to grow high quality low-dimensional In2O3 films and devices via ultrasonic spray pyrolysis over large area substrates while at the same time it provides guidelines for further material and device improvements.

  16. Synthesis of kerosene based nanocarbons by a nebulized spray pyrolysis method

    SciTech Connect

    Widjaja, Ongky Arie, Arenst Andreas; Halim, Martin; Lee, Joong Kee

    2016-04-19

    In this work, kerosene oil based nanocarbons were synthesized by a nebulized spray pyrolysis method. This method was conducted at temperature of 700°C under a nitrogen inert atmospheric condition. Activated carbon and ferrocene were used as substrate and catalyst, respectively. Initially, ferrocene was dissolved in the oil with fixed concentration of 0.02 g/ml. The pyrolysis reaction was carried out by varying the operating time of 15, 30 and 45 minutes. The main aim of this work was to investigate the effect of varying the operation time on the morphology and structural characteristics of as-prepared carbon products. The morphology and structural characteristics of synthesized nanocarbons were examined by Scanning Electron Microscope (SEM), Transmission Electron Microscopy (TEM), and Raman Spectroscopy, respectively. SEM and TEM observations showed that nano carbons were formed as agglomerated carbon nanospheres (CNSs) and graphene for all variation of operating time. Furthermore, it was observed that the size of agglomerated CNSs was proportional with the operating time from 15 to 45 minutes. Raman analysis showed that the ratio between graphite like and disorder carbon structure (I{sub G}/I{sub D})of carbon samples increased from operating time of 15 to 30 minutes, however the ratio decreased from 30 minutes to 45 minutes.

  17. Synthesis of kerosene based nanocarbons by a nebulized spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Widjaja, Ongky; Arie, Arenst Andreas; Halim, Martin; Lee, Joong Kee

    2016-04-01

    In this work, kerosene oil based nanocarbons were synthesized by a nebulized spray pyrolysis method. This method was conducted at temperature of 700°C under a nitrogen inert atmospheric condition. Activated carbon and ferrocene were used as substrate and catalyst, respectively. Initially, ferrocene was dissolved in the oil with fixed concentration of 0.02 g/ml. The pyrolysis reaction was carried out by varying the operating time of 15, 30 and 45 minutes. The main aim of this work was to investigate the effect of varying the operation time on the morphology and structural characteristics of as-prepared carbon products. The morphology and structural characteristics of synthesized nanocarbons were examined by Scanning Electron Microscope (SEM), Transmission Electron Microscopy (TEM), and Raman Spectroscopy, respectively. SEM and TEM observations showed that nano carbons were formed as agglomerated carbon nanospheres (CNSs) and graphene for all variation of operating time. Furthermore, it was observed that the size of agglomerated CNSs was proportional with the operating time from 15 to 45 minutes. Raman analysis showed that the ratio between graphite like and disorder carbon structure (IG/ID)of carbon samples increased from operating time of 15 to 30 minutes, however the ratio decreased from 30 minutes to 45 minutes.

  18. Flame spray pyrolysis: An enabling technology for nanoparticles design and fabrication.

    PubMed

    Teoh, Wey Yang; Amal, Rose; Mädler, Lutz

    2010-08-01

    Combustion of appropriate precursor sprays in a flame spray pyrolysis (FSP) process is a highly promising and versatile technique for the rapid and scalable synthesis of nanostuctural materials with engineered functionalities. The technique was initially derived from the fundamentals of the well-established vapour-fed flame aerosols reactors that was widely practised for the manufacturing of simple commodity powders such as pigmentary titania, fumed silica, alumina, and even optical fibers. In the last 10 years however, FSP knowledge and technology was developed substantially and a wide range of new and complex products have been synthesised, attracting major industries in a diverse field of applications. Key innovations in FSP reactor engineering and precursor chemistry have enabled flexible designs of nanostructured loosely-agglomerated powders and particulate films of pure or mixed oxides and even pure metals and alloys. Unique material morphologies such as core-shell structures and nanorods are possible using this essentially one step and continuous FSP process. Finally, research challenges are discussed and an outlook on the next generation of engineered combustion-made materials is given.

  19. Flame spray pyrolysis: An enabling technology for nanoparticles design and fabrication

    NASA Astrophysics Data System (ADS)

    Teoh, Wey Yang; Amal, Rose; Mädler, Lutz

    2010-08-01

    Combustion of appropriate precursor sprays in a flame spray pyrolysis (FSP) process is a highly promising and versatile technique for the rapid and scalable synthesis of nanostuctural materials with engineered functionalities. The technique was initially derived from the fundamentals of the well-established vapour-fed flame aerosols reactors that was widely practised for the manufacturing of simple commodity powders such as pigmentary titania, fumed silica, alumina, and even optical fibers. In the last 10 years however, FSP knowledge and technology was developed substantially and a wide range of new and complex products have been synthesised, attracting major industries in a diverse field of applications. Key innovations in FSP reactor engineering and precursor chemistry have enabled flexible designs of nanostructured loosely-agglomerated powders and particulate films of pure or mixed oxides and even pure metals and alloys. Unique material morphologies such as core-shell structures and nanorods are possible using this essentially one step and continuous FSP process. Finally, research challenges are discussed and an outlook on the next generation of engineered combustion-made materials is given.

  20. Synthesis and characterization of ZnO nano and micro structures grown by low temperature spray pyrolysis and vapor transport.

    PubMed

    Agouram, S; Bushiri, M J; Montenegro, D N; Reig, C; Martínez-Tomás, M C; Muñoz-Sanjosé, V

    2012-08-01

    In this work we present a systematic study of ZnO micro and nanostructures grown by spray pyrolysis (SP) and by physical vapour transport (PVT) on glass and c-sapphire substrates at low temperatures. Optimised growth conditions have allowed to obtain homogeneous ZnO nanolayers composed of quasi-spherical nanoparticles in the range 2 to 8 nm by spray pyrolysis, while by PVT the selected growth conditions allow to produce a wide variety of morphologies (tripods, grains, arrows and wires) of nano and microsize dimension. Grazing incidence X-ray diffraction, field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and energy dispersive X-ray spectroscopy (EDX) were used as characterization techniques in the investigation of structural, morphological and compositional nature of these nanostructures in relation with the growth method.

  1. Electrocatalytic upgrading of biomass pyrolysis oils to chemical and fuel

    NASA Astrophysics Data System (ADS)

    Lam, Chun Ho

    The present project's aim is to liquefy biomass through fast pyrolysis and then upgrade the resulting "bio-oil" to renewable fuels and chemicals by intensifying its energy content using electricity. This choice reflects three points: (a) Liquid hydrocarbons are and will long be the most practical fuels and chemical feedstocks because of their energy density (both mass and volume basis), their stability and relative ease of handling, and the well-established infrastructure for their processing, distribution and use; (b) In the U.S., the total carbon content of annually harvestable, non-food biomass is significantly less than that in a year's petroleum usage, so retention of plant-captured carbon is a priority; and (c) Modern technologies for conversion of sunlight into usable energy forms---specifically, electrical power---are already an order of magnitude more efficient than plants are at storing solar energy in chemical form. Biomass fast pyrolysis (BFP) generates flammable gases, char, and "bio-oil", a viscous, corrosive, and highly oxygenated liquid consisting of large amounts of acetic acid and water together with hundreds of other organic compounds. With essentially the same energy density as biomass and a tendency to polymerize, this material cannot practically be stored or transported long distances. It must be upgraded by dehydration, deoxygenation, and hydrogenation to make it both chemically and energetically compatible with modern vehicles and fuels. Thus, this project seeks to develop low cost, general, scalable, robust electrocatalytic methods for reduction of bio-oil into fuels and chemicals.

  2. Investigation of ZnO Thin Film Synthesized by Spray Pyrolysis Method as a Toxic Gases Sensor

    NASA Astrophysics Data System (ADS)

    Khojier, K.

    2017-10-01

    In recent years, environmental pollution, particularly toxic gases and vapors, have greatly increased; hence, their detection has become increasingly important. This paper investigates ZnO thin films fabricated by the spray pyrolysis method to fabricate a toxic gases sensor. A ZnO thin film of 100 nm thickness was deposited on a glass substrate at 100°C. The crystallographic structure was characterized by x-ray diffraction and a field-emission scanning electron microscope was employed to investigate the surface physical morphology and chemical composition. Sensitivity and selectivity of the sample were tested with respect to different toxic gases and vapors including carbon monoxide, ammonia, hydrogen sulfide, chlorine, nitrogen dioxide, benzene, formaldehyde and toluene in the temperature range of 100-300°C. The results showed that the ZnO thin film is more selective to NO2 gas than the other toxic gases and vapors in the studied temperature range. The ZnO thin film-based NO2 gas sensor also showed a good reproducibility, stability, and detection limit of 10 ppm at the operating temperature of 200°C.

  3. Performance enhancement through post-treatments of CdS-sensitized solar cells fabricated by spray pyrolysis deposition.

    PubMed

    Lee, Yong Hui; Im, Sang Hyuk; Rhee, Jae Hui; Lee, Jong-Heun; Seok, Sang Il

    2010-06-01

    The CdS-sensitized solar cells (CdS-SSC) were fabricated by spray pyrolysis deposition (SPD) method. The performance of the cells was greatly improved through post-treatments that included thermal oxidation at 500 degrees C for 30 min in an air atmosphere and subsequent chemical etching by 40 mM aqueous HCl solution at room temperature for 30 min, as compared to as-deposited CdS-SSC. The CdS-SSC in a I(-)/I(3)(-) electrolyte system was resulted in the improvement of J(sc) (3.3 --> 5.2 mA/cm(2)), V(oc) (697 --> 758 mV), FF (41.4% --> 46.9%), and (0.95% --> 1.84%). Similarly, the efficiency of CdS-SSC in a noncorrosive polysulfide electrolyte system was also enhanced by the proposed thermal oxidation and etching process. The increase in the cell efficiency is attributed to the reduced charge recombination among sensitizer themselves through the mitigation of overaggregated CdS sensitizers deposited by SPD.

  4. Influence of Annealing Duration on the Growth of V2O5 Nanorods Synthesized by Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Abd-Alghafour, N. M.; Ahmed, Naser M.; Hassan, Z.; Abubakar, D.; Bououdina, M.

    2016-06-01

    This paper deals with the investigation of annealing effects on the structural, morphological and optical properties of V2O5 nanorods (NRs) grown on the glass substrates by using chemical spray pyrolysis technique. The as-prepared samples were annealed at 500∘ for 40, 60 and 120 min in a quartz tube furnace. The high resolution X-ray diffraction (XRD) analysis revealed V2O5 NRs with preferred orientation along (001) plane. The crystallite size of the V2O5 NRs was increased by increasing the annealing duration. The morphological observations using field emission scanning electron microscope (FESEM) displayed NRs structures whose diameter and length were found to increase with increase of the annealing duration. The transmission electron microscopy (TEM) analysis confirmed the orthorhombic structures of the NRs. The AFM measurements indicated an increase of the average surface roughness by increasing the annealing time. The Raman spectroscopy revealed V-O-V phonon mode in the NRs annealed for 120 min. The optical bandgap was found in the range 2.6-2.58eV and observed to decrease with various duration annealed.

  5. Thickness-Dependent Structural and Optoelectronic Properties of In2O3 Films Prepared by Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Khan, M. A. Majeed; Khan, Wasi

    2016-08-01

    In this work, nanostructured In2O3 thin films with thickness in the range of 40-160 nm were deposited on glass substrates by the chemical spray pyrolysis technique. The microstructural, surface morphology and optical properties were investigated as a function of film thickness through x-ray diffraction, scanning electron microscopy equipped with energy dispersive spectroscopy, atomic force microscopy, Raman spectroscopy, UV-visible spectroscopy and photoluminescence measurements. The x-ray diffraction analysis showed that the deposited films were polycrystalline in nature with a cubic structure having (222) as preferred orientation. The morphological analyses of the samples exhibited uniform and smooth surface of the films with systematical increments in the surface roughness with increasing film thickness. The grain size increased from 9 nm to 13 nm with increasing film thickness. Raman spectroscopy has been employed to study the crystalline quality and the structural disorder of the films. A blue-shift in the energy band gap ( E g) from 3.74 eV to 3.98 eV was observed with the increase of film thickness. Moreover, photoluminescence peaks of the In2O3 films appeared at 443 nm and 527 nm for all films. The thickness had a substantial influence on the microstructural and optical properties as well as on the luminescence intensity of the films. The strategy presented here indicates that the prepared films could be suitable candidates for optoelectronic device applications.

  6. Study of Optical and Electrical Properties of In2S3:Sn Films Deposited by Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Kraini, M.; Bouguila, N.; Halidou, I.; Moadhen, A.; Vázquez-Vázquez, C.; López-Quintela, M. A.; Alaya, S.

    2015-07-01

    Tin-doped In2S3 films were grown by the chemical spray pyrolysis method using compressed air as a carrier gas. Tin is incorporated in the solution using SnCl4. Structural and optical properties of films were investigated by x-ray diffraction (XRD), absorption, Raman and photoluminescence spectroscopies. Field emission scanning electron microscopy (FESEM) and energy dispersive x-ray spectroscopy were used to explore the surface morphology. The properties of In2S3 thin films are influenced by Sn doping. XRD studies revealed that the deposited films were polycrystalline in nature exhibiting cubic structure and oriented preferentially towards (111). According to FESEM, the surface morphology of the films was free of defects. Raman studies showed different peaks related to In2S3 phase and did not show any secondary phases of In-Sn and Sn-S. In2S3:Sn films exhibited transparency over 60-85% in the visible and infrared regions. The optical band gap was found to vary in the range 2.71-2.58 eV for direct transitions. The room temperature photoluminescence (PL) studies revealed two PL bands, centered at 529 nm (band A) and 725 nm (band B). From these results, one can conclude that our material can be used as transmittive windows in low-cost solar cells. The conductance and capacitance characterization at ambient temperature were also investigated and gave interesting physical properties for photovoltaic applications.

  7. Influence of the process parameters on the spray pyrolysis technique, on the synthesis of gadolinium doped-ceria thin film

    SciTech Connect

    Halmenschlager, C.M.; Neagu, R.; Rose, L.; Malfatti, C.F.

    2013-02-15

    Graphical abstract: Gas-tight CGO made by spray pyrolysis suitable to be used as SOFC electrolyte. Display Omitted Highlights: ► Dense and crystalline CGO films deposited by spray pyrolysis on various substrates. ► Solvent did not have a strong influence on the film microstructure, defect concentration or thickness. ► The substrate did not have a strong influence on the film microstructure, defect concentration or thickness. ► Films with at least 2.5 μm of thickness presented high impermeability. ► The films obtained are suitable to use as a SOFC electrolyte. -- Abstract: This work presents the results of a process of optimization applied to gadolinia-doped ceria (Ce{sub 0.8}Gd{sub 0.2}O{sub 1.9−x}, or CGO) thin films, deposited by spray pyrolysis (SP). Spray pyrolysis is a high thermal deposition method that combines material deposition and heat treatment. This combination is advantageous since the post-deposition heat treatment step is not necessary. However, stresses are solidified in the coating during the deposition, which may lead to the initiation of a crack in the coating. The aim of this work was to achieve thin, dense, and continuous CGO coatings, which may be used as gas separation membranes and as a solid state electrochemical interfaces. Dense, flat, low-defect substrates such as silica slides, silicon mono crystal wafers, and porous substrates were used as substrates in this work. Cerium ammonium nitrate and gadolinium acetylacetonate were dissolved in ethanol and butyl carbitol to form a precursor solution that was sprayed on the heated substrates. Process parameters such as solvent composition, deposition rate and different heating regimes were analyzed. The microstructure was analyzed by secondary electron microscopy (SEM) and was found that thin, dense, and defect-free films could be produced on dense and porous substrates. The results obtained show that it is possible to obtain a CGO dense film deposited by spray pyrolysis. X

  8. Synthesis of TiO{sub 2} core/RuO{sub 2} shell particles using multistep ultrasonic spray pyrolysis

    SciTech Connect

    Stopic, Srecko; Friedrich, Bernd; Schroeder, Michael; Weirich, Thomas E.

    2013-09-01

    Graphical abstract: - Highlights: • TiO{sub 2} core/RuO{sub 2} shell submicron-particles were prepared via a sequential spray pyrolysis. • Spherical particles have the mean particle diameters between 200 and 400 nm. • This method is promising for synthesis of core–shell and core–multishell materials. - Abstract: Spherical submicron-particles with TiO{sub 2} core–RuO{sub 2} shell structure have been synthesized by employing sequential ultrasonic spray pyrolysis. The particles have been investigated by X-ray powder diffraction, scanning electron microscopy and different transmission electron microscopy techniques. The quality of the core–shell structure of the particles has been confirmed by comparison of the experimental data with those generated on the basis of a hard sphere core–shell model. It has been found that the mixing of the Ru-containing aerosol with the TiO{sub 2} particle stream has a significant impact on the core–shell formation. The method introduced in this study can probably be applied for preparation of core–shell and core–multishell materials that are difficult to synthesize in a single step spray pyrolysis process.

  9. Generation of metal, metal oxide and metal-metal oxide powders by spray pyrolysis for microelectronic thick film applications

    NASA Astrophysics Data System (ADS)

    Majumdar, Diptarka

    Materials in powdered form have wide ranging applications. In thick film microelectronics, powders are dispersed in organic liquids to form pastes which are screen printed on ceramic substrates and fired to fabricate active and passive electronic devices. The functional phase is a metal powder in conductive pastes, a metal or conductive metal oxide powder in resistive pastes and a ceramic powder in dielectric pastes. Particulate additives such as glasses and metal oxides in pastes promote adhesion of conductor lines to the substrate, minimize shrinkage mismatch during cofiring of conductors and dielectrics and facilitate densification of the functional phase during firing. This dissertation focuses on the generation of metal, metal oxide and metal-metal oxide powders by spray pyrolysis for microelectronic applications. The important results of this work are outlined below. (1) This work has demonstrated the ability to synthesize phase-pure, micron-sized, spherical, unagglomerated metal (gold) and metal oxide (copper (I) oxide) particles by spray pyrolysis. (2) It has extended the versatility of spray pyrolysis as a powdermaking technique to include the synthesis of metal-metal oxide composite particles. Such particles have been generated for both wetting (silver-copper (II) oxide) and poorly wetting (silver-silica) metal-metal oxide pairs. (3) The sintering of thick films of the metal-metal oxide particles has indicated the possibility of retarding the sintering kinetics of silver by using composite particles of the metal with relatively refractory metal oxides.

  10. Thermal and chemical effects of turkey feathers pyrolysis.

    PubMed

    Kluska, Jacek; Kardaś, Dariusz; Heda, Łukasz; Szumowski, Mateusz; Szuszkiewicz, Jarosław

    2016-03-01

    This study examines the thermal and chemical effects of the pyrolysis of turkey feathers. Research of feathers pyrolysis is important because of their increasing production and difficulties of their utilization. The experiments were carried out by means of thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and two pyrolytic reactors. The experimental investigation indicated that the feather material liquefies at temperatures between 210 and 240°C. This liquefaction together with the agglomeration of various dispersed and porous elements of the feathers into larger droplets leads to the volume reduction. Moreover, this work presents characteristics of the composition of the solid, liquid and gaseous products of turkey feathers pyrolysis at different temperatures. The higher heating value (HHV) of gaseous products in temperature 900°C equals 19.28 MJ/Nm(3) making the gases suitable for use as a fuel. The thermochemical conversion of turkey feathers leads to the formation of poisonous compounds such as hydrogen cyanide (HCN) in the liquid (0.13%) and gaseous (88 mg/Nm(3)) products. The phenomenon of liquefaction of feathers is important because it can lead to rapid degradation of the walls of reactors, and the formation of deposits.

  11. Chemical recycling of mixed waste plastics by selective pyrolysis

    SciTech Connect

    Tatsumoto, K.; Meglen, R.; Evans, R.

    1995-05-01

    The goal of this work is to use selective pyrolysis to produce high-value chemicals from waste plastics mixtures. Selectivity is achieved by exploiting differences in reaction rates, catalysis, and coreactants. Target wastes are molecular mixtures such as; blends or composites, or mixtures from manufactured products such as; carpets and post-consumer mixed-plastic wastes. The experimental approach has been to use small-scale experiments using molecular beam mass spectrometry (MBMS), which provides rapid analysis of reaction products and permits rapid screening of process parameters. Rapid screening experiments permit exploration of many potential waste stream applications for the selective pyrolysis process. After initial screening, small-scale, fixed-bed and fluidized-bed reactors are used to provide products for conventional chemical analysis, to determine material balances, and to test the concept under conditions that will be used at a larger scale. Computer assisted data interpretation and intelligent chemical processing are used to extract process-relevant information from these experiments. An important element of this project employs technoeconomic assessments and market analyses of durables, the availability of other wastes, and end-product uses to identify target applications that have the potential for economic success.

  12. Comparative study of ITO and FTO thin films grown by spray pyrolysis

    SciTech Connect

    Ait Aouaj, M.; Diaz, R.; Belayachi, A.; Rueda, F.; Abd-Lefdil, M.

    2009-07-01

    Tin doped indium oxide (ITO) and fluorine doped tin oxide (FTO) thin films have been prepared by one step spray pyrolysis. Both film types grown at 400 deg. C present a single phase, ITO has cubic structure and preferred orientation (4 0 0) while FTO exhibits a tetragonal structure. Scanning electron micrographs showed homogeneous surfaces with average grain size around 257 and 190 nm for ITO and FTO respectively. The optical properties have been studied in several ITO and FTO samples by transmittance and reflectance measurements. The transmittance in the visible zone is higher in ITO than in FTO layers with a comparable thickness, while the reflectance in the infrared zone is higher in FTO in comparison with ITO. The best electrical resistivity values, deduced from optical measurements, were 8 x 10{sup -4} and 6 x 10{sup -4} {Omega} cm for ITO (6% of Sn) and FTO (2.5% of F) respectively. The figure of merit reached a maximum value of 2.15 x 10{sup -3} {Omega}{sup -1} for ITO higher than 0.55 x 10{sup -3} {Omega}{sup -1} for FTO.

  13. Deposition of Ni-CGO composite anodes by electrostatic assisted ultrasonic spray pyrolysis method

    SciTech Connect

    Chen, J.-C.; Chang, C.-L.; Hsu, C.-S.; Hwang, B.-H. . E-mail: zorro@mail.nsysu.edu.tw

    2007-09-04

    Deposition of composite films of Ni and Gd-doped ceria was carried out using the electrostatic assisted ultrasonic spray pyrolysis method for the first time. The composite films were highly homogeneous, as revealed by element mapping via energy-dispersive spectrometry. Scanning electron microscope examinations revealed that deposition temperature and electric field strength had profound influence on resultant microstructure, while composition of the precursor solution had little effect. A highly porous cauliflower structure ideal for solid oxide fuel cell anode performance was obtained with a deposition temperature of 450 deg. C under an electric field introduced by an applied voltage of 12 kV. Films obtained with a lower deposition temperature of 250 deg. C or a higher applied voltage of 15 kV resulted in denser films with low porosity, while lower applied voltages of 7 or 5 kV resulted in thinner or discontinuous films due to the insufficient electrostatic attraction on the aerosol droplets. As revealed by AC impedance measurement, the area specific resistances of the Ni-CGO anode with porous cauliflower structure were rather low and a value of 0.09 {omega} cm{sup 2} at 550 deg. C was obtained.

  14. Synthesis of Carbon Nano Materials Originated from Waste Cooking Oil Using a Nebulized Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Arie, A. A.; Hadisaputra, L.; Susanti, R. F.; Devianto, H.; Halim, M.; Enggar, R.; Lee, J. K.

    2017-07-01

    Synthesis of nanocarbon on snake fruit-peel’s activated carbon from waste cooking oil palm was conducted by a nebulized spray pyrolysis process (NSP) by varying the processing temperature from 650 to 750 °C. Ferrocene was used as a catalyst with constant concentration of 0.015 g/ml of carbon source. The structure of nanocarbon was studied by using scanning electron microscope (SEM),x-ray diffraction (XRD), surface area analyzer and Raman spectroscopy. SEM results showed that the structures of carbon products was in the the form of carbon nanopsheres (CNS). XRD and Raman analysis confirmed the CNS structure. The carbon producs were then tested as electrode’s materials for lithium ion capacitors (LIC) by cyclic voltammetry (CV) instruments. From the CV results the specific capacitance was estimated as 79.57 F / g at a scan rate of 0.1 mV / s and voltage range from 2.5 - 4 V. This study shows that the nano carbons synthesized from the waste cooking oil can be used as prospective electrode materials for LIC.

  15. Investigation on vanadium oxide thin films deposited by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Margoni, Mudaliar Mahesh; Mathuri, S.; Ramamurthi, K.; Babu, R. Ramesh; Sethuraman, K.

    2016-05-01

    Vanadium oxide thin films were deposited at 400 °C by spray pyrolysis technique using 0.1 M aqueous precursor solution of ammonium meta vanadate (AMV) with two different pH values. X-ray diffraction results showed that the film prepared using aqueous precursor AMV solution (solution A; pH 7) is amorphous in nature and the film prepared by adding HNO3 in the AMV aqua solution A (solution B; pH 3) is polycrystalline in nature. Vanadium oxide film prepared from the precursor solution B is in the mixed phases of V2O5 and V4O7. Crystallinity is improved for the film prepared using solution B when compared to film prepared from solution A. Crystallite size, strain and dislocation density calculated for the film prepared from solution B is respectively 72.1 nm, 0.4554 × 10-3 lin.-2m-4 and 1.7263 × 1014 lin.m-2. Morphology study revealed that the size of the flakes formed on the surface of the films is influenced by the pH of the precursor solution. Average Visible Transmittance and maximum transmittance of the deposited films exceed 70% and the direct optical band gap value calculated for the films deposited from A and B solution is 1.91 eV and 2.08 eV respectively.

  16. Growth and characterization of molybdenum doped ZnO thin films by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Swapna, R.; Santhosh Kumar, M. C.

    2013-03-01

    Undoped and molybdenum doped zinc oxide (MZO) thin films were deposited on the glass substrate at a substrate temperature of 623 K by spray pyrolysis method. The effect of molybdenum (Mo) dopant concentration (0-4 at%) on the structural, morphological, optical and electrical properties of n-type MZO films was studied. The X-ray diffraction (XRD) results confirmed that the MZO thin films were polycrystalline with wurtzite structure. The scanning electron microscopy (SEM) measurements showed that the surface morphology of the films changes with Mo doping. The surface roughness of the films was investigated by atomic force microscopy (AFM). It was observed that the roughness of the films increases with the increase of Mo doping percentage. A blue shift of the optical band gap was observed. Room temperature photoluminescence (PL) measurement of the deposited films indicates the incorporation of Mo in ZnO lattice. The temperature dependence of the electrical conductivity was studied in the range of 300 K-425 K. At 2 at% Mo doping, the films have shown comparatively high electrical conductivity.

  17. Electrical and optical properties of Al doped Zno film prepared by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Shrestha, Shankar Prasad; Basnet, Pradeep

    2008-04-01

    Transparent conducting thin films of zinc oxides and aluminum doped zinc oxide (AZO) were prepared by the spray pyrolysis technique using an aqueous solution of dehydrate zinc acetate (CH 3COOH. 2H IIO, pure- Merck A. R. grade) and hex hydrate aluminum chloride (AlCl 3 .6H IIO) on the micro glass slides. The prepared thin films are found to be highly adherent to the substrate and possess uniform conduction. The optical and electrical properties of the film were investigated in terms of different Al concentration in the starting solution and different substrate temperature. Four probe method in Van der pauw configuration was used for electrical resistivity measurements. The resistivity of Al doped film is observed to vary with doping concentration. The lowest resistivity is observed in the film doping with 2 at % [Al/Zn]. The Hall coefficient measurements show that both ZnO and AZO show the n-type conduction. The carrier concentration was observed to be highest at 2 at% of Al doping. The optical measurements of all the samples with aluminum concentrations was found to be >85 % showing the film to be highly transparent in nature. With increase in Al concentration, the optical band gap was observed increase from 3.27 eV to 3.41 eV.

  18. Conductivity study of nitrogen-doped calcium zinc oxide prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Hsu, Yu-Ting; Lan, Wen-How; Huang, Kai-Feng; Lin, Jia-Ching; Chang, Kuo-Jen

    2016-01-01

    In this study, the spray pyrolysis method was used to prepare unintentionally doped and nitrogen-doped calcium zinc oxide films by using zinc acetate, calcium nitrate precursor, and ammonium acetate precursor. Morphological and structural analyses were conducted using scanning electron microscopy and X-ray diffraction. The results indicated that film grain size decreased as the nitrogen doping was increased. Both calcium oxide and zinc oxide structures were identified in the unintentionally doped calcium zinc oxide. When nitrogen doping was introduced, the film mainly exhibited a zinc oxide structure with preferred (002) and (101) orientations. The concentration and mobility were investigated using a Hall measurement system. P-type films with a mobility and concentration of 10.6 cm2 V-1 s-1 and 2.8×1017 cm-3, respectively, were obtained. Moreover, according to a temperature-dependent conductivity analysis, an acceptor state with activation energy 0.266 eV dominated the p-type conduction for the unintentionally doped calcium zinc oxide. By contrast, a grain boundary with a barrier height of 0.274-0.292 eV dominated the hole conduction for the nitrogen-doped calcium zinc oxide films.

  19. Photoelectrochemical performance of W-doped BiVO4 thin films deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Holland, S. Keith; Dutter, Melissa R.; Lawrence, David J.; Reisner, Barbara A.; DeVore, Thomas C.

    2014-01-01

    The effects of tungsten doping and hydrogen annealing on the photoelectrochemical (PEC) performance of bismuth vanadate (BiVO4) photoanodes for solar water splitting were studied. Thin films of BiVO were deposited on indium tin oxide-coated glass slides by ultrasonic spray pyrolysis of an aqueous solution containing bismuth nitrate and vanadium oxysulfate. Tungsten doping was achieved by adding either silicotungstic acid (STA) or ammonium metatungstate (AMT) to the precursor. The 1.7- to 2.2-μm-thick films exhibited a highly porous microstructure. Undoped films that were reduced at 375°C in 3% H exhibited the largest photocurrent densities under 0.1 W cm-2 AM1.5 illumination, where photocurrent densities of up to 1.3 mA cm-2 at 0.5 V with respect to Ag/AgCl were achieved. Films doped with 1% or 5% (atomic percent) tungsten from either STA or AMT exhibited reduced PEC performance and greater sample-to-sample performance variations. Powder x-ray diffraction data indicated that the films continue to crystallize in the monoclinic polymorph at low doping levels but crystallize in the tetragonal scheelite structure at higher doping. It is surmised that the phase and morphology differences promoted by the addition of W during the deposition process reduced the PEC performance as measured by photovoltammetry.

  20. Spray pyrolysis synthesis of ZnS nanoparticles from a single-source precursor.

    PubMed

    Liu, Sha; Zhang, Hongwang; Swihart, Mark T

    2009-06-10

    ZnS, a II-VI semiconductor with a relatively high direct bandgap (approximately 3.6 eV) in the near-UV region, has potential applications in areas such as solar cells, lasers and displays. In addition, ZnS nanoparticles can be applied as phosphors, probes for bioimaging, emitters in light emitting diodes and photocatalysts. Here, we report synthesis of cubic ZnS nanoparticles from a low-cost single-source precursor in a continuous spray pyrolysis reactor. In this approach, the evaporation and decomposition of precursor and nucleation of particles occur sequentially. Product particles were characterized by HRTEM, XRD, and EDX. Particles with diameters ranging from 2 to 7 nm were produced. HF was used to remove ZnO impurities and other surface contamination. As-synthesized ZnS nanoparticles exhibit blue photoluminescence near 440 nm under UV excitation and have quantum yields up to 15% after HF treatment. This demonstrates a potentially general approach for continuous low-cost synthesis of semiconductor quantum dots for applications where tight control of the size distribution is less important than scalable, economical production.

  1. Carbon monoxide gas sensing using zinc oxide film deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Leano, J. M. G.; Villapando, J. M. L. A.; Balaaldia, A. E.; Gianan, G.; Manalo, F. K. B.; Florido, E. A.

    2017-05-01

    This study was aimed to determine the carbon monoxide (CO) gas sensing ability of zinc oxide (ZnO) film fabricated by spray pyrolysis on glass substrate heated at 3000C using 0.2 M zinc acetate precursor solution. The temperature of the precursor solution was maintained at room temperature. Carbon monoxide gas was synthesized by mixing the required amount of formic acid and excess sulfuric acid in the ratio of 1:6 to produce CO gas concentrations of 100, 200, 300, 400, and 500 parts per million (ppm) v/v. There were five trials for each concentration. The films produced exhibited good sensor characteristics such as high linearity in current voltage relationship and voltage response versus concentration. Electrical characterization using the four-point probe showed a linear relationship between current and voltage with resistivity of 0.49 ohm-cm and R2 value of 0.994 The zinc oxide film exhibited a sensitivity of 0.19 Volt per 100 ppm of CO gas and linearity R2 value of 0.993.

  2. Spray pyrolysis deposition and photoelectrochemical properties of n-type BiOI nanoplatelet thin films.

    PubMed

    Hahn, Nathan T; Hoang, Son; Self, Jeffrey L; Mullins, C Buddie

    2012-09-25

    Bismuth oxy-iodide is a potentially interesting visible-light-active photocatalyst; yet there is little research regarding its photoelectrochemical properties. Herein we report the synthesis of BiOI nanoplatelet photoelectrodes by spray pyrolysis on fluorine-doped tin oxide substrates at various temperatures. The films exhibited n-type conductivity, most likely due to the presence of anion vacancies, and optimized films possessed incident photon conversion efficiencies of over 20% in the visible range for the oxidation of I(-) to I(3)(-) at 0.4 V vs Ag/AgCl in acetonitrile. Visible-light photons (λ > 420 nm) contributed approximately 75% of the overall photocurrent under AM1.5G illumination, illustrating their usefulness under solar light illumination. A deposition temperature of 260 °C was found to result in the best performance due to the balance of morphology, crystallinity, impurity levels, and optical absorption, leading to photocurrents of roughly 0.9 mA/cm(2) at 0.4 V vs Ag/AgCl. Although the films performed stably in acetonitrile, their performance decreased significantly upon extended exposure to water, which was apparently caused by a loss of surface iodine and subsequent formation of an insulating bismuth hydroxide layer.

  3. Solar selective coatings based on nickel oxide obtained via spray pyrolysis.

    PubMed

    Voinea, Mihaela; Ienei, Elena; Bogatu, Cristina; Duta, Anca

    2009-07-01

    The paper presents the optimization process for obtaining NiO thin layers on copper substrate for solar absorber coatings, using an inexpensive and up-scalable technique: spray pyrolysis deposition (SPD). Efficient selective coatings must present a high absorption coefficient of the incident solar irradiation, and low emission of heat. The solar selective coatings design involves tailoring the surface properties for superior optical properties. The deposition parameters were varied for maximizing the solar absorbance and minimizing the thermal emittance. The film morphology was controlled using copolymers of the maleic anhydride as additives into the precursors' solution. The structural and surface properties of the films were investigated by X-ray diffraction and atomic force microscopy, respectively. The Cu/CuO(x)/NiO solar absorber shows good values for the solar absorptance (alpha(s) = 0.95) and thermal emittance (epsilon(T) = 0.05) compared with the ones obtained by other methods employed in literature and new additives are recommended in tailoring the surface of solar selective coatings.

  4. Electrical conductivity and crystallization of amorphous bismuth ruthenate thin films deposited by spray pyrolysis.

    PubMed

    Ryll, Thomas; Brunner, Andreas; Ellenbroek, Stefan; Bieberle-Hutter, Anja; Rupp, Jennifer L M; Gauckler, Ludwig J

    2010-11-14

    Amorphous oxide thin films with tailored functionality will be crucial for the next generation of micro-electro-mechanical-systems (MEMS). Due to potentially favorable electronic and catalytic properties, amorphous bismuth ruthenate thin films might be applied in this regard. We report on the deposition of amorphous bismuth ruthenate thin films by spray pyrolysis, their crystallization behavior and electrical conductivity. At room temperature the 200 nm thin amorphous films exhibit a high electrical conductivity of 7.7 × 10(4) S m(-1), which was found to be slightly thermally activated (E(a) = 4.1 × 10(-3) eV). It follows that a long-range order of the RuO(6) octahedra is no precondition for the electrical conductivity of Bi(3)Ru(3)O(11). Upon heating to the temperature range between 490 °C and 580 °C the initially amorphous films crystallize rapidly. Simultaneously, a transition from a dense and continuous film to isolated Bi(3)Ru(3)O(11) particles on the substrate takes place. Solid-state agglomeration is proposed as the mechanism responsible for disintegration. The area specific resistance of Bi(3)Ru(3)O(11) particles contacted by Pt paste on gadolinia doped ceria electrolyte pellets was found to be 7 Ω cm(2) at 607 °C in air. Amorphous bismuth ruthenate thin films are proposed for application in electrochemical devices operating at low temperatures, where a high electrical conductivity is required.

  5. Superhydrophobic and transparent ZnO thin films synthesized by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Tarwal, N. L.; Patil, P. S.

    2010-10-01

    Superhydrophobic and transparent zinc oxide (ZnO) thin films were deposited by a simple and cost effective spray pyrolysis technique (SPT) onto the glass substrates at 723 K from an aqueous zinc acetate precursor solution. The solution concentration was varied from 0.1 to 0.4 M and its effect on structural, morphological, wetting and optical properties of ZnO thin films was studied. The synthesized films were found to be polycrystalline, with preferential growth along c-axis. A slight improvement in the crystallite size and texture coefficient is observed as the concentration of the solution is increased. SEM micrographs show the uniform distribution of spherical grains of about 60-80 nm grain size. The films were specular and highly transparent with average transmittance of about 85%. The spectrum shows sharp absorption band edge at 381 nm, corresponding to optical gap of 3.25 eV. The samples of texture coefficient less than 90% and roughness less than 75 nm are hydrophobic and above these values they become superhydrophobic in nature. The hydrophobicity coupled with high transmittance is of great importance in commercial application such as transparent self-cleaning surfaces, anti-fog, anti-snow, fluid microchips and microreactors.

  6. Effects of deposition conditions on the phase formation of YBCO films prepared by spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Kim, Ho-Jin; Joo, Jinho; Park, Shin-Geun; Hong, Suck-Kwan; Lee, Sun-Wang; Lim, Sun-Weon; Hong, Gye-Won; Lee, Hee-Gyoun

    2006-10-01

    YBa2Cu3Oy superconducting films were deposited on LaAlO3(1 0 0) single crystal substrates by spray pyrolysis method. Two types of ultrasonic and concentric nebulizer were used in order to generate fine droplets of metal-inorganic precursor solution. c-Axis oriented films were obtained at deposition temperature of 750-850 °C and at working pressures of 100 Torr and 500 Torr. In case of ultrasonic nebulizer, the films showed rough surface morphology due to the presence of enormous droplets, whereas smooth and dense films were obtained for concentric nebulizer. The good c-axis oriented YBCO films were formed at the wide range of the oxygen partial pressure. Oxygen which is generated via the decomposition of nitrate precursors is considered to participate in the formation reaction of YBCO film. Microstructures of YBCO films varied depending on oxygen partial pressure and rod-like grains were appeared when the oxygen partial pressure was lower than 30 Torr. YBCO films were deposited epitaxially on LAO(1 0 0) substrate. Δϕ of in-plane and Δω of out-of-plane texture were measured as 3.3° and 1.0°, respectively. A transport Jc value of 0.50 MA/cm2 at 77 K and self-field was achieved for the YBCO film deposited on LaAlO3(1 0 0) single crystal substrate.

  7. Hierarchical porous carbon by ultrasonic spray pyrolysis yields stable cycling in lithium-sulfur battery.

    PubMed

    Jung, Dae Soo; Hwang, Tae Hoon; Lee, Ji Hoon; Koo, Hye Young; Shakoor, Rana A; Kahraman, Ramazan; Jo, Yong Nam; Park, Min-Sik; Choi, Jang Wook

    2014-08-13

    Utilizing the unparalleled theoretical capacity of sulfur reaching 1675 mAh/g, lithium-sulfur (Li-S) batteries have been counted as promising enablers of future lithium ion battery (LIB) applications requiring high energy densities. Nevertheless, most sulfur electrodes suffer from insufficient cycle lives originating from dissolution of lithium polysulfides. As a fundamental solution to this chronic shortcoming, herein, we introduce a hierarchical porous carbon structure in which meso- and macropores are surrounded by outer micropores. Sulfur was infiltrated mainly into the inner meso- and macropores, while the outer micropores remained empty, thus serving as a "barricade" against outward dissolution of long-chain lithium polysulfides. On the basis of this systematic design, the sulfur electrode delivered 1412 mAh/g sulfur with excellent capacity retention of 77% after 500 cycles. Also, a control study suggests that even when sulfur is loaded into the outer micropores, the robust cycling performance is preserved by engaging small sulfur crystal structures (S2-4). Furthermore, the hierarchical porous carbon was produced in ultrahigh speed by scalable spray pyrolysis. Each porous carbon particle was synthesized through 5 s of carrier gas flow in a reaction tube.

  8. ZnO based visible-blind UV photodetector by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Inamdar, S. I.; Ganbavle, V. V.; Rajpure, K. Y.

    2014-12-01

    Zinc oxide (ZnO) metal-semiconductor-metal ultraviolet photodetectors were fabricated by economical spray pyrolysis method. The devices have been characterized to investigate the effect of precursor solution concentration on the photoconductive properties of ZnO. The structural, morphological and optical properties of the ZnO thin films were studied using different techniques. The crystal structure, size and lattice parameters have been estimated by X-ray diffraction (XRD) analysis. The UV photodetector device prepared using 0.1 M solution concentration exhibits low dark current and high UV photocurrent of about 134 μA at 5 V bias at 365 nm peak wavelength. The surface morphology and the surface roughness have been studied by AFM analysis. UV-Vis measurements have been used to study the effect of solution concentration on absorption spectra and hence on the band gap. The present device shows fast response in UV region of electromagnetic spectrum and shows almost no response to visible light. The characteristic times for rise and fall of the photocurrent device were 12 s and 9 s respectively. This devices are providing a simple and economical way to fabricate high-performance 'visible-blind' UV detectors and promising for use in large-area UV-A photodetector applications.

  9. Effects of Mn Doping on Zinc Oxide Films Prepared by Spray Pyrolysis Technique

    NASA Astrophysics Data System (ADS)

    Singh, Bhavana; Shrivastava, S. B.; Ganesan, V.

    The work deals with the preparation of Zinc Oxide (ZnO) thin films on microscopic glass substrate by spray pyrolysis technique. The systematic study on the influence of Mn doping up to 15% has been performed. The structural studies revealed that pure and doped film has hexagonal structure. In order to reduce the internal strain due to Mn doping, the crystallite size decreases. The atomic force microscopy (AFM) measurement shows the decrease in grain size and roughness with doping. The resistivity curve shows a clear hump corresponding to smaller Mn doping (x=0.5-4%) around T˜340-365 K. This hump was found to reduce with the increase in Mn concentration and for x≥7.5, beyond which it vanishes completely. This is attributed to critical behavior of resistivity and may be due to the scattering of carriers by magnetic spin fluctuation via exchange interaction. The optical measurement shows the shift in absorption edge of Mn doped ZnO films toward the longer wavelength side. This correlates the reduction in grain size as a function of Mn concentration. The optical bandgap goes down, whereas refractive index increases with dopant concentration.

  10. Synthesis of CuInS2 thin films by spray pyrolysis deposition system

    NASA Astrophysics Data System (ADS)

    Hussain, K. M. A.; Podder, J.; Saha, D. K.

    2013-02-01

    Copper indium disulfide (CuInS2) thin films were deposited on the glass substrate by the locally made spray pyrolysis deposition system. The films were characterized by using energy dispersive analytical X-ray (EDAX) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and UV-VIS-NIR spectrophotometry. The XRD pattern indicated that the prepared CuInS2 thin films are chalcopyrite structure. Lattice parameters and FWHM values were verified by the standard values of JCPDS 270159 file. The EDAX analysis indicated the stoichiometric ratio of 1.14:1:1.88 (CIS-2) thin films. The SEM analysis showed that the average grain size of the film was 100-800 nm and that of XRD data indicate the values of 30-50 nm. The high absorption co-efficient and 1.48 eV band gap of the films indicate that the films are useful as an absorber for photovoltaic application in the solar cell.

  11. Synthesis of nanocrystalline Cu2ZnSnS4 thin films grown by the spray-pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Chandel, Tarun; Singh, Joginder; Rajaram, P.

    2015-08-01

    Spray pyrolysis was used to deposit Cu2ZnSnS4 (CZTS) thin films on soda lime glass substrates at 300 °C. Aqueous solutions of copper chloride, zinc chloride, stannous chloride and thiourea were mixed together to form the spray liquid. The sprayed films were annealed under vacuum at 350 °C, 400 °C and 450 °C. Structural and optical characterization was performed on the CZTS films using X-ray diffraction (XRD) and UV-VIS spectrophotometry. XRD results indicate that the films are single phase nanocrystalline CZTS. Optical studies show that the optical gap values are 1.44 eV for the as-grown film and 1.46 eV, 1.48 eV and 1.49 eV for the films annealed at 350 °C, 400 °C and 450 °C, respectively.

  12. Evolution of Zinc Oxide Nanostructures Grown on Graphene by Ultrasonic Spray Pyrolysis and Its Statistical Growth Modelling.

    PubMed

    Ali, Amgad Ahmed; Hashim, Abdul Manaf

    2015-12-01

    The evolution of zinc oxide nanostructures grown on graphene by alcohol-assisted ultrasonic spray pyrolysis was investigated. The evolution of structures is strongly depended on pyrolysis parameters, i.e., precursor molarity, precursor flow rate, precursor injection/deposition time, and substrate temperature. Field-effect scanning electron microscope analysis, energy dispersive X-ray spectroscopy, X-ray diffraction, and transmission electron microscopy were used to investigate the properties of the synthesized nanostructures and to provide evidence for the structural changes according to the changes in the pyrolysis parameters. The optimum parameters to achieve maximum density and well-defined hexagonally shaped nanorods were a precursor molarity of 0.2 M, an injection flow rate of 6 ml/min, an injection time of 10 min, and a substrate temperature of 250-355 °C. Based on the experimental results, the response surface methodology (RSM) was used to model and optimize the independent pyrolysis parameters using the Box-Behnken design. Here, the responses, i.e., the nanostructure density, size, and shape factor, are evaluated. All of the computations were performed using the Design-Expert software package. Analysis of variance (ANOVA) was used to evaluate the results of the model and to determine the significant values for the independent pyrolysis parameters. The evolution of zinc oxide (ZnO) structures are well explained by the developed modelling which confirms that RSM is a reliable tool for the modelling and optimization of the pyrolysis parameters and prediction of nanostructure sizes and shapes.

  13. Ultrasonic spray pyrolysis growth of ZnO and ZnO:Al nanostructured films: Application to photocatalysis

    SciTech Connect

    Kenanakis, G.; Katsarakis, N.

    2014-12-15

    Highlights: • Al–ZnO thin films and nanostructures were obtained by ultrasonic spray pyrolysis. • The texture and morphology of the samples depend on the deposition parameters. • The photocatalytic degradation of stearic acid was studied upon UV-A irradiation. - Abstract: Pure and Al-doped ZnO (Al = 1, 3, 5%) nanostructured thin films were grown at 400 °C on glass substrates by ultrasonic spray pyrolysis, a simple, environmental-friendly and inexpensive method, using aqueous solutions as precursors. The structural and morphological characteristics of the samples depend drastically on deposition parameters; ZnO nanostructured films, nanopetals and nanorods were systematically obtained by simply varying the precursor solution and/or the spraying time. Transmittance measurements have shown that all samples are transparent in the visible wavelength region. Finally, the photocatalytic properties of the samples were investigated against the degradation of stearic acid under UV-A light illumination (365 nm); both pure and Al-doped ZnO nanostructured thin films show good photocatalytic activity regarding the degradation of stearic acid, due to their good crystallinity and large surface area.

  14. Influence of solution deposition rate on properties of V2O5 thin films deposited by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Abd-Alghafour, N. M.; Ahmed, Naser M.; Hassan, Zai; Mohammad, Sabah M.

    2016-07-01

    Vanadium oxide (V2O5) thin films were deposited on glass substrates by using a cost-efficient spray pyrolysis technique. The films were grown at 350° through thermal decomposition of VCl3 in deionized water with different solution spray rates. The high resolution X-ray diffraction results revealed the formation of nanocrystalline films having orthorhombic structures with preferential orientation along (101) direction. The spray rate influenced the surface morphology and crystallite size of the films. The crystallite size was found to increase whereas the micro-strain was decreased by increasing the spray deposition rates. The increase in crystallite size and decrease in the macrostrain resulted in an improvement in the films' crystallinity. The UV-Visible spectroscopy analysis indicated that the average transmittance of all films lies in the range 75-80 %. The band gap of V2O5 film was decreased from 2.65 to 2.46 eV with increase of the spray deposition rate from 5 ml/min to 10 ml/min. first, second, and third level headings (first level heading).

  15. Structural, optical and electrical properties of undoped and indium doped zinc oxide prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Addou, M.; Moumin, A.; El Idrissi, B.; Regragui, M.; Bougrine, A.; Kachouane, A.; Monty, C.

    1999-02-01

    Thin films of transparent undoped and indium doped ZnO have been deposited using the spray pyrolysis technique. The structural, optical properties and electrical resistivity of these films are investigated as a function of substrate temperature and indium concentration in the solution. X-ray diffraction showed that the films prepared at substrate temperature greater than 300 °C exhibit the hexagonal wurtzite structure with a preferential orientation along the (002) direction. Indium doping changes the orientation of grains to the (110) direction. This result is confirmed by SEM. The composition of the films is also examined by XPS. High transmittance (80%) in the visible region and low resistivity of about 10-1 Ω.cm at room temperature are obtained for thin films prepared under optimum deposition conditions: Ts = 450 ^circC and In/Zn = 2 at.%. Des couches minces transparentes et conductrices d'oxydes de zinc (ZnO) non dopées et dopées indium ont été élaborées par pulvérisation chimique réactive en phase liquide (spray). Les propriétés structurales, optiques et électriques de ces couches ont été étudiées en fonction de certains paramètres expérimentaux tel que la température du dépôt et la concentration d'indium dans la solution. L'étude par diffraction X a montré que les couches préparées à des températures de dépôt supérieures à 300 °C ont une structure hexagonale type wurtzite avec une orientation préférentielle suivant l'axe [002]. Le dopage à l'indium change l'orientation des cristallites suivant la direction [110]. Ce résultat a été confirmé par la microscopie électronique à balayage. La résistivité électrique de l'ordre de 10-1 Ω.cm et la transmission optique de 80 % ont été obtenues pour des couches préparées dans les conditions optimales : Ts = 450 ^circC et In/Zn = 2 at.%.

  16. The Effect of Film Composition on the Texture and Grain Size of CuInS2 Prepared by Spray Pyrolysis

    NASA Technical Reports Server (NTRS)

    Jin, Michael H.; Banger, Kulinder K.; Harris, Jerry D.; Hepp, Aloysius F.

    2003-01-01

    Ternary single-source precursors were used to deposit CuInS2 thin films using chemical spray pyrolysis. We investigated the effect of the film composition on texture, secondary phase formation, and grain size. As-grown films were most often In-rich. They became more (204/220)-oriented as indium concentration increased, and always contained a yet unidentified secondary phase. The (112)-prefened orientation became more pronounced as the film composition became more Cu-rich. The secondary phase was determined to be an In-rich compound based on composition analysis and Raman spectroscopy. In addition, as-grown Cu-rich (112)-oriented films did not exhibit the In-rich compound. Depositing a thin Cu layer prior to the growth of CuInS2 increased the maximum grain size from - 0.5 micron to - 1 micron, and prevented the formation of the In-rich secondary phase.

  17. Investigation on vanadium oxide thin films deposited by spray pyrolysis technique

    SciTech Connect

    Margoni, Mudaliar Mahesh; Mathuri, S.; Ramamurthi, K. E-mail: ramamurthi.k@ktr.srmuniv.ac.in; Babu, R. Ramesh; Sethuraman, K.

    2016-05-06

    Vanadium oxide thin films were deposited at 400 °C by spray pyrolysis technique using 0.1 M aqueous precursor solution of ammonium meta vanadate (AMV) with two different pH values. X-ray diffraction results showed that the film prepared using aqueous precursor AMV solution (solution A; pH 7) is amorphous in nature and the film prepared by adding HNO{sub 3} in the AMV aqua solution A (solution B; pH 3) is polycrystalline in nature. Vanadium oxide film prepared from the precursor solution B is in the mixed phases of V{sub 2}O{sub 5} and V{sub 4}O{sub 7}. Crystallinity is improved for the film prepared using solution B when compared to film prepared from solution A. Crystallite size, strain and dislocation density calculated for the film prepared from solution B is respectively 72.1 nm, 0.4554 × 10{sup −3} lin.{sup −2}m{sup −4} and 1.7263 × 10{sup 14} lin.m{sup −2}. Morphology study revealed that the size of the flakes formed on the surface of the films is influenced by the pH of the precursor solution. Average Visible Transmittance and maximum transmittance of the deposited films exceed 70% and the direct optical band gap value calculated for the films deposited from A and B solution is 1.91 eV and 2.08 eV respectively.

  18. Boron doped nanostructure ZnO films deposited by ultrasonic spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Karakaya, Seniye; Ozbas, Omer

    2015-02-01

    ZnO is an II-VI compound semiconductor with a wide direct band gap of 3.3 eV at room temperature. Doped with group III elements (B, Al or Ga), it becomes an attractive candidate to replace tin oxide (SnO2) or indium tin oxide (ITO) as transparent conducting electrodes in solar cell devices and flat panel display due to competitive electrical and optical properties. In this work, ZnO and boron doped ZnO (ZnO:B) films have been deposited onto glass substrates at 350 ± 5 °C by a cost-efficient ultrasonic spray pyrolysis technique. The optical, structural, morphological and electrical properties of nanostructure undoped and ZnO:B films have been investigated. Electrical resistivity of films has been analyzed by four-probe technique. Optical properties and thicknesses of the films have been examined in the wavelength range 1200-1600 nm by using spectroscopic ellipsometry (SE) measurements. The optical constants (refractive index (n) and extinction coefficient (k)) and the thicknesses of the films have been fitted according to Cauchy model. The optical method has been used to determine the band gap value of the films. Transmission spectra have been taken by UV spectrophotometer. It is found that both ZnO and ZnO:B films have high average optical transmission (≥80%). X-ray diffraction (XRD) patterns indicate that the obtained ZnO has a hexagonal wurtzite type structure. The morphological properties of the films were studied by atomic force microscopy (AFM). The surface morphology of the nanostructure films is found to depend on the concentration of B. As a result, ZnO:B films are promising contender for their potential use as transparent window layer and electrodes in solar cells.

  19. Direct Preparation of Uniformly-Distributed YBa2Cu3O7-x Powders by Spray-Pyrolysis

    NASA Astrophysics Data System (ADS)

    Tohge, Noboru; Tatsumisago, Masahiro; Minami, Tsutomu; Okuyama, Kikuo; Adachi, Motoaki; Kousaka, Yasuo

    1988-06-01

    Fine powders of the compound YBa2Cu3O7-x have been prepared directly by the spray-pyrolysis of aqueous solutions of corresponding metal nitrates. The powders obtained in a temperature range of 900 to 1000°C were spherical and their diameters were uniformly distributed below 1 μm. The crystallinity of these powders was increased with increasing decomposition temperature; an orthorhombic single phase was indeed obtained at 1000°C. The sintered bodies from these powders showed the offset of superconducting transition at 84 K.

  20. Release mitigation spray safety systems for chemical demilitarization applications.

    SciTech Connect

    Leonard, Jonathan; Tezak, Matthew Stephen; Brockmann, John E.; Servantes, Brandon; Sanchez, Andres L.; Tucker, Mark David; Allen, Ashley N.; Wilson, Mollye C.; Lucero, Daniel A.; Betty, Rita G.

    2010-06-01

    Sandia National Laboratories has conducted proof-of-concept experiments demonstrating effective knockdown and neutralization of aerosolized CBW simulants using charged DF-200 decontaminant sprays. DF-200 is an aqueous decontaminant, developed by Sandia National Laboratories, and procured and fielded by the US Military. Of significance is the potential application of this fundamental technology to numerous applications including mitigation and neutralization of releases arising during chemical demilitarization operations. A release mitigation spray safety system will remove airborne contaminants from an accidental release during operations, to protect personnel and limit contamination. Sandia National Laboratories recently (November, 2008) secured funding from the US Army's Program Manager for Non-Stockpile Chemical Materials Agency (PMNSCMA) to investigate use of mitigation spray systems for chemical demilitarization applications. For non-stockpile processes, mitigation spray systems co-located with the current Explosive Destruction System (EDS) will provide security both as an operational protective measure and in the event of an accidental release. Additionally, 'tented' mitigation spray systems for native or foreign remediation and recovery operations will contain accidental releases arising from removal of underground, unstable CBW munitions. A mitigation spray system for highly controlled stockpile operations will provide defense from accidental spills or leaks during routine procedures.

  1. Chemical yields from low-temperature pyrolysis of CCA-treated wood

    Treesearch

    Qirong Fu; Dimitris Argyropolous; Lucian Lucia; David Tilotta; Stan Lebow

    2009-01-01

    Low-temperature pyrolysis offers a feasible option for wood-waste management and the recovery of a variety of useful chemicals. The effect of chromated copper arsenate (CCA) wood preservative on the yield and composition of various pyrolysis products was investigated in the present research. A novel quantitative 31P nuclear magnetic resonance (...

  2. Chemicals from Lignin by Catalytic Fast Pyrolysis, from Product Control to Reaction Mechanism.

    PubMed

    Ma, Zhiqiang; Custodis, Victoria; Hemberger, Patrick; Bährle, Christian; Vogel, Frédéric; Jeschk, Gunnar; van Bokhoven, Jeroen A

    2015-01-01

    Conversion of lignin into renewable and value-added chemicals by thermal processes, especially pyrolysis, receives great attention. The products may serve as feedstock for chemicals and fuels and contribute to the development of a sustainable society. However, the application of lignin conversion is limited by the low selectivity from lignin to the desired products. The opportunities for catalysis to selectively convert lignin into useful chemicals by catalytic fast pyrolysis and our efforts to elucidate the mechanism of lignin pyrolysis are discussed. Possible research directions will be identified.

  3. One-Step Synthesis of Pt/Graphene Composites from Pt Acid Dissolved Ethanol via Microwave Plasma Spray Pyrolysis

    PubMed Central

    Jo, Eun Hee; Chang, Hankwon; Kim, Sun Kyung; Choi, Ji-Hyuk; Park, Su-Ryeon; Lee, Chong Min; Jang, Hee Dong

    2016-01-01

    Pt nanoparticles-laden graphene (Pt/GR) composites were synthesized in the gas phase from a mixture of ethanol and Pt precursor by microwave plasma spray pyrolysis. The morphology of Pt/GR composites has the shape of wrinkled sheets of paper, while Pt nanoparticles (Pt NPs) that are less than 2.6 nm in the mean diameter are uniformly well deposited on the surface of GR sheets stacked in only three layers. The Pt/GR composite prepared with 20 wt% of Pt had the highest specific surface area and electrochemical surface area of up to 402 m2 g−1 and 77 m2 g−1 (Pt), respectively. In addition, the composite showed superior electrocatalytic activity compared with commercial Pt-carbon black. The excellent electrocatalytic activity was attributed to the high specific surface area and electrochemical surface area of the Pt/GR composite directly produced by microwave plasma spray pyrolysis. Thus, it is clearly expected that the Pt/GR composite is a promising material for DMFC catalysts. PMID:27622908

  4. Crumpled rGO-supported Pt-Ir bifunctional catalyst prepared by spray pyrolysis for unitized regenerative fuel cells

    NASA Astrophysics Data System (ADS)

    Kim, In Gyeom; Nah, In Wook; Oh, In-Hwan; Park, Sehkyu

    2017-10-01

    Three-dimensional (3D) crumpled reduced graphene oxide supported Pt-Ir alloys that served as bifunctional oxygen catalysts for use in untized regenerative fuel cells were synthesized by a facile spray pyrolysis method. Pt-Ir catalysts supported on rGO (Pt-Ir/rGOs) were physically characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) to observe change in composition by heat treatment, alloying, and morphological transition of the catalysts. Their catalytic activities and stabilities for the oxygen reduction reaction (ORR) and the oxygen evolution reaction (OER) conditions were electrochemically investigated using cyclic voltammetry (CV), linear sweep voltammetry (LSV), potential cycling and hold tests on the rotating disk electrode (RDE). Pt-Ir/rGO with no post heat-treatment (Pt-Ir/rGO_NP) showed a lower activity for ORR and OER although metal nanoparticles decorated on the support are relatively small. However, Pt-Ir/rGO showed remarkably enhanced activity following heat treatment, depending on temperature. Pt-Ir/rGO heat-treated at 600 °C after spray pyrolysis (Pt-Ir/rGO_P600) exhibited a higher activity and stability than a commercially available Pt/C catalyst kept under the ORR condition, and it also revealed a comparable OER activity and durability versus the commercial unsupported Ir catalyst.

  5. Leidenfrost temperature related CVD-like growth mechanism in ZnO-TFTs deposited by pulsed spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Ortel, Marlis; Wagner, Veit

    2013-01-01

    Zinc oxide thin films were prepared by pulsed spray pyrolysis (SP) from aqueous zinc acetate precursor solution. The deposition behavior of the solution with regard to the pool boiling curve of the solvent was investigated to gain insights of the deposition mechanism which leads to homogeneous and reproducible ZnO layers. The Leidenfrost effect was found to play an important role since the Leidenfrost temperature has to be exceeded to form high quality layers. It is concluded that 3D nucleation of ZnO nano-crystals takes place out of the gaseous phase by a CVD-like process on ITO as well as on SiO2 substrates. Crystal orientation and surface roughness of the zinc oxide layer are found to depend strongly on the substrate. An increasing grain size with film thickness is observed. These findings were utilized to fabricate and investigate the semiconducting properties of the films in ZnO thin film transistors (TFTs). The mobility exceeded 12 cm2 V-1 s-1, the on-set was at 1 V and the on-off current ratio was found to be higher than 108. Hence the morphology and the electrical parameters of the ZnO films deposited by pulsed spray pyrolysis from non-toxic aqueous zinc acetate solution above the Leidenfrost point show excellent properties for electronic applications.

  6. Photocatalytic Activities of Copper Doped Cadmium Sulfide Microspheres Prepared by a Facile Ultrasonic Spray-Pyrolysis Method.

    PubMed

    Su, Jinzhan; Zhang, Tao; Li, Yufeng; Chen, Yubin; Liu, Maochang

    2016-06-15

    Ultrasonic spray pyrolysis is a superior method for preparing and synthesizing spherical particles of metal oxide or sulfide semiconductors. Cadmium sulfide (CdS) photocatalysts with different sizes and doped-CdS with different dopants and doping levels have been synthesized to study their properties of photocatalytic hydrogen production from water. The CdS photocatalysts were characterized with scanning electron microscopy (SEM), X-ray fluorescence-spectrometry (XRF), UV-Vis absorption spectra and X-ray diffraction (XRD) to study their morphological and optical properties. The sizes of the prepared CdS particles were found to be proportional to the concentration of the metal nitrates in the solution. The CdS photocatalyst with smaller size showed a better photocatalytic activity. In addition, Cu doped CdS were also deposited and their photocatalytic activities were also investigated. Decreased bandgaps of CdS synthesized with this method were found and could be due to high density surface defects originated from Cd vacancies. Incorporating the Cu elements increased the bandgap by taking the position of Cd vacancies and reducing the surface defect states. The optimal Cu-doped level was found to be 0.5 mol % toward hydrogen evolution from aqueous media in the presence of sacrificial electron donors (Na₂S and Na₂SO₃) at a pH of 13.2. This study demonstrated that ultrasonic spray pyrolysis is a feasible approach for large-scale photocatalyst synthesis and corresponding doping modification.

  7. Modelling and experimental investigations of thin films of Mg phosphorus-doped tungsten bronzes obtained by ultrasonic spray pyrolysis.

    PubMed

    Jokanović, V; Nedić, Z; Colović, B

    2008-12-01

    In this study, the synthesis of thin films of Mg phosphorus doped tungsten bronzes (MgPTB; MgHPW(12)O(40).29H(2)O) by the self-assembly of nano-structured particles of MgPTB obtained using the ultrasonic spray pyrolysis method was investigated. As the precursor, MgPTB, prepared by the ionic exchange method, was used. Nano-structured particles of MgPTB were obtained using the ultrasonic spray pyrolysis method. The nano-structure of the particles used as the building blocks in the MgPTB thin film were investigated experimentally and theoretically, applying the model given in this article. The obtained data for the mean particle size and their size distribution show a high degree of agreement. These previously tailored particles used for the preparation of thin films during the next synthesis step, by their self-assembly over slow deposition on a silica glass substrate, show how it is possible to create thin MgPTB films under advance projected conditions of the applied physical fields with a fully determined nanostructure of their building block particles, with a relatively small roughness and unique physical properties.

  8. Amorphous Molybdenum Sulfide/Carbon Nanotubes Hybrid Nanospheres Prepared by Ultrasonic Spray Pyrolysis for Electrocatalytic Hydrogen Evolution.

    PubMed

    Ye, Zhifeng; Yang, Jia; Li, Bo; Shi, Lei; Ji, Hengxing; Song, Li; Xu, Hangxun

    2017-04-11

    Developing cost-effective electrocatalysts with high activity and stability for hydrogen evolution reaction (HER) plays an important role in modern hydrogen economy. Amorphous molybdenum sulfide (MoSx ) has recently emerged as one of the most promising alternatives to Pt-based catalysts in HER, especially in acidic electrolytes. Here this study reports a simple ultrasonic spray pyrolysis method to synthesize hybrid HER catalysts composed of MoSx firmly attached on entangled carbon nanotube nanospheres (MoSx /CNTs). This synthetic process is fast, continuous, highly durable, and amenable to high-volume production with high yields and exceptional quality. The MoSx /CNTs hybrid catalyst prepared at 300 °C exhibits a low overpotential of 168 mV at the current density of 10 mA cm(-2) with a small Tafel slope of 36 mV dec(-1) . Electrochemical measurements and X-ray photoelectron spectroscopy analyses reveal that the CNT network not only promotes the charge transfer in corresponding HER process but also enhances the stability of the active sites in MoSx . This work demonstrates that ultrasonic spray pyrolysis is a reliable and versatile approach for synthesizing amorphous MoSx -based HER catalysts.

  9. One-Step Synthesis of Pt/Graphene Composites from Pt Acid Dissolved Ethanol via Microwave Plasma Spray Pyrolysis.

    PubMed

    Jo, Eun Hee; Chang, Hankwon; Kim, Sun Kyung; Choi, Ji-Hyuk; Park, Su-Ryeon; Lee, Chong Min; Jang, Hee Dong

    2016-09-13

    Pt nanoparticles-laden graphene (Pt/GR) composites were synthesized in the gas phase from a mixture of ethanol and Pt precursor by microwave plasma spray pyrolysis. The morphology of Pt/GR composites has the shape of wrinkled sheets of paper, while Pt nanoparticles (Pt NPs) that are less than 2.6 nm in the mean diameter are uniformly well deposited on the surface of GR sheets stacked in only three layers. The Pt/GR composite prepared with 20 wt% of Pt had the highest specific surface area and electrochemical surface area of up to 402 m(2) g(-1) and 77 m(2) g(-1) (Pt), respectively. In addition, the composite showed superior electrocatalytic activity compared with commercial Pt-carbon black. The excellent electrocatalytic activity was attributed to the high specific surface area and electrochemical surface area of the Pt/GR composite directly produced by microwave plasma spray pyrolysis. Thus, it is clearly expected that the Pt/GR composite is a promising material for DMFC catalysts.

  10. One-Step Synthesis of Pt/Graphene Composites from Pt Acid Dissolved Ethanol via Microwave Plasma Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Jo, Eun Hee; Chang, Hankwon; Kim, Sun Kyung; Choi, Ji-Hyuk; Park, Su-Ryeon; Lee, Chong Min; Jang, Hee Dong

    2016-09-01

    Pt nanoparticles-laden graphene (Pt/GR) composites were synthesized in the gas phase from a mixture of ethanol and Pt precursor by microwave plasma spray pyrolysis. The morphology of Pt/GR composites has the shape of wrinkled sheets of paper, while Pt nanoparticles (Pt NPs) that are less than 2.6 nm in the mean diameter are uniformly well deposited on the surface of GR sheets stacked in only three layers. The Pt/GR composite prepared with 20 wt% of Pt had the highest specific surface area and electrochemical surface area of up to 402 m2 g‑1 and 77 m2 g‑1 (Pt), respectively. In addition, the composite showed superior electrocatalytic activity compared with commercial Pt-carbon black. The excellent electrocatalytic activity was attributed to the high specific surface area and electrochemical surface area of the Pt/GR composite directly produced by microwave plasma spray pyrolysis. Thus, it is clearly expected that the Pt/GR composite is a promising material for DMFC catalysts.

  11. Low Temperature Synthesis of Fluorine-Doped Tin Oxide Transparent Conducting Thin Film by Spray Pyrolysis Deposition.

    PubMed

    Ko, Eun-Byul; Choi, Jae-Seok; Jung, Hyunsung; Choi, Sung-Churl; Kim, Chang-Yeoul

    2016-02-01

    Transparent conducting oxide (TCO) is widely used for the application of flat panel display like liquid crystal displays and plasma display panel. It is also applied in the field of touch panel, solar cell electrode, low-emissivity glass, defrost window, and anti-static material. Fluorine-doped tin oxide (FTO) thin films were fabricated by spray pyrolysis of ethanol-added FTO precursor solutions. FTO thin film by spray pyrolysis is very much investigated and normally formed at high temperature, about 500 degrees C. However, these days, flexible electronics draw many attentions in the field of IT industry and the research for flexible transparent conducting thin film is also required. In the industrial field, indium-tin oxide (ITO) film on polymer substrate is widely used for touch panel and displays. In this study, we investigated the possibility of FTO thin film formation at relatively low temperature of 250 degrees C. We found out that the control of volume of input precursor and exhaust gases could make it possible to form FTO thin film with a relatively low electrical resistance, less than 100 Ohm/sq and high optical transmittance about 88%.

  12. Liquid-feed flame spray pyrolysis synthesis of oxide nanopowders for the processing of ceramic composites

    NASA Astrophysics Data System (ADS)

    Taylor, Nathan John

    In the liquid-feed flame spray pyrolysis (LF-FSP) process, alcohol solutions of metalloorganic precursors are aerosolized by O2 and combusted. The metal oxide combustion products are rapidly quenched (< 10 ms) from flame temperatures of 1500°C to temperatures < 400° C, limiting particle growth. The resulting nanopowders are typically agglomerated but unaggregated. Here, we demonstrate two processing approaches to dense materials: nanopowders with the exact composition, and mixed single metal oxide nanopowders. The effect of the initial degree of phase separation on the final microstructures was determined by sintering studies. Our first studies included the production of yttrium aluminum garnet, Y3Al5O12 (YAG), tubes which we extruded from a thermoplastic/ceramic blend. At equivalent final densities, we found finer grain sizes in the from the mixed Y2O3 and Al2 O3 nanopowders, which was attributed to densification occurring before full transformation to the YAG phase. The enhanced densification in production of pure YAG from the reactive sintering process led us to produce composites in the YAG/alpha-Al 2O3 system. Finally, a third Y2O3 stabilized ZrO2 (YSZ) phase was added to further refine grain sizes using the same two processing approaches. In a separate study, single-phase metastable Al2O3 rich spinels with the composition MO•3Al 2O3 where M = Mg, Ni, and Co were sintered to produce dense MAl2O4/alpha-Al2O3 composites. All of these studies provide a test of the bottom-up approach; that is, how the initial length scale of mixing affects the final composite microstructure. Overall, the length scale of mixing is highly dependent upon the specific oxide composites studied. This work provides a processing framework to be adopted by other researchers to further refine microstructural size. LF-FSP flame temperatures were mapped using different alcohols with different heats of combustion: methanol, ethanol, 1-propanol, and n-butanol. The effect of different

  13. Superior Na-ion storage properties of high aspect ratio SnSe nanoplates prepared by a spray pyrolysis process

    NASA Astrophysics Data System (ADS)

    Park, Gi Dae; Lee, Jong-Heun; Kang, Yun Chan

    2016-06-01

    SnSe nanoplates with thin and uniform morphology are prepared by one-pot spray pyrolysis, and are examined as anode materials for Na-ion batteries. During the spray pyrolysis process, metallic Se and Sn are prepared from SeO2 and SnO2, respectively, under a reducing atmosphere. Metallic Sn and metalloid Se, with melting points of 232 and 221 °C, respectively, form a melted Sn-Se mixture, which reacts exothermally to form SnSe nanocrystals. Several of these nanocrystals are grown simultaneously forming a micron-sized powder. Complete elimination of the excess amount of metalloid Se, by forming H2Se gas, results in aggregation-free SnSe nanoplates. The aspect ratio of these nanoplates is as high as 11.3. The discharge capacities for the SnSe nanoplates, prepared from spray solutions containing 100, 400, and 800% of the stoichiometric SeO2 content needed to form SnSe, are 407, 558, and 211 mA h g-1, respectively, after 50 cycles at a constant current density of 0.3 A g-1 their capacity retentions calculated from the second cycle onwards are 77, 100, and 60%, respectively. The phase pure SnSe nanoplates with a high aspect ratio show good cycling and rate performances for Na-ion storage.SnSe nanoplates with thin and uniform morphology are prepared by one-pot spray pyrolysis, and are examined as anode materials for Na-ion batteries. During the spray pyrolysis process, metallic Se and Sn are prepared from SeO2 and SnO2, respectively, under a reducing atmosphere. Metallic Sn and metalloid Se, with melting points of 232 and 221 °C, respectively, form a melted Sn-Se mixture, which reacts exothermally to form SnSe nanocrystals. Several of these nanocrystals are grown simultaneously forming a micron-sized powder. Complete elimination of the excess amount of metalloid Se, by forming H2Se gas, results in aggregation-free SnSe nanoplates. The aspect ratio of these nanoplates is as high as 11.3. The discharge capacities for the SnSe nanoplates, prepared from spray solutions

  14. Finding the chemistry in biomass pyrolysis: Millisecond chemical kinetics and visualization

    NASA Astrophysics Data System (ADS)

    Krumm, Christoph

    Biomass pyrolysis is a promising thermochemical method for producing fuels and chemicals from renewable sources. Development of a fundamental understanding of biomass pyrolysis chemistry is difficult due to the multi-scale and multi-phase nature of the process; biomass length scales span 11 orders of magnitude and pyrolysis phenomena include solid, liquid, and gas phase chemistry in addition to heat and mass transfer. These complexities have a significant effect on chemical product distributions and lead to variability between reactor technologies. A major challenge in the study of biomass pyrolysis is the development of kinetic models capable of describing hundreds of millisecond-scale reactions of biomass into lower molecular weight products. In this work, a novel technique for studying biomass pyrolysis provides the first- ever experimental determination of kinetics and rates of formation of the primary products from cellulose pyrolysis, providing insight into the millisecond-scale chemical reaction mechanisms. These findings highlight the importance of heat and mass transport limitations for cellulose pyrolysis chemistry and are used to identify the length scales at which transport limitations become relevant during pyrolysis. Through this technique, a transition is identified, known as the reactive melting point, between low and high temperature depolymerization. The transition between two mechanisms of cellulose decompositions unifies the mechanisms that govern low temperature char formation, intermediate pyrolysis conditions, and high temperature gas formation. The conditions under which biomass undergoes pyrolysis, including modes of heat transfer, have been shown to significantly affect the distribution of biorenewable chemical and fuel products. High-speed photography is used to observe the liftoff of initially crystalline cellulose particles when impinged on a heated surface, known as the Leidenfrost effect for room-temperature liquids. Order

  15. Modifying Optical Properties of ZnO Films by Forming Zn[subscript 1-x] Co[subscript x]O Solid Solutions via Spray Pyrolysis

    ERIC Educational Resources Information Center

    Bentley, Anne K.; Weaver, Gabriela C.; Russell, Cianan B.; Fornes, William L.; Choi, Kyoung-Shin; Shih, Susan M.

    2007-01-01

    A simple and cost-effective experiment for the development and characterization of semiconductors using Uv-vis spectroscopy is described. The study shows that the optical properties of ZnO films can be easily modified by forming Zn[subscript 1-x] Co[subscript x]O solid solutions via spray pyrolysis.

  16. Modifying Optical Properties of ZnO Films by Forming Zn[subscript 1-x] Co[subscript x]O Solid Solutions via Spray Pyrolysis

    ERIC Educational Resources Information Center

    Bentley, Anne K.; Weaver, Gabriela C.; Russell, Cianan B.; Fornes, William L.; Choi, Kyoung-Shin; Shih, Susan M.

    2007-01-01

    A simple and cost-effective experiment for the development and characterization of semiconductors using Uv-vis spectroscopy is described. The study shows that the optical properties of ZnO films can be easily modified by forming Zn[subscript 1-x] Co[subscript x]O solid solutions via spray pyrolysis.

  17. CdS or CdSe decorated TiO2 nanotube arrays from spray pyrolysis deposition: use in photoelectrochemical cells.

    PubMed

    Shin, Kahee; Seok, Sang Il; Im, Sang Hyuk; Park, Jong Hyeok

    2010-04-14

    In the present work we report on an investigation of TiO(2) nanotube arrays sensitized by low band-gap materials, such as CdS and CdSe, prepared by the one-step spray pyrolysis deposition method, which is very suitable for mass production, and their performance in photoelectrochemical cells.

  18. Effect of annealing on the properties of nanocrystalline CuInSSe thin films deposited by spray pyrolysis

    SciTech Connect

    Shrotriya, Vipin Rajaram, P.

    2015-08-28

    The effect of annealing CuInSSe thin films, which were grown on glass substrates using the spray pyrolysis technique from spray solutions having S/Se ionic ratio 0.6, were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and optical transmission measurements. The CuInSSe films were co-deposited from an aqueous solution containing CuCl{sub 2}, InCl{sub 3}, thiourea and SeO{sub 2}. EDC was used as a complexing agent and films were deposited at the constant temperature 300°C. Post annealing (at 350°C) was used to improve the structural, morphological and optical properties of CuInSSe thin films. From the results, it is found that the films are single phase, p-type in conductivity having the chalcopyrite structure. From the Scherrer formula the average size of the films was found to be in the range (15-28) nm. Optical studies show that the optical band gap value increases slightly from 1.35 eV to 1.37 eV with annealing for films grown from spray solutions having S/Se ionic ratio 0.6.

  19. Effect of annealing on the properties of nanocrystalline CuInSSe thin films deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Shrotriya, Vipin; Rajaram, P.

    2015-08-01

    The effect of annealing CuInSSe thin films, which were grown on glass substrates using the spray pyrolysis technique from spray solutions having S/Se ionic ratio 0.6, were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and optical transmission measurements. The CuInSSe films were co-deposited from an aqueous solution containing CuCl2, InCl3, thiourea and SeO2. EDC was used as a complexing agent and films were deposited at the constant temperature 300°C. Post annealing (at 350°C) was used to improve the structural, morphological and optical properties of CuInSSe thin films. From the results, it is found that the films are single phase, p-type in conductivity having the chalcopyrite structure. From the Scherrer formula the average size of the films was found to be in the range (15-28) nm. Optical studies show that the optical band gap value increases slightly from 1.35 eV to 1.37 eV with annealing for films grown from spray solutions having S/Se ionic ratio 0.6.

  20. Systematically reduced chemical mechanisms for sulfur oxidation and pyrolysis

    SciTech Connect

    Cerru, F.G.; Kronenburg, A.; Lindstedt, R.P.

    2006-08-15

    Recent research on sulfur chemistry has predominantly focused on the high-temperature chemistry typical of flames. The present work initially assesses the ability of a sulfur submechanism featuring 12 sulfur-containing species and 70 reversible reactions to reproduce measured data. The functionality includes the pyrolysis and oxidation of hydrogen sulfide as well as the chemistry of sulfur dioxide. The sensitivity of reaction paths to alternative rate determinations has been analyzed. In particular, the consumption paths of sulfanyl and the rates of the reactions involved in the SO{sub 2}-catalyzed radical recombination highlight existing uncertainties. Despite these difficulties, the detailed mechanism generally produces good agreement with experimental data. Most industrial combustion processes are turbulent and turbulence-chemistry interactions cannot be included through high-Damkohler-number limit approximations. Accordingly, chemical kinetic effects need to be accounted for and the implementation of systematically reduced mechanisms has the potential to increase the computational efficiency. The detailed reaction mechanism is thus subsequently reduced to six independent scalars with HSO, HOSO, HOSO{sub 2}, HSSH, and S in steady state. The reduced mechanism provides good agreement over the range of conditions studied. Further simplifications are made in the context of oxides of sulfur and a two-step mechanism involving SO, SO{sub 2}, and SO{sub 3} is derived and shown to retain good agreement with the experimental data for a more limited set of conditions. (author)

  1. Single-Step Synthesis of Cubic Y2O3:Eu3+ Nanophosphor by Flame Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Lee, Jae Seok; Lee, Jinhyung; Han, Hyuksu; Kumar, Purushottam; Singh, Rajiv K.

    2016-12-01

    In this report, we investigated a single-step process for formation of high crystallinity Y2O3:Eu3+ red nanophosphor by flame spray pyrolysis (FSP) without post-heat treatments. Crystallinity of as-formed nanophosphor particle was improved by addition of urea to the nitrate-based liquid precursor. Urea increased the temperature in the flame zone thus ensuring Y2O3:Eu3+ formation at higher flame temperature. Higher temperature reached during combustion of urea promoted the formation of better crystallinity, nano-sized and spherical-shaped particles. The effect of urea in the precursor to obtain high-efficiency Y2O3:Eu3+ nanophosphor was studied.

  2. Electrical properties of Cu4ZnSnS2/ZnS heterojunction prepared by ultrasonic spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Guitouni, S.; Khammar, M.; Messaoudi, M.; Attaf, N.; Aida, M. S.

    2016-12-01

    Cu2ZnSnS4 (CZTS)/ZnS heterojunctions have been prepared by a successive deposition of ZnS and CZTS thin films by ultrasonic spray pyrolysis technique on glass substrates. The cupric chloride concentration has been varied in the starting solution in order to investigate its influence on device properties. CZTS/ZnS heterojunctions were characterized by recording their current-voltage characteristics at different temperatures. The obtained results exhibit a good rectifying behavior of the realized heterojunction. Analysis of these results yields saturation current, series resistance and ideality factor determination. From the activation energy of saturation current we inferred that the thermal emission through the barrier height is the dominant mechanism of the reverse current rather than the defects contribution.

  3. Optical, electrical and surface properties of annealed CdO:Mg thin films prepared by spray pyrolysis

    SciTech Connect

    Karakaya, Seniye E-mail: oozbas@ogu.edu.tr; Ozbas, Omer E-mail: oozbas@ogu.edu.tr

    2013-12-16

    The use of transparent conducting oxides in optoelectronic and photovoltaic devices has encouraged research on this field in recent years. Especially, cadmium oxide is a promising material for solar cell application but also for photodiodes and gas sensors. Mg doped CdO (CdO:Mg) films have been prepared on glass substrates by the ultrasonic spray pyrolysis (USP) technique. After the production, the films have been annealed in air atmosphere at 475°C and half hour. Results on surface, optical and electrical properties of the films as a function of the thermal annealing have been reported. Thicknesses of the films have been determined by the filmetrics thin film measurement system. Transmission and absorbance spectra have been taken by UV-vis spectrophotometer. Atomic Force Microscopy (AFM) analysis indicates that the roughness of the surface decreases upon increasing Mg concentration. The minimum resistivity value of the films was 2×10{sup −3} Ω cm.

  4. Low-temperature spray-pyrolysis of FeS2 films and their electrical and optical properties

    NASA Astrophysics Data System (ADS)

    Orletskii, I. G.; Mar'yanchuk, P. D.; Maistruk, E. V.; Solovan, M. N.; Brus, V. V.

    2016-01-01

    Iron disulfide (FeS2) films with a wide range of electrical resistivities 100 Ω cm ⩽ ρ ⩽ 800 kΩ cm, a high adhesion to the substrate, and a resistance to aggressive media have been prepared by the spray pyrolysis of aqueous solutions of the salts FeCl3 · 6H2O and (NH2)2CS at low temperatures in the range 250°C ⩽ T S ⩽ 400°C. It has been found that the FeS2 films have a high transmittance T ≈ 60-70% and are characterized by a sharp transmission edge. It has been shown that the optical band gap for direct ( E g op = 2.19-2.78 eV) and indirect ( E g 'op = 1.26-1.36 eV) optical transitions depends on the conditions of film preparation.

  5. Growth and characterization of V{sub 2}O{sub 5} nanorods deposited by spray pyrolysis at low temperatures

    SciTech Connect

    Abd-Alghafour, N. M. Ahmed, Naser M. Hassan, Zai.; Mohammad, Sabah M.; Bououdina, M.

    2016-07-06

    Vanadium pentoxide (V{sub 2}O{sub 5}) nanorods were deposited by spray pyrolysis on preheated glass substrates at low temperatures. The influence of substrate temperature on the crystallization of V{sub 2}O{sub 5} has been investigated. X-ray diffraction analysis (XRD) revealed that the films deposited at T{sub sub} = 300°C were orthorhombic structures with preferential along (001) direction. Formation of nanorods from substrate surface which led to the formation of films with small-sized and rod-shaped nanostructure is observed by field scanning electron microscopy. Optical transmittance in the visible range increases to reach a maximum value of about 80% for a substrate temperature of 350°C. PL spectra reveal one main broad peak centered around 540 nm with high intensity.

  6. Optical, electrical and surface properties of annealed CdO:Mg thin films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Karakaya, Seniye; Ozbas, Omer

    2013-12-01

    The use of transparent conducting oxides in optoelectronic and photovoltaic devices has encouraged research on this field in recent years. Especially, cadmium oxide is a promising material for solar cell application but also for photodiodes and gas sensors. Mg doped CdO (CdO:Mg) films have been prepared on glass substrates by the ultrasonic spray pyrolysis (USP) technique. After the production, the films have been annealed in air atmosphere at 475°C and half hour. Results on surface, optical and electrical properties of the films as a function of the thermal annealing have been reported. Thicknesses of the films have been determined by the filmetrics thin film measurement system. Transmission and absorbance spectra have been taken by UV-vis spectrophotometer. Atomic Force Microscopy (AFM) analysis indicates that the roughness of the surface decreases upon increasing Mg concentration. The minimum resistivity value of the films was 2×10-3 Ω cm.

  7. Studies on structural and optical properties of Cu doped CdxZn1-XS thin films by Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Rane, D. S.; Patil, L. A.

    2012-06-01

    Cu doped CdxZn1-XS thin films have been produced by Spray Pyrolysis technique at 2750C±50C. This work describes structural, surface morphology and optical (UV-Vis) properties of as-deposited Cu doped CdxZn1-XS thin films as a function of Zn in the solution. It has been observed that CdZnS films have hexagonal structure and the grain sizes are found to increase with increasing Zn content in the solution. The energy band gap values obtained are 2.330, 2,447, 2.716, 3.044 and 3.519eV for Zn as 0, 25, 50, 75, and 100% respectively.

  8. Spin wave study and optical properties in Fe-doped ZnO thin films prepared by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Lmai, F.; Moubah, R.; El Amiri, A.; Abid, Y.; Soumahoro, I.; Hassanain, N.; Colis, S.; Schmerber, G.; Dinia, A.; Lassri, H.

    2016-07-01

    We investigate the magnetic and optical properties of Zn1-xFexO (x = 0, 0.03, 0.05, and 0.07) thin films grown by spray pyrolysis technique. The magnetization as a function of temperature [M (T)] shows a prevailing paramagnetic contribution at low temperature. By using spin wave theory, we separate the M (T) curve in two contributions: one showing intrinsic ferromagnetism and one showing a purely paramagnetic behavior. Furthermore, it is shown that the spin wave theory is consistent with ab-initio calculations only when oxygen vacancies are considered, highlighting the key role played by structural defects in the mechanism driving the observed ferromagnetism. Using UV-visible measurements, the transmittance, reflectance, band gap energy, band tail, dielectric coefficient, refractive index, and optical conductivity were extracted and related to the variation of the Fe content.

  9. Structure and morphology of Sn1-xAlxO2 thin films prepared by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Bhatia, G.; Gupta, V. K.; Shrivastava, S. B.; Patidar, M. M.; Ganesan, V.

    2017-05-01

    Al-doped tin oxide [Sn1-x AlxO2(x=0, 0.03 and 0.09)] thin films were prepared by spray pyrolysis technique (SPT) on glass substrate. XRD and AFM techniques have been used for the investigation of structural and morphological properties of the films. XRD spectra reveal the polycrystalline nature of the films having tetragonal structure. AFM images show an evolution in the morphology in the sense that larger grains of SnO2 are converted in some smaller grains upon Al inclusion. This may be due to the strain developed due to the Al substitution. The roughness has been found to decrease with the increase in Al concentration.

  10. Investigation of the properties of nanostructured Li-doped NiO films using the modified spray pyrolysis method

    PubMed Central

    2013-01-01

    The lithium-doped nickel oxide (L-NiO) films were synthetized using the modified spray pyrolysis method with a two-step grown process. By observing the spectra of X-ray photoemission spectroscopy of L-NiO films, the intensity of Ni 2p3/2 peak of Ni3+ bonding state increases with increasing Li concentration that causes the decrease of transparency and resistivity. The L-NiO films with optimum characteristics were obtained at Li = 8 at%, where a p-type resistivity of 4.1 × 10−1 Ω cm and optical transparency above 76% in the visible region are achieved. PMID:23331663

  11. Effect of lithium on linear and nonlinear optical properties of Sn-doped zinc oxide prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Rherari, A.; Addou, M.; Sofiani, Z.; El jouad, M.; Jbilou, M.; Diani, M.

    2017-03-01

    Li and Sn codoped ZnO (LTZO) thin films have been successfully deposited on heated glass substrates at 450°C using the spray pyrolysis technique, the effect of lithium of Sn-doped zinc oxide on the structural, morphological, optical and nonlinear optical properties was investigated using X-ray diffraction, transmission, the RMS average surface roughness, and third harmonic generation (THG). The value of optical band gap Eg was found to be decreased from 3.24 eV to 3.16 eV when the concentration of Li from 0 to 7%, while the concentration of Sn is fixed at 2%.The doping of ZnO films improves the nonlinear response and the highest susceptibility value χ (3) =13.422 × 10-12 (esu) is found at concentration of lithium 7%.

  12. Effect of annealing on the properties of Sb doped ZnO thin films prepared by spray pyrolysis technique

    SciTech Connect

    Kumar, N. Sadananda; Bangera, Kasturi V.; Shivakumar, G. K.

    2014-01-28

    Sb doped ZnO thin films have been deposited on glass substrate at 450°C using spray pyrolysis technique. The X-ray diffraction studies revealed that the as deposited films are polycrystalline in nature with (100) preferred orientation. Whereas the films annealed at 450° C for 6h show a preferential orientation along (101) direction. Crystallites size varies from 15.7 nm to 34.95 nm with annealing duration. The Scanning electron microscopic analysis shows the plane and smooth surface of the films. The optical properties of annealed films have shown a variation in the band gap between 3.37 eV and 3.19 eV. Transparency of as grown and annealed films decreases from 78 % to 65% respectively in the visible region. The electrical conductivity of the as grown film shows an increase in the electrical conductivity by one order of magnitude with increase in the annealing duration.

  13. Study of optical and structural properties of CZTS thin films grown by co-evaporation and spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Moreno, R.; Ramirez, E. A.; Gordillo Guzmán, G.

    2016-02-01

    Results regarding optical and structural properties of Cu2ZnSnS4 (CZTS) thin films prepared by co-evaporation using a novel procedure are compared with those obtained with CZTS films grown using a solution based route. The lattice strain ε and crystallite size D of CZTS films prepared by co-evaporation and by spray pyrolysis were estimated through X-ray diffraction (XRD) measurements using Williamson-Hall-isotropic strain model. The results of estimated average crystallite size of CZTS films by Scherrer and Williamson-Hall plot methods were compared with AFM (atomic force microscopy) measurements. It was found that the average crystallite size measured by Williamson-Hall plot methods agree quite well with AFM results. Further, information regarding the influence of preparation method on both, crystalline phases and the formation of structural defects was achieved through Raman and Urbach energy measurements.

  14. Synthesis and characterization of Co-doped zinc oxide nanorods prepared by ultrasonic spray pyrolysis and hydrothermal methods

    NASA Astrophysics Data System (ADS)

    Febrianti, Y.; Putri, N. A.; Sugihartono, I.; Fauzia, V.; Handoko, D.

    2017-07-01

    ZnO nanorods was synthesized by using ultrasonic spray pyrolysis deposition process and grown by hydrothermal method on a glass substrate. The influences of varying Co doping in structural, morphological and optical properties were investigated by X-Ray Diffractometer (XRD), Scanning Electron Microscopy (SEM), and UV-Visible (UV-Vis) spectrometry, respectively. All the nanorods exhibit polycrystalline wurtzite structure with smaller crystalline size on the Co-doped nanorods. The nanorods also show no orientation alignment and random particle size. Interestingly, the nanorods with 3 wt.% Co doped shows high absorbance at UV and visible region indicating that optical properties of the ZnO nanorods have been modified by Co doping.

  15. Dopant-induced bandgap shift in Al-doped ZnO thin films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Hung-Chun Lai, Henry; Basheer, Tahseen; Kuznetsov, Vladimir L.; Egdell, Russell G.; Jacobs, Robert M. J.; Pepper, Michael; Edwards, Peter P.

    2012-10-01

    A series of 1 at. % Al-doped ZnO (AZO) films were deposited onto glass substrates by a spray pyrolysis technique. We find that the observed blue shift in the optical bandgap of 1% AZO films is dominated by the Burstein Moss effect. The Fermi level for an 807 nm thick AZO film rose by some 0.16 eV with respect to the edge of the conduction band. By controlling the film thickness, all AZO films exhibit the same lattice strain values. The influence of strain-induced bandgap shift was excluded by selecting films with nearly the same level of bandgap volume-deformation potentials, and the differences in out-plain strain and in-plain stress remained effectively constant.

  16. Effect of In doping on the properties and antibacterial activity of ZnO films prepared by spray pyrolysis.

    PubMed

    Manoharan, C; Pavithra, G; Dhanapandian, S; Dhamodharan, P

    2015-01-01

    Pure and In-doped ZnO thin films were deposited onto glass substrates by spray pyrolysis technique. XRD results showed that all films were polycrystalline in nature with the wurzite structure. A change in preferential orientation from (002) to (101) plane was observed with increase in content of Indium. A reduce in crystallite size was observed with increase of In content. The small sized grains with the porous nature of the film was observed from SEM analysis. AFM study depicted polycrystalline nature and uniformly distributed grains with small pores in the doped film. A decrease in band gap was noticed with increase in In content. The absence of green emission in PL spectra indicated the decreased oxygen defects. The decrease in the resistivity with increase of Hall mobility was noted for the doped film. A better antibacterial activity was observed against Staphylococcus aureus by doped ZnO thin film.

  17. Ethylene glycol assisted spray pyrolysis for the synthesis of hollow BaFe12O19 spheres

    SciTech Connect

    Xu, X; Park, J; Hong, YK; Lane, AM

    2015-04-01

    Hollow spherical BaFe12O19 particles were synthesized by spray pyrolysis from a solution containing ethylene glycol (EG) and precursors at 1000 degrees C. The effects of EG concentration on particle morphology, crystallinity and magnetic properties were investigated. The hollow spherical particles were found to consist of primary particles, and higher EG concentration led to a bigger primary particle size. EG concentration did not show much effect on the hollow particle size. Better crystallinity and higher magnetic coercivity were obtained with higher EG concentration, which is attributed to further crystallization with the heat produced from EG combustion. Saturation magnetization (emu/g) decreased with increasing EG concentration due to residual carbon from EG incomplete combustion, contributing as a non-magnetic phase to the particles. Published by Elsevier B.V.

  18. One-step synthesis of luminescent YVO4:Eu(3+)/γ-Al2O3 nanocomposites by spray pyrolysis.

    PubMed

    Riul, André; Justino, Larissa G; Caiut, José Maurício A

    2017-06-09

    Spray pyrolysis (SP) easily affords nano or sub-micro phosphor particles even on an industrial scale. However, control of the coordination environment around the emitting ion is inefficient, and the final solid matrix will dictate the symmetry of the emitter. Moreover, the fast heat treatment typical of SP usually results in heterogeneous symmetry sites. This paper aimed to obtain inorganic matrices incorporated with phosphors by SP while keeping the symmetry of the emitting ion unchanged along the pyrolysis process. Nanoparticles consisting of Eu(3+)-doped YVO4 phosphors with average diameter of 15 nm were prepared by the co-precipitation method and were subsequently incorporated into the alumina matrix by SP, to yield YVO4:Eu(3+)/γ-Al2O3 composite particles with mean size of 600 nm. X-ray powder diffraction confirmed that the vanadate particles were incorporated into the alumina matrix, and that the γ-Al2O3 phase emerged. The band due to the [Formula: see text] → Eu(3+) transition intensified as a consequence of the incorporation of YVO4:Eu(3+) into alumina-the suppression effects caused by the surface properties of the YVO4:Eu(3+) phosphor nanoparticles diminished, while the structure of Eu(3+) remained unchanged in the matrix.

  19. Low-Temperature Preparation of Tungsten Oxide Anode Buffer Layer via Ultrasonic Spray Pyrolysis Method for Large-Area Organic Solar Cells.

    PubMed

    Ji, Ran; Zheng, Ding; Zhou, Chang; Cheng, Jiang; Yu, Junsheng; Li, Lu

    2017-07-18

    Tungsten oxide (WO₃) is prepared by a low-temperature ultrasonic spray pyrolysis method in air atmosphere, and it is used as an anode buffer layer (ABL) for organic solar cells (OSCs). The properties of the WO₃ transition metal oxide material as well as the mechanism of ultrasonic spray pyrolysis processes are investigated. The results show that the ultrasonic spray pyrolysized WO₃ ABL exhibits low roughness, matched energy level, and high conductivity, which results in high charge transport efficiency and suppressive recombination in OSCs. As a result, compared to the OSCs based on vacuum thermal evaporated WO₃, a higher power conversion efficiency of 3.63% is reached with low-temperature ultrasonic spray pyrolysized WO₃ ABL. Furthermore, the mostly spray-coated OSCs with large area was fabricated, which has a power conversion efficiency of ~1%. This work significantly enhances our understanding of the preparation and application of low temperature-processed WO₃, and highlights the potential of large area, all spray coated OSCs for sustainable commercial fabrication.

  20. Low-Temperature Preparation of Tungsten Oxide Anode Buffer Layer via Ultrasonic Spray Pyrolysis Method for Large-Area Organic Solar Cells

    PubMed Central

    Ji, Ran; Zheng, Ding; Zhou, Chang; Cheng, Jiang; Yu, Junsheng; Li, Lu

    2017-01-01

    Tungsten oxide (WO3) is prepared by a low-temperature ultrasonic spray pyrolysis method in air atmosphere, and it is used as an anode buffer layer (ABL) for organic solar cells (OSCs). The properties of the WO3 transition metal oxide material as well as the mechanism of ultrasonic spray pyrolysis processes are investigated. The results show that the ultrasonic spray pyrolysized WO3 ABL exhibits low roughness, matched energy level, and high conductivity, which results in high charge transport efficiency and suppressive recombination in OSCs. As a result, compared to the OSCs based on vacuum thermal evaporated WO3, a higher power conversion efficiency of 3.63% is reached with low-temperature ultrasonic spray pyrolysized WO3 ABL. Furthermore, the mostly spray-coated OSCs with large area was fabricated, which has a power conversion efficiency of ~1%. This work significantly enhances our understanding of the preparation and application of low temperature-processed WO3, and highlights the potential of large area, all spray coated OSCs for sustainable commercial fabrication. PMID:28773177

  1. Metal-insulator transition characteristics of vanadium dioxide thin films synthesized by ultrasonic nebulized spray pyrolysis of an aqueous combustion mixture

    NASA Astrophysics Data System (ADS)

    Bharathi, R.; Naorem, Rameshwari; Umarji, A. M.

    2015-08-01

    We report the synthesis of high quality vanadium dioxide (VO2) thin films by a novel spray pyrolysis technique, namely ultrasonic nebulized spray pyrolysis of aqueous combustion mixture (UNSPACM). This simple and cost effective two step process involves synthesis of a V2O5 film on an LaAlO3 substrate followed by a controlled reduction to form single phase VO2. The formation of M1 phase (P21/c) is confirmed by Raman spectroscopic studies. A thermally activated metal-insulator transition (MIT) was observed at 61 ^\\circ C, where the resistivity changes by four orders of magnitude. Activation energies for the low conduction phase and the high conduction phase were obtained from temperature variable resistance measurements. The infrared spectra also show a dramatic change in reflectance from 13% to over 90% in the wavelength range of 7-15 μ m. This indicates the suitability of the films for optical switching applications at infrared frequencies.

  2. Thin Film Electrode Materials Li4Ti5O12 and LiCoO2 Prepared by Spray Pyrolysis Method

    NASA Astrophysics Data System (ADS)

    Takahashi, M.; Tani, J.; Kido, H.; Hayashi, A.; Tadanaga, K.; Tatsumisago, M.

    2011-05-01

    The Li4Ti5O12 and the LiCoO2 have been considered as promising candidates of electrode materials for all-solid-state lithium secondary batteries. The spray pyrolysis method is a useful economical technique to prepare various thicknesses of oxide films though have not been intensively studied for fabrication of thin film lithium batteries. Thin films of Li4Ti5O12 and LiCoO2 electrode materials about 100-400 nm were prepared on quartz and gold substrates by the spray pyrolysis method by using Liacac and, TiO(acac)4 or Co(acac)3 with DMF solvent as starting materials. Electric properties as electrode materials for lithium batteries were estimated by using 3 probe liquid cells with liquid electrolyte LiPF6 in EC-DMC and Li metal as reference and counter electrodes. Structure and morphology of the films were investigated by XRD and SEM. Crystalline Li4Ti5O12 and LiCoO2 thin films were found to be prepared over 700 °C of substrate temperature. Cyclic voltammograms of the Li4Ti5O12 electrode thin films showed sharp oxidation and reduction peaks around 1.6 and 1.5 V, respectively. Charge-discharge curves for both Li4Ti5O12 and LiCoO2 electrode thin films showed discharge plateaus around 1.4 and 3.8 V with about 80 mAhg-1 of capacity. These results showed that these electrode thin films prepared by the spray pyrolysis method are electrochemically active and spray pyrolysis method is a promising technique to prepare thin film electrode materials.

  3. Value-added organonitrogen chemicals evolution from the pyrolysis of chitin and chitosan.

    PubMed

    Liu, Chao; Zhang, Huiyan; Xiao, Rui; Wu, Shubin

    2017-01-20

    Thermogravimetric characteristics of chitin and chitosan and their potentials to produce value-added organonitrogen chemicals were separately evaluated via TG/DSC-FTIR and Py-GC/MS. Results shown that chitin had the better thermal stability and higher activation energy than chitosan because of the abundant acetamido group. Furthermore, the dominated volatilization in active pyrolysis of chitin contributed to its endothermic property, whereas the charring in chitosan led to the exothermal. During fast pyrolysis, the acetamido group in chitin and chitosan was converted into acetic acid or acetamide. Typical products from chitosan pyrolysis were aza-heterocyclic chemicals, i.e. pyridines, pyrazines, and pyrroles, with the total selectivity of 50.50% at 600°C. Herein, selectivity of pyrazine compounds was up to 22.99%. These aza-heterocyclic chemicals came from the nucleophilic addition reaction of primary amine and carbonyl. However, main reaction during chitin pyrolysis was ring-opening degradation, which led to the formation of acetamido chemicals, especially acetamido acetaldehyde with the highest selectivity of 27.27% at 450°C. In summary, chitosan had the potential to produce aza-heterocyclic chemicals, and chitin to acetamido chemicals.

  4. Synthesis of hollow cobalt oxide nanopowders by a salt-assisted spray pyrolysis process applying nanoscale Kirkendall diffusion and their electrochemical properties.

    PubMed

    Ju, Hyeon Seok; Cho, Jung Sang; Kim, Jong Hwa; Choi, Yun Ju; Kang, Yun Chan

    2015-12-21

    A new concept for preparing hollow metal oxide nanopowders by salt-assisted spray pyrolysis applying nanoscale Kirkendall diffusion is introduced. The composite powders of metal oxide and indecomposable metal salt are prepared by spray pyrolysis. Post-treatment under a reducing atmosphere and subsequent washing using distilled water produce aggregation-free metal nanopowders. The metal nanopowders are then transformed into metal oxide hollow nanopowders by nanoscale Kirkendall diffusion. Co3O4 hollow nanopowders are prepared as first target materials. A cobalt oxide-NaCl composite powder prepared by spray pyrolysis transforms into several Co3O4 hollow nanopowders by several treatment processes. The discharge capacities of the Co3O4 nanopowders with filled and hollow structures at a current density of 1 A g(-1) for the 150th cycle are 605 and 775 mA h g(-1), respectively. The hollow structure formed by nanoscale Kirkendall diffusion improves the lithium-ion storage properties of Co3O4 nanopowders.

  5. Fabrication and characterization of n-ZnO:Eu/p-ZnO:(Ag, N) homojunction by spray pyrolysis

    SciTech Connect

    Swapna, R.; Kumar, M.C. Santhosh

    2014-01-01

    Graphical abstract: In this paper authors report the fabrication of ZnO homojunction by the deposition of 2 at.% Eu doped ZnO (n-ZnO:Eu) layer grown over the 4 at.% Ag–N dual acceptor doped ZnO (p-ZnO:(Ag, N)) layer by spray pyrolysis technique. The as-grown n-type and p-type ZnO films on glass substrates have been characterized by Hall measurements, X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), UV–vis and luminescence spectroscopy techniques. Hall measurement shows that 4 at.% ZnO:(Ag, N) film exhibits p-type conductivity with high hole concentration of 2.17 × 10{sup 18} cm{sup −3} and n-type conductivity is observed in the ZnO:Eu film. The current–voltage characteristics measured from the two-layer structure show typical rectifying characteristics of p–n homojunction with a low turn on voltage of about 1.85 V. I–V characteristics of the n-ZnO:Eu/p-ZnO:(Ag, N) homojunction. - Highlights: • The n-ZnO:Eu/p-ZnO:(Ag, N) homojunction is fabricated and characterized. • Low resistive and stable p-type ZnO films are achieved by dual acceptor-doping. • Homojunction with best dual-doped ZnO film shows good rectifying characteristics. • The fabricated ZnO homojunction is suitable for optoelectronic devices. - Abstract: In the present study, the authors report the fabrication of ZnO homojunction by the deposition of 2 at.% Eu doped ZnO (n-ZnO:Eu) layer grown over the 4 at.% Ag–N dual acceptor doped ZnO (p-ZnO:(Ag, N)) layer by spray pyrolysis technique. The as-grown n-type and p-type ZnO films on glass substrates have been characterized by Hall measurements, X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), UV–vis and luminescence spectroscopy techniques. Hall measurement shows that 4 at.% ZnO:(Ag, N) film exhibits p-type conductivity with high hole concentration of 2.17 × 10{sup 18} cm{sup −3} and n-type conductivity is observed in the ZnO:Eu film. The current–voltage characteristics measured from the two

  6. ZnO-based thin film transistors employing aluminum titanate gate dielectrics deposited by spray pyrolysis at ambient air.

    PubMed

    Afouxenidis, Dimitrios; Mazzocco, Riccardo; Vourlias, Georgios; Livesley, Peter J; Krier, Anthony; Milne, William I; Kolosov, Oleg; Adamopoulos, George

    2015-04-08

    The replacement of SiO2 gate dielectrics with metal oxides of higher dielectric constant has led to the investigation of a wide range of materials with superior properties compared with SiO2. Despite their attractive properties, these high-k dielectrics are usually manufactured using costly vacuum-based techniques. To overcome this bottleneck, research has focused on the development of alternative deposition methods based on solution-processable metal oxides. Here we report the application of spray pyrolysis for the deposition and investigation of Al2x-1·TixOy dielectrics as a function of the [Ti(4+)]/[Ti(4+)+2·Al(3+)] ratio and their implementation in thin film transistors (TFTs) employing spray-coated ZnO as the active semiconducting channels. The films are studied by UV-visible absorption spectroscopy, spectroscopic ellipsometry, impedance spectroscopy, atomic force microscopy, X-ray diffraction and field-effect measurements. Analyses reveal amorphous Al2x-1·TixOy dielectrics that exhibit a wide band gap (∼4.5 eV), low roughness (∼0.9 nm), high dielectric constant (k ∼ 13), Schottky pinning factor S of ∼0.44 and very low leakage currents (<5 nA/cm(2)). TFTs employing stoichiometric Al2O3·TiO2 gate dielectrics and ZnO semiconducting channels exhibit excellent electron transport characteristics with low operating voltages (∼10 V), negligible hysteresis, high on/off current modulation ratio of ∼10(6), subthreshold swing (SS) of ∼550 mV/dec and electron mobility of ∼10 cm(2) V(-1) s(-1).

  7. Electrical and morphological properties of conducting layers formed from the silver-glass composite conducting powders prepared by spray pyrolysis.

    PubMed

    Jung, D S; Koo, H Y; Kang, Y C

    2010-03-01

    Ag-glass composite powders with various glass contents and excellent conducting properties were prepared by spray pyrolysis. Irrespective of the glass content, all the prepared powders were found to comprise spherical particles with nonaggregation characteristics. The crystal structure of the powder particles resembled that of pure Ag particles, irrespective of the glass content. Conducting layers formed from pure Ag did not melt even when sintered at 400 degrees C. On the other hand, conducting layers formed from composite powders containing 3 and 5 wt% glass melted when sintered at 400 degrees C. The optimum glass content of the composite powders was 3 wt% at sintering temperatures of 400 and 450 degrees C. However, the optimum glass content decreased to 1 wt% when the sintering temperature was increased to 550 degrees C. The lowest specific resistances of the conducting layers formed from the composite powders were 5.3 and 2.3 microohms-cm at sintering temperatures of 400 and 550 degrees C, respectively.

  8. Electrochemical performance of gadolinia-doped ceria (CGO) electrolyte thin films for ITSOFC deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Reolon, Raquel Pereira; Halmenschlager, Cibele Melo; Neagu, Roberto; de Fraga Malfatti, Célia; Bergmann, Carlos Pérez

    2014-09-01

    Solid Oxide Fuel Cell is an attractive, efficient, alternative source of power generation. However several challenges remained for this technology to be viable. These challenges include high power density, degradation rate, and cost. One way to decrease the SOFC cost is to use stainless steel interconnector. To be able to use a stainless steel interconnector one of the challenges is to find a way to produce an electrolyte, which does not need sintering at high temperature. This work presents the results of the process applied to gadolinia-doped ceria thin films deposited in cycles by spray pyrolysis. The aim of this work was to obtain thin, dense, and continuous CGO coatings, which has electrochemical performance suitable to be used as electrolyte for SOFC. The results obtained show that the air flow rate influenced the droplets size and hence the film quality. X-ray diffraction analysis showed that the films were crystalline after the deposition. Electrochemical tests showed maximum power density of 510 mW cm-2 at 650 °C with a thickness average of 3.30 μm when the film was deposited in 12 cycles showing that the film has a potential to be used as an electrolyte for ITSOFC on metal support.

  9. Transparent heaters made by ultrasonic spray pyrolysis of nanograined SnO2 layers on soda-lime glass substrates

    NASA Astrophysics Data System (ADS)

    Gharesi, Mohsen; Ansari, Mohammad; Akbari-Saatlu, Mehdi

    2017-07-01

    Transparent heaters have become important owing to the increasing demand in automotive and display device manufacturing industries. Indium tin oxide (ITO) is the most commonly used material for the production of transparent heaters, but the fabrication cost is high as the indium resources are diminishing fast. This has been the driving force behind the intense research for discovering more durable and cost-effective alternatives. Tin oxide, with its high temperature stability and coexisting high levels of conductivity and transparency, can replace expensive ITO in the fabrication of transparent heaters. Here, we propose nanograined tin oxide films deposited using ultrasonic spray pyrolysis as the raw material for the fabrication of transparent heaters. Silver contacts are paste printed on the deposited SnO2 layers, which provide the necessary connections to the external circuitry. Deposition of films having sheet resistance in the 120 Ω □-1 range takes only ~5 min and the utilized methods are fully scalable to the mass production level. Durability tests, carried out for weeks of continuous operation at different elevated temperatures, demonstrated the long load life of the produced heaters.

  10. The effect of solution concentration on the physical and electrochemical properties of vanadium oxide films deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M. M.

    2013-10-01

    Vanadium oxide thin films were prepared on glass substrates by using the spray pyrolysis technique. The effect of solution concentration (0.1 M, 0.2 M and 0.3 M) on the nanostructural, electrical, optical, and electrochromic properties of deposited films were investigated using X-ray diffraction, scanning electron microscopy, UV—vis spectroscopy, and cyclic volta-metrics. The X-ray diffraction shows that only the sample at 0.1 M has a single β-V2O5 phase and the others have mixed phases of vanadium oxide. The lowest sheet resistance was obtained for the samples prepared at 0.3 M solution. It was also found that the optical transparency of the samples changes from 70% to 35% and the optical band gap of the samples was in the range of 2.20 to 2.41 eV, depending on the morality of solution. The cycle voltammogram shows that the sample prepared at 0.3 M has one-step electerochoromic but the other samples have two-step electerochoromic. The results show a correlation between the cycle voltammogram and the physical properties of the films.

  11. Structural and magnetic properties of Co-doped ZnO thin films grown by ultrasonic spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Baghdad, R.; Lemée, N.; Lamura, G.; Zeinert, A.; Hadj-Zoubir, N.; Bousmaha, M.; Bezzerrouk, M. A.; Bouyanfif, H.; Allouche, B.; Zellama, K.

    2017-04-01

    Cobalt-doped ZnO thin films with several different percentage of Co from 0 up to 15 at% were synthesized via a cheap, simple and versatile method i.e. ultrasonic spray pyrolysis at atmospheric pressure and a substrate temperature of 350 °C. The structure of the as-prepared samples was characterized by X-ray diffraction (XRD), Raman spectroscopy and FTIR. The Co-doping effect is revealed by the presence of three additional peaks around 235, 470 and 538 cm-1 respect to the Raman spectra of the unsubstituted film. Fourier transform infrared spectroscopy (FTIR) put in evidence the decrease of the bond force constant f with increasing Co-doping. By ultra-violet visible near infrared (UV-Vis-NIR) spectroscopy on Co-doped samples it was possible to show the presence of additional absorption bands at approximately 570, 620 and 660 nm suggesting that Co2+ ions do not change their oxidation when substituted to zinc and the ZnO lattice does not change its wurtzite structure as well. Finally, all our samples exhibit a paramagnetic behavior without any trace of intrinsic room temperature ferromagnetism.

  12. High-throughput screening of nanoparticle catalysts made by flame spray pyrolysis as hydrocarbon/NO oxidation catalysts.

    PubMed

    Weidenhof, B; Reiser, M; Stöwe, K; Maier, W F; Kim, M; Azurdia, J; Gulari, E; Seker, E; Barks, A; Laine, R M

    2009-07-08

    We describe here the use of liquid-feed flame spray pyrolysis (LF-FSP) to produce high surface area, nonporous, mixed-metal oxide nanopowders that were subsequently subjected to high-throughput screening to assess a set of materials for deNO(x) catalysis and hydrocarbon combustion. We were able to easily screen some 40 LF-FSP produced materials. LF-FSP produces nanopowders that very often consist of kinetic rather than thermodynamic phases. Such materials are difficult to access or are completely inaccessible via traditional catalyst preparation methods. Indeed, our studies identified a set of Ce(1-x)Zr(x)O(2) and Al(2)O(3)-Ce(1-x)Zr(x)O(2) nanopowders that offer surprisingly good activities for both NO(x) reduction and propane/propene oxidation both in high-throughput screening and in continuous flow catalytic studies. All of these catalysts offer activities comparable to traditional Pt/Al(2)O(3) catalysts but without Pt. Thus, although Pt-free, they are quite active for several extremely important emission control reactions, especially considering that these are only first generation materials. Indeed, efforts to dope the active catalysts with Pt actually led to lower catalytic activities. Thus the potential exists to completely change the materials used in emission control devices, especially for high-temperature reactions as these materials have already been exposed to 1500 degrees C; however, much research must be done before this potential is verified.

  13. Luminescence properties of Eu-complex formations into ordered mesoporous silica particles obtained by the spray pyrolysis process

    NASA Astrophysics Data System (ADS)

    Rocha, Lucas A.; Freiria, Janaina do C.; Caiut, José Maurício A.; Ribeiro, Sidney J. L.; Messaddeq, Younes; Verelst, Marc; Dexpert-Ghys, Jeannette

    2015-08-01

    Ordered mesoporous, highly luminescent SiO2 particles have been synthesized by spray pyrolysis from solutions containing tetraethylorthosilicate (TEOS), Eu(NO3)3.6H2O, and cetyltrimethylammonium bromide (CTAB) as structure-directing agents. The 1,10-phenantroline (Phen) molecules were coordinated in a post-synthesis step by a simple wet impregnation method. In addition, other matrices were also prepared by the encapsulation of europium complex Eu(fod)3 (where fod = 6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedionato) into mesoporous silica, and then the Phen molecules were encapsulated by different impregnation steps, after which the luminescence properties were investigated. The obtained materials were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder x-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Powders with polydisperse spherical grains were obtained, displaying an ordered hexagonal array of mesochannels. Luminescence results revealed that Phen molecules had been successfully coordinated as an additional ligand in the Eu(fod)3 complex into the channels of the mesoporous particles without disrupting the structure.

  14. High-performance p-n heterojunction photodetectors based on V2O5 nanorods by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Abd-Alghafour, N. M.; Ahmed, Naser. M.; Hassan, Z.; Bououdina, M.

    2016-09-01

    V2O5 heterojunction photodetector was fabricated onto Si(100) substrate using spray pyrolysis technique. Vanadium chloride (VCl3) precursor with 0.05 M concentration was used to prepare V2O5 thin film. The structural, morphological, and optical properties of V2O5 thin film were investigated. High-resolution X-ray diffraction analysis confirmed the formation of V2O5 thin film with a preferred orientation along (110) plane. Morphological observations using field emission scanning electron microscope displayed the formation of thin film with rod-like nanostructure. The optical properties examined by photoluminescence spectroscopy indicated a high-intensity visible peak centered around 530 nm. Current-voltage ( I- V) characteristics of the fabricated device under visible light exhibited low dark current and high photocurrent of 540 μA at 3 V bias voltages. Upon exposure to 560 nm visible light (24 mW/cm2) at 3 V, the device displayed a good sensitivity of 20.16 × 102. In addition, the internal gain of the photodiode was 21.16, and the photoresponse peak was 50 mA/W. The rise and recovery times of the photodiode were calculated to be 0.127 and 0.526 s under visible light (560 nm, 24 mW/cm2), respectively, at 3 V.

  15. Influence of concentration and volume of precursor on the electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Ingole, R. S.; Fugare, B. Y.; Lokhande, B. J.

    2016-04-01

    Vanadium oxide (V2O5) thin films have been prepared by spray pyrolysis using different concentrations and volumes of precursor solution via aqueous route at 673K deposition temperature. The influences of concentration and volume on the structural, morphological and electrochemical properties of the deposited samples are studied well. X - ray diffraction study shows orthorhombic crystal structure with V2O5 phase, confirmed by FTIR spectroscopy. Scanning electron microscopy shows granular, homogeneous and dense surface morphology. Cyclic voltammetery of all samples carried at all scan rates. Samples prepared using 0.05M, 40 ml of precursor solution shows highest specific capacitance 428.25 F/gm at 5 mV/s, Charge discharge behavior exhibits specific energy 18.73 Wh/kg, specific power 36.00 kW/kg, columbic efficiency 87.50 %. Impedance spectroscopy study was carried in the frequency range 1mHz - 1MHz, reveals pseudocapacitive behavior of the electrode exhibiting internal resistance 1.34 ohm.

  16. Effect of S-doping on structural, optical and electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M.-M.

    2013-12-01

    In this research, S-doped vanadium oxide thin films, with doping levels from 0 to 40 at.%, are prepared by spray pyrolysis technique on glass substrates. For electrochemical measurements, the films were deposited on florin-tin oxide coated glass substrates. The effect of S-doping on structural, electrical, optical and electrochemical properties of vanadium oxide thin films was studied. The x-ray diffractometer analysis indicated that most of the samples have cubic β-V2O5 phase structure with preferred orientation along [200]. With increase in the doping levels, the structure of the samples tends to be amorphous. The scanning electron microscopy images show that the structure of the samples is nanobelt-shaped and the width of the nanobelts decreases from nearly 100 to 40 nm with increase in the S concentration. With increase in the S-doping level, the sheet resistance and the optical band gap increase from 940 to 4015 kΩ/square and 2.41 to 2.7 eV, respectively. The cyclic voltammogram results obtained for different samples show that the undoped sample is expanded and the sample prepared at 20 at.% S-doping level has sharper anodic and cathodic peaks.

  17. Optical and electrical properties of lithium doped nickel oxide films deposited by spray pyrolysis onto alumina substrates

    NASA Astrophysics Data System (ADS)

    Garduño, I. A.; Alonso, J. C.; Bizarro, M.; Ortega, R.; Rodríguez-Fernández, L.; Ortiz, A.

    2010-11-01

    Non-doped and lithium doped nickel oxide crystalline films have been prepared onto quartz and crystalline alumina substrates at high substrate temperature (600 °C) by the pneumatic spray pyrolysis process using nickel and lithium acetates as source materials. The structure of all the deposited films was the crystalline cubic phase related to NiO, although this crystalline structure was a little bit stressed for the films with higher lithium concentration. The grain size had values between 60 and 70 nm, almost independently of doping concentration. The non-doped and lithium doped films have an energy band gap of the order of 3.6 eV. Hot point probe results show that all deposited films have a p-type semiconductor behavior. From current-voltage measurements it was observed that the electrical resistivity decreases as the lithium concentration increases, indicating that the doping action of lithium is carried out. The electrical resistivity changed from 10 6 Ω cm for the non-doped films up to 10 2 Ω cm for the films prepared with the highest doping concentration.

  18. Nickel-induced microwheel-like surface morphological evolution of ZnO thin films by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Tarwal, N. L.; Shinde, P. S.; Oh, Y. W.; Cerc Korošec, Romana; Patil, P. S.

    2012-11-01

    Nickel-zinc oxide (Ni-ZnO) thin films were deposited onto glass and tin-doped indium oxide-coated glass substrates by using a pneumatic spray pyrolysis technique at 450 °C from aqueous solutions of zinc acetate and nickel acetate precursors. The effect of nickel doping on structural, morphological and optical properties of the ZnO thin films has been studied. The X-ray diffraction patterns confirmed the polycrystalline nature of the films having hexagonal crystal structure. Ni-ZnO films with appropriate nickel doping revealed the occurrence of novel wheel-like surface morphology. The absorption edge of the Ni-ZnO films showed a red shift, meaning that the optical band gap energy decreases as the nickel doping concentration increases. A growth model is developed and proposed for the novel wheel-like morphology. All the thin films exhibited room-temperature photoluminescence. Pure ZnO and Ni-ZnO thin films were tested for their photoelectrochemical performance in 0.5 M Na2SO4 electrolyte solution. The values of fill factor and open circuit voltage were improved for the Ni-ZnO thin films.

  19. Mössbauer studies of nanocrystalline ZnFe2O4 particles prepared by spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Kurian, Jessyamma; John, Subin P.; M, Jacob Mathew; Reddy, V. R.; E, Abraham K.; Prasad, V. S.

    2015-02-01

    This paper reports the synthesis and characterization of nanoparticles of Zn Fe2O4 by spray pyrolysis method. XRD studies indicates that the particle formed are ultra fine (20 nm) associated with strain. The particle size is confirmed by TEM analysis. The room temperature Mossbauer spectrum shows only a doublet which could be indicative of either paramaganetic or superparamagnetic phase. The value of isomer shift is in the range 0.34±0.01 mm/s while quadruple splitting is in the range 0.48±0.01 mm/s. A series of low temperature studies has been performed and the spectra obtained at 20 K and 5K show the presence of two well resolved sextets, which are attributed to the Fe3+ ion in the tetrahedral and octahedral sites of the spinel structure. The application of external magnetic field yields a better fitting resolution of the sub spectra between A and B sites. The temperature dependant and in-field measurements yielded valuable insights about magnetic phase (superparamagnetic), local cation distribution among A sites and B sites, inversion parameter (δ =0.74), canted spin alignment (ψA = 29.58, ψB= 48.46) and the blocking temperature (TB= 50 K).

  20. Fourier transform infrared and Raman spectroscopic properties of Cd1-xSbxS films deposited by ultrasonic spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Özer, T.; Aksay, S.; Köse, S.

    2010-07-01

    Cd1-xSbxS films (x = 0.0, 0.1 and 0.2) were deposited by the ultrasonic spray pyrolysis method. The films were deposited on glass substrates at temperatures of 300 °C. The effect of antimony doping on the structural and vibrational (FT-IR and Raman) properties of cadmium sulphide films were examined. Structural investigations of the films showed the hexagonal polycrystalline structure and that the incorporation of antimony leads to substantial changes in the structural characteristics of CdS films. The preferential orientation of the Cd1-xSbxS films shifts from (002) to (101) with increasing x values. The Raman spectrum for CdS films is dominated by an intense band at 301.5 cm-1(1LO) assigned to the first-order longitudinal optic phonon and the second-order phonon peak 598.5 cm-1 (2LO). Cd1-xSbxS films have been prepared and their FT-IR (400-4000 cm-1) spectra are reported for the first time. The vibrations at 550-1164 cm-1 are caused by Cd-S and C-O stretching vibrations.

  1. Optical properties and mechanisms of current flow in Cu2ZnSnS4 films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Orletskii, I. G.; Mar'yanchuk, P. D.; Solovan, M. N.; Brus, V. V.; Maistruk, E. V.; Kozyarskii, D. P.; Abashin, S. L.

    2016-05-01

    Thin films Cu2ZnSnS4 (up to 0.9 μm thick) with p-type conductivity and band gap E g = 1.54 eV have been prepared by the spray pyrolysis of 0.1 M aqueous solutions of the salts CuCl2 · 2H2O, ZnCl2 · 2H2O, SnCl4 · 5H2O, and (NH2)2CS at a temperature T S = 290°C. The electrophysical properties of the films have been analyzed using the model for polycrystalline materials with electrically active grain boundaries. The energy and geometric parameters of the grain boundaries have been determined as follows: the height of the barriers is E b ≈ 0.045-0.048 eV, and the thickness of the depletion region is δ ≈ 3.25 nm. The effective concentrations of charge carriers p 0 = 3.16 × 1018 cm-3 and their mobilities in crystallites μ p = 85 cm2/(V s) have been found using the technique for determining the kinetic parameters from the absorption spectra of thin films at a photon energy hν ≈ E g . The density of states at grain boundaries N t = 9.57 × 1011 cm-2 has been estimated.

  2. Growth of tin oxide thin films composed of nanoparticles on hydrophilic and hydrophobic glass substrates by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Paloly, Abdul Rasheed; Satheesh, M.; Martínez-Tomás, M. Carmen; Muñoz-Sanjosé, Vicente; Rajappan Achary, Sreekumar; Bushiri, M. Junaid

    2015-12-01

    In this paper, we have demonstrated the growth of tin oxide (SnO2) thin films composed of nanoparticles on hydrophobic (siliconized) and hydrophilic (non-siliconized) glass substrates by using the spray pyrolysis technique. X-ray diffraction (XRD) analysis confirmed the formation of SnO2 thin films with tetragonal rutile-phase structure. Average particle size of nanoparticles was determined to be in the range of 3-4 nm measured from the front view images obtained by a field emission gun scanning electron microscope (FESEM), while the size of nanoparticle clusters, when present, were in the range of 11-20 nm. Surface morphology of SnO2 films grown over hydrophobic substrates revealed larger isolated particles which are less crowded compared to the highly crowded and agglomerated smaller particles in films on hydrophilic substrates. Blue shift in the band gap is observed in samples in which the average particle size is slightly larger than the exciton Bohr radius. Photoluminescence (PL) analysis of samples grown over hydrophobic substrates exhibited an intense defect level emission and a weak near band edge emission. The enhanced visible emission from these SnO2 thin films is attributed to lattice defects formed during the film growth due to the mismatch between the film and the hydrophobic substrate surface.

  3. Ethanol sensing of V2O5 thin film prepared by spray pyrolysis technique: Effect of substrate to nozzle distance

    NASA Astrophysics Data System (ADS)

    Immanuel, P.; Prakash, A. Arockia; Mohan, C. Raja

    2017-05-01

    In the present investigation V2O5 thin films were prepared by spray pyrolysis by varying substrate to nozzle distance (SND) from 20 to 35 cm in steps of 5 cm. The structural studies by XRD results indicates that the crystallinity increases with increase in SND along (101), (201) orientation and for the film prepared at 30 cm gives a good crystallinity. The SEM image shows that the change in morphology, which strongly depends on the SND. Above 30 cm it slightly affects the surface morphology of the V2O5 thinfilm due to agglomeration. The presence of elemental constituents is confirmed from EDAX analysis. The band gap of the film prepared at 30 cm has a lowest value of 2.1 eV. The electrical studies like I-V, Hall Effect measurement and the conductivity is maximum for the film prepared at 30 cm. The ethanol sensing of the prepared film has been studied using Keithley source meter and the detailed results are presented and discussed.

  4. Photoelectrochemical performance of W-doped BiVO4 thin-films deposited by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Holland, Stephen K.; Dutter, Melissa R.; Lawrence, David J.; Reisner, Barbara A.; DeVore, Thomas C.

    2013-09-01

    The effect of tungsten doping and hydrogen annealing treatments on the photoelectrochemical (PEC) performance of bismuth vanadate (BiVO4) photoanodes for solar water splitting was studied. Thin films of BiVO4 were deposited on ITO-coated glass slides by ultrasonic spray pyrolysis of an aqueous solution containing bismuth nitrate and vanadium oxysulfate. Tungsten doping was achieved by adding either silicotungstic acid (STA) or ammonium metatungstate (AMT) in the aqueous precursor. The 1.7 μm - 2.2 μm thick films exhibited a highly porous microstructure. Undoped films that were reduced at 375 ºC in 3% H2 exhibited the largest photocurrent densities under 0.1 W cm-2 AM1.5 illumination. This performance enhancement was believed to be due to the formation of oxygen vacancies, which are shallow electron donors, in the films. Films doped with 1% or 5% tungsten from either STA or AMT exhibited reduced photoelectrochemical performance and greater sample-to-sample performance variations. Powder X-ray diffraction data of the undoped films indicated that they were comprised primarily of the monoclinic scheelite phase while unidentified phases were also present. Scanning electron microscopy showed slightly different morphology characteristics for the Wdoped films. It is surmised that the addition of W in the deposition process promoted the morphology differences and the formation of different phases, thus reducing the PEC performance of the photoanode samples. Significant PEC performance variability was also observed among films deposited using the described process.

  5. Optical, Electrical, and Morphological Effects of Yttrium Doping of Cadmium Oxide Thin Films Grown by Ultrasonic Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Tombak, Ahmet; Baturay, Silan; Kilicoglu, Tahsin; Ocak, Yusuf Selim

    2016-11-01

    CdO films doped with Y concentrations of 0%, 1%, 2%, and 3% were deposited onto soda lime glass using ultrasonic spray pyrolysis. The effect of the doping level on the structural, morphological, optical, and electrical properties of the films was characterized. X-ray diffraction analysis was used to establish that all of the samples were polycrystalline and to determine the structural parameters, i.e., lattice spacing (d), phases and associated (hkl) planes, grain size (D), and dislocation density (δ). The films possessed high conductivity and carrier concentration, showing n-type semiconducting behavior. The films were almost transparent over the range from 600 nm to 1100 nm. The energy bandgap was 2.43 eV, 2.53 eV, 2.68 eV, and 2.70 eV for Y doping of 0%, 1%, 2%, and 3%, respectively. The refractive index and extinction coefficient of the films over the range from 700 nm to 1100 nm were determined by spectroscopic ellipsometry. Atomic force microscopy revealed the effect of Y doping on the surface morphology of the CdO films.

  6. Spray pyrolysis prepared yellow to red color tunable Sr₁-xCaxSe:Eu²+ phosphors for white LED.

    PubMed

    Chung, Wonkeun; Jung, Hyunchul; Lee, Chang Hun; Kim, Jihyun; Kim, Sung Hyun

    2012-06-04

    The spherical and submicron size of Sr₁-xCaxSe:Eu²⁺ phosphors were successfully prepared by ultrasonic spray pyrolysis. The phosphors adopted a cubic structure, and the replacement of Sr²⁺ with Ca²⁺ decreased the lattice parameter. The Sr₁-xCaxSe:Eu²⁺ showed broad and strong excitation under 420-460 nm blue light, and the emission band could be tuned from 565 to 607 nm by increasing the Ca²⁺ ratio in the host lattice. In addition, the doping of Zn²⁺ into Sr²⁺ or Ca²⁺ enhanced the emission intensity with a small red shift due to the change in crystal field strength and nephelauxetic effects. The warm and high CRI of white LED was achieved using blue LED pumped with blending phosphors of 612 nm emitting Ca₀.₉₈Zn₀.₀₂Se:Eu²⁺ and 565 nm emitting YAG. The correlated color temperatures and CRI were 4719.2K, and 86.3, respectively, and an acceptable color variation was also observed at operating currents ranging from 20 to 70 mA.

  7. In vitro and in vivo antimicrobial properties of silver-containing hydroxyapatite prepared via ultrasonic spray pyrolysis route.

    PubMed

    Honda, Michiyo; Kawanobe, Yusuke; Ishii, Ken; Konishi, Toshiisa; Mizumoto, Minori; Kanzawa, Nobuyuki; Matsumoto, Morio; Aizawa, Mamoru

    2013-12-01

    Hydroxyapatite (HAp), with its high biocompatibility and osteoconductivity, readily absorbs proteins, amino acids and other substances, which in turn favor the adsorption and colonization of bacteria. To prevent bacterial growth and biofilm formation on HAp discs, silver-containing (1-20 mol%) HAp (Ag-HAp) powders were synthesized using an ultrasonic spray pyrolysis (USSP) technique. The X-ray diffraction (XRD) peaks were very broad, indicating low crystallinity, and this induced the release of Ag(+) ions from Ag-HAp powders. In addition, a gradual increase in Ca(2+) ion release was observed. These results suggest that dissolution of Ca(2+) ion in Ag-HAp triggered the release of Ag(+) ions. The antimicrobial efficacy of Ag-HAp disc was tested against Staphylococcus aureus. Samples with Ag contents of more than 5 mol% were found to be highly effective against bacterial colonization and biofilm formation in vitro. In vivo antibacterial tests using bioluminescent strains also showed reductions in the viability of bacteria with Ag-HAp (5 mol%) discs. Biocompatibility tests using a modified Transwell® insert method showed that Ag-HAp (5 mol%) discs have negative effects on osteoblast proliferation. These results indicate that Ag-HAp (5 mol%) has effective antibacterial activity and good biocompatibility both in vitro and in vivo together with good biocompatibility, thus confirming its utility as a bactericidal material.

  8. Influence of concentration and volume of precursor on the electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

    SciTech Connect

    Ingole, R. S.; Fugare, B. Y.; Lokhande, B. J.

    2016-04-13

    Vanadium oxide (V{sub 2}O{sub 5}) thin films have been prepared by spray pyrolysis using different concentrations and volumes of precursor solution via aqueous route at 673K deposition temperature. The influences of concentration and volume on the structural, morphological and electrochemical properties of the deposited samples are studied well. X - ray diffraction study shows orthorhombic crystal structure with V{sub 2}O{sub 5} phase, confirmed by FTIR spectroscopy. Scanning electron microscopy shows granular, homogeneous and dense surface morphology. Cyclic voltammetery of all samples carried at all scan rates. Samples prepared using 0.05M, 40 ml of precursor solution shows highest specific capacitance 428.25 F/gm at 5 mV/s, Charge discharge behavior exhibits specific energy 18.73 Wh/kg, specific power 36.00 kW/kg, columbic efficiency 87.50 %. Impedance spectroscopy study was carried in the frequency range 1mHz – 1MHz, reveals pseudocapacitive behavior of the electrode exhibiting internal resistance 1.34 ohm.

  9. Optical, Electrical, and Morphological Effects of Yttrium Doping of Cadmium Oxide Thin Films Grown by Ultrasonic Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Tombak, Ahmet; Baturay, Silan; Kilicoglu, Tahsin; Ocak, Yusuf Selim

    2017-04-01

    CdO films doped with Y concentrations of 0%, 1%, 2%, and 3% were deposited onto soda lime glass using ultrasonic spray pyrolysis. The effect of the doping level on the structural, morphological, optical, and electrical properties of the films was characterized. X-ray diffraction analysis was used to establish that all of the samples were polycrystalline and to determine the structural parameters, i.e., lattice spacing ( d), phases and associated ( hkl) planes, grain size ( D), and dislocation density ( δ). The films possessed high conductivity and carrier concentration, showing n-type semiconducting behavior. The films were almost transparent over the range from 600 nm to 1100 nm. The energy bandgap was 2.43 eV, 2.53 eV, 2.68 eV, and 2.70 eV for Y doping of 0%, 1%, 2%, and 3%, respectively. The refractive index and extinction coefficient of the films over the range from 700 nm to 1100 nm were determined by spectroscopic ellipsometry. Atomic force microscopy revealed the effect of Y doping on the surface morphology of the CdO films.

  10. Synthesis of nanocrystalline Cu{sub 2}ZnSnS{sub 4} thin films grown by the spray-pyrolysis technique

    SciTech Connect

    Chandel, Tarun Singh, Joginder; Rajaram, P.

    2015-08-28

    Spray pyrolysis was used to deposit Cu{sub 2}ZnSnS{sub 4} (CZTS) thin films on soda lime glass substrates at 300 °C. Aqueous solutions of copper chloride, zinc chloride, stannous chloride and thiourea were mixed together to form the spray liquid. The sprayed films were annealed under vacuum at 350 °C, 400 °C and 450 °C. Structural and optical characterization was performed on the CZTS films using X-ray diffraction (XRD) and UV-VIS spectrophotometry. XRD results indicate that the films are single phase nanocrystalline CZTS. Optical studies show that the optical gap values are 1.44 eV for the as-grown film and 1.46 eV, 1.48 eV and 1.49 eV for the films annealed at 350 °C, 400 °C and 450 °C, respectively.

  11. Effect of Deposition Rate and Annealing on Physical Properties of In2O3 Thin Films Prepared by Spray Pyrolysis: Ultraviolet (UV) Photoconductivity Response

    NASA Astrophysics Data System (ADS)

    Shamsoddini, Khadijeh; Eshghi, Hosein

    2017-07-01

    As-grown and annealed indium oxide thin films deposited by spray pyrolysis at various rates (2 mL/min, 3.5 mL/min, and 5 mL/min) on glass substrate have been studied. Field-emission scanning electron microscopy images and x-ray diffraction analysis of the samples revealed that the deposition spray rate and annealing process affected both the surface morphology and preferred orientation of the polycrystalline cubic phase of the layers. Electrical investigations confirmed presence of oxygen vacancy ( V O) defects related to band tail, having minimum width in the sample deposited at the highest spray rate (5 mL/min). Ultraviolet photoconductivity results indicated that, although this sample had the highest light sensitivity, its sensitivity decreased after annealing due to increased V O defects.

  12. Highly photoconducting O2-doped CdS films deposited by spray pyrolysis

    NASA Technical Reports Server (NTRS)

    Richards, D.; El-Korashy, A. M.; Stirn, R. J.; Karulkar, P. C.

    1984-01-01

    CdS films have been prepared by spraying in air solutions of thiourea with either cadmium chloride or cadmium acetate with varying mole ratio and substrate temperature, and subsequently heat treating in oxygen. Substrates included both bare glass or sapphire and transparent conducting oxide-coated sapphire for electrical measurements lateral and transverse to the CdS plane, respectively. Dark resistances of over 10 to the 14th ohms and light-to-dark conductivities of up to 10 to the 7th were obtained using uncoated substrates. The use of Cd(C2H3O2)2 in place of CdCl2 greatly increased the speed of response although with some sacrifice in photoconductivity. Deposition of CdS on ITO-coated surfaces led to greatly reduced dark resistances for the case of CdCl2, but not Cd(C2H3O2)2, presumably due to HCl reaction with the ITO coating in the course of spraying with the former. Ion microprobe analysis detected indium within the CdS films exhibiting low dark resistance. Measurements of the dark and light conductivities at temperatures down to 77 K are given as are the response times for unetched and HCl-etched surfaces.

  13. Spray pyrolysis deposition of Cu-ZnO and Zn-SnO2 solar cells

    NASA Astrophysics Data System (ADS)

    Khelfane, A.; Tarzalt, H.; Sebboua, B.; Zerrouki, H.; Kesri, N.

    2015-12-01

    Large-gap metal oxides, such as titanium, tin, and zinc oxides, have attracted great interest because of their remarkable potential in dye-sensitized solar cells (DSSC) and their low cost and simple preparation procedure. In this work, we investigated several Zn-SnO2 and Cu-ZnO thin films that were sprayed under different experimental conditions. We varied [Zn/[Sn] and [Cu/[Zn] ratios, calculated on atomic percent in the starting solution. We report some structural results of the films using X-ray diffraction. Optical reflection and transmission spectra investigated by an UV/VIS/NIR spectrophotometer permit the determination of optical constants. The direct band gap was deduced from the photon energy dependence of the absorption coefficient.

  14. Catalyzed pyrolysis of grape and olive bagasse. Influence of catalyst type and chemical treatment

    SciTech Connect

    Encinar, J.M.; Beltran, F.J.; Ramiro, A.; Gonzalez, J.F.

    1997-10-01

    Catalyzed pyrolysis of grape and olive bagasse under different experimental conditions has been studied. Variables investigated were temperature and type and concentration of catalysts. Experiments were carried out in an isothermal manner. Products of pyrolysis are gases (H{sub 2}, CO, CO{sub 2}, and CH{sub 4}), liquids (methanol, acetone, furfurylic alcohol, phenol, furfural, naphthalene, and o-cresol), and solids (chars). Temperature is a significant variable, yielding increases of fixed carbon content, gases, and to a lesser extent, ash percentage. Catalyst presence also yields increases of solid phase content, but the amount of liquid components decrease. Among catalysts applied those of Fe and Zn are the most advisable to obtain gases. Chemical treatment of bagasses with sulfuric or phosphoric acid washing leads to lower char yields, although fixed carbon content is higher and ash presence diminishes with respect to catalyst pyrolysis without chemical pretreatment. A pyrolysis kinetic study based on gas generation from thermal decomposition of residues has been carried out. From the model proposed, rate constants for the formation of each gas, reaction order of the catalyst, and activation energies were determined.

  15. Gluconic acid from biomass fast pyrolysis oils: specialty chemicals from the thermochemical conversion of biomass.

    PubMed

    Santhanaraj, Daniel; Rover, Marjorie R; Resasco, Daniel E; Brown, Robert C; Crossley, Steven

    2014-11-01

    Fast pyrolysis of biomass to produce a bio-oil followed by catalytic upgrading is a widely studied approach for the potential production of fuels from biomass. Because of the complexity of the bio-oil, most upgrading strategies focus on removing oxygen from the entire mixture to produce fuels. Here we report a novel method for the production of the specialty chemical, gluconic acid, from the pyrolysis of biomass. Through a combination of sequential condensation of pyrolysis vapors and water extraction, a solution rich in levoglucosan is obtained that accounts for over 30% of the carbon in the bio-oil produced from red oak. A simple filtration step yields a stream of high-purity levoglucosan. This stream of levoglucosan is then hydrolyzed and partially oxidized to yield gluconic acid with high purity and selectivity. This combination of cost-effective pyrolysis coupled with simple separation and upgrading could enable a variety of new product markets for chemicals from biomass. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Estimation of risks by chemicals produced during laser pyrolysis of tissues

    NASA Astrophysics Data System (ADS)

    Weber, Lothar W.; Spleiss, Martin

    1995-01-01

    Use of laser systems in minimal invasive surgery results in formation of laser aerosol with volatile organic compounds of possible health risk. By use of currently identified chemical substances an overview on possibly associated risks to human health is given. The class of the different identified alkylnitriles seem to be a laser specific toxicological problem. Other groups of chemicals belong to the Maillard reaction type, the fatty acid pyrolysis type, or even the thermally activated chemolysis. In relation to the available different threshold limit values the possible exposure ranges of identified substances are discussed. A rough estimation results in an exposure range of less than 1/100 for almost all substances with given human threshold limit values without regard of possible interactions. For most identified alkylnitriles, alkenes, and heterocycles no threshold limit values are given for lack of, until now, practical purposes. Pyrolysis of anaesthetized organs with isoflurane gave no hints for additional pyrolysis products by fragment interactions with resulting VOCs. Measurements of pyrolysis gases resulted in detection of small amounts of NO additionally with NO2 formation at plasma status.

  17. Economics evaluation for on-site pyrolysis of kraft lignin to value-added chemicals.

    PubMed

    Farag, Sherif; Chaouki, Jamal

    2015-01-01

    This work is part of a series of investigations on pyrolysis of lignin. After obtaining the necessary information regarding the quantity and quality of the obtained products, a first step economics evaluation for converting lignin into chemicals was essential. To accomplish this aim, a pyrolysis plant with a 50t/d capacity was designed, and the total capital investment and operating costs were estimated. Next, the minimal selling price of the obtained dry oil was calculated and the effect of crucial variables on the estimated price was examined. The key result indicates the estimated selling price would not compete with the price of the chemicals that are fossil fuel based, which is primarily due to the high cost of the feedstock. To overcome this challenge, different scenarios for reducing the selling price of the obtained oil, which consequently is helping by taking a place among the fossil fuel based chemicals, were discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Rates and Mechanisms of Oil Shale Pyrolysis: A Chemical Structure Approach

    SciTech Connect

    Fletcher, Thomas; Pugmire, Ronald

    2015-01-01

    Three pristine Utah Green River oil shale samples were obtained and used for analysis by the combined research groups at the University of Utah and Brigham Young University. Oil shale samples were first demineralized and the separated kerogen and extracted bitumen samples were then studied by a host of techniques including high resolution liquid-state carbon-13 NMR, solid-state magic angle sample spinning 13C NMR, GC/MS, FTIR, and pyrolysis. Bitumen was extracted from the shale using methanol/dichloromethane and analyzed using high resolution 13C NMR liquid state spectroscopy, showing carbon aromaticities of 7 to 11%. The three parent shales and the demineralized kerogens were each analyzed with solid-state 13C NMR spectroscopy. Carbon aromaticity of the kerogen was 23-24%, with 10-12 aromatic carbons per cluster. Crushed samples of Green River oil shale and its kerogen extract were pyrolyzed at heating rates from 1 to 10 K/min at pressures of 1 and 40 bar and temperatures up to 1000°C. The transient pyrolysis data were fit with a first-order model and a Distributed Activation Energy Model (DAEM). The demineralized kerogen was pyrolyzed at 10 K/min in nitrogen at atmospheric pressure at temperatures up to 525°C, and the pyrolysis products (light gas, tar, and char) were analyzed using 13C NMR, GC/MS, and FTIR. Details of the kerogen pyrolysis have been modeled by a modified version of the chemical percolation devolatilization (CPD) model that has been widely used to model coal combustion/pyrolysis. This refined CPD model has been successful in predicting the char, tar, and gas yields of the three shale samples during pyrolysis. This set of experiments and associated modeling represents the most sophisticated and complete analysis available for a given set of oil shale samples.

  19. Preparation of iron aluminate (FeAl2O4) nanoparticles from FeAl2O4 hollow particles fabricated by using a spray pyrolysis process

    NASA Astrophysics Data System (ADS)

    Yun, Jaecheol; Kim, Yangdo; Park, Dahee; Yun, Jung-Yeul

    2015-05-01

    Iron aluminate (FeAl2O4) hollow particles with a spinel structure were synthesized by using a spray pyrolysis process. FeAl2O4 hollow particles were formed at a reaction temperature of 900 °C at a flow rate of 40 L/min as a result of the rapid solvent evaporation and decomposition gases from the droplets in the spray solution prepared from metal salts and organic reagents. FeAl2O4 hollow particles were fabricated at a reaction temperature of 900 °C with a flow rate of 40 L/min. The FeAl2O4 hollow particles were heat treated for 3 hours at 600 °C in a 5% H2/Ar atmosphere to form the crystal particles. Subsequently, FeAl2O4 nanoparticles were fabricated from the FeAl2O4 hollow particles by using the wet milling process. After milling for 60 minutes, transmission electron microscopy revealed the FeAl2O4 particles to have a mean size of approximately 50 nm. The FeAl2O4 nanoparticles were fabricated successfully by using a two-step process, spray pyrolysis and wet milling.

  20. Preparation, characterisation and optimisation of lithium battery anodes consisting of silicon synthesised using Laser assisted Chemical Vapour Pyrolysis

    NASA Astrophysics Data System (ADS)

    Veliscek, Ziga; Perse, Lidija Slemenik; Dominko, Robert; Kelder, Erik; Gaberscek, Miran

    2015-01-01

    Suitability of silicon prepared using Laser assisted Chemical Vapour Pyrolysis (LaCVP) as a potential anode material in lithium batteries is systematically investigated. Its compositional, morphological, physical-chemical and electrochemical properties are compared to a current benchmark commercial silicon. Important differences in particle size and particle composition are found which, as shown, affect critically the rheological properties of the corresponding electrode slurries. In order to overcome the rheological problems of prepared nanosilicon, we introduce and optimise a spraying method instead of using the usual casting technique for slurry application. Interestingly, the optimised electrodes show similar electrochemical performance, regardless of the particle size or composition of nanosilicon. This unexpected result is explained by the unusually high resistance of electrochemical wiring in silicon-based electrodes (about 60 Ohm per 1 mg cm-2 of active material loading). Despite that, the optimised material still shows a capacity up to 1200 mA h g-1 at a relatively high loading of 1.6 mg cm-2 and after 20 cycles. On the other hand, by decreasing the loading to below ca. 0.9 mg cm-2 the wiring problems are effectively overcome and capacities close to theoretical values can be obtained.

  1. Influence of solution deposition rate on properties of V{sub 2}O{sub 5} thin films deposited by spray pyrolysis technique

    SciTech Connect

    Abd–Alghafour, N. M.; Ahmed, Naser M.; Hassan, Zai; Mohammad, Sabah M.

    2016-07-19

    Vanadium oxide (V{sub 2}O{sub 5}) thin films were deposited on glass substrates by using a cost-efficient spray pyrolysis technique. The films were grown at 350° through thermal decomposition of VCl{sub 3} in deionized water with different solution spray rates. The high resolution X-ray diffraction results revealed the formation of nanocrystalline films having orthorhombic structures with preferential orientation along (101) direction. The spray rate influenced the surface morphology and crystallite size of the films. The crystallite size was found to increase whereas the micro-strain was decreased by increasing the spray deposition rates. The increase in crystallite size and decrease in the macrostrain resulted in an improvement in the films’ crystallinity. The UV-Visible spectroscopy analysis indicated that the average transmittance of all films lies in the range 75-80 %. The band gap of V{sub 2}O{sub 5} film was decreased from 2.65 to 2.46 eV with increase of the spray deposition rate from 5 ml/min to 10 ml/min. first, second, and third level headings (first level heading).

  2. Synthesis and characterization of nanosized calcium phosphates by flame spray pyrolysis, and their effect on osteogenic differentiation of stem cells

    NASA Astrophysics Data System (ADS)

    Ataol, Sibel; Tezcaner, Ayşen; Duygulu, Ozgur; Keskin, Dilek; Machin, Nesrin E.

    2015-02-01

    The present study evaluates the synthesis of biocompatible osteoconductive and osteoinductive nano calcium phosphate (CaP) particles by industrially applied, aerosol-derived flame spray pyrolysis method for biomedical field. Calcium phosphate nanoparticles were produced in a range of calcium-to-phosphorus ratio, (1.20-2.19) in order to analyze the morphology and crystallinity changes, and to test the bioactivity of particles. The characterization results confirmed that nanometer-sized, spherical calcium phosphate particles were produced. The average primary particle size was determined as 23 nm by counting more than 500 particles in TEM pictures. XRD patterns, HRTEM, SAED, and SEM analyses revealed the amorphous nature of the as-prepared nano calcium phosphate particles at low Ca/P ratios. Increases in the specific surface area and crystallinity were observed with the increasing Ca/P ratio. TGA-DTA analysis showed that the thermally stable crystal phases formed after 700 °C. Cell culture studies were conducted with urine-derived stem cells that possess the characteristics of mesenchymal stem cells. Synthesized amorphous nanoparticles did not have cytotoxic effect at 5-50 μg/ml concentration range. Cells treated with the as-prepared nanoparticles had higher alkaline phosphatase (ALP) enzyme activity than control cells, indicating osteogenic differentiation of cells. A slight decrease in ALP activity of cells treated with two highest Ca:P ratios at 50 μg/ml concentration was observed at day 7. The findings suggest that calcium phosphate nanoparticles produced in this work have a potential to be used as biomaterials in biomedical applications.

  3. Dual acceptor doping and aging effect of p-ZnO:(Na, N) nanorod thin films by spray pyrolysis

    SciTech Connect

    Swapna, R. E-mail: santhoshmc@nitt.edu; Amiruddin, R. E-mail: santhoshmc@nitt.edu; Santhosh Kumar, M. C. E-mail: santhoshmc@nitt.edu

    2014-01-28

    An attempt has been made to realize p-type ZnO by dual acceptor doping (Na-N) into ZnO thin films. Na and N doped ZnO thin films of different concentrations (0 to 8 at.%) have been grown by spray pyrolysis at 623 K. The grown films on glass substrate have been characterized by X-ray diffraction (XRD), Hall measurement, UV-Vis spectrophotometer, Photoluminescence (PL) and Energy dispersive spectroscopy (EDS) to validate the p-type conduction. The surface morphology and roughness of the ZnO:(Na, N) films are studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM), respectively. Hall measurement shows that all the films exhibit p-type conductivity except for 0 at.% Na-N doped ZnO film. The obtained resistivity (5.60×10{sup −2} Ω cm) and hole concentration (3.15×10{sup 18} cm{sup −3}) for the best dual acceptor doped film is 6 at.%. It has been predicted that (Na{sub Zn}−N{sub O}) acceptor complex is responsible for the p-type conduction. The p-type conductivity of the ZnO:(Na, N) films is stable even after 6 months. The crystallinity of the films has been studied by XRD. Energy dispersive spectroscopy (EDS) confirms the presence of Na and N in 6 at.% ZnO:(Na, N) film. Photoluminescence (PL) spectra of ZnO:(Na, N) films show NBE and deep level emissions in the UV and visible regions, respectively. The ZnO:(Na, N) films exhibit a high transmittance about 90% in the visible region.

  4. Influences of alcoholic solvents on spray pyrolysis deposition of TiO{sub 2} blocking layer films for solid-state dye-sensitized solar cells

    SciTech Connect

    Jiang, Changyun; Koh, Wei Lin; Leung, Man Yin; Hong, Wei; Li, Yuning; Zhang, Jie

    2013-02-15

    Influences of alcoholic solvents for titanium diisopropoxide bis(acetylacetonate) (TPA) precursor solutions on the spray pyrolysis deposited TiO{sub 2} films and the photovoltaic performance of the solid-state dye-sensitized solar cells (SDSCs) using these TiO{sub 2} films as the blocking layers were investigated. Smooth TiO{sub 2} films were obtained by spray pyrolysis deposition of a TPA solution in isopropanol (IPA) at a relatively low temperature of 260 Degree-Sign C. On the other hand, when ethanol was used as solvent, the TiO{sub 2} films fabricated at the same temperature showed much rougher surfaces with many pinholes. Our results showed that ethanol reacts with TPA to form titanium diethoxide bis(acetylacetonate) (TEA), which requires a higher thermal decomposition temperature than that of TPA. SDSCs with TiO{sub 2} blocking layer films fabricated using a TPA solution in IPA showed higher power conversion efficiencies with smaller variations. - Graphical abstract: Alcoholic solvents used for the TiO{sub 2} precursor play a critical role in determining the surface morphology of blocking layers and thus the photovoltaic performance of the SDSCs. Highlights: Black-Right-Pointing-Pointer Solvent influences morphology of spray pyrolysis deposited TiO{sub 2} blocking layer. Black-Right-Pointing-Pointer Ethanol reacts with TPA, resulting poor quality of blocking layer. Black-Right-Pointing-Pointer Isopropanol is better than ethanol for obtaining smooth blocking layer. Black-Right-Pointing-Pointer SDSC with blocking layer made with isopropanol showed better performance.

  5. Smart Windows, Switchable between Transparent, Mirror, and Black States, Fabricated Using Rough and Smooth Indium Tin Oxide Films Deposited by Spray Chemical Vapor Deposition

    NASA Astrophysics Data System (ADS)

    Onodera, Ryou; Seki, Yoshiyuki; Seki, Shigeyuki; Yamada, Katsumi; Sawada, Yutaka; Uchida, Takayuki

    2013-02-01

    Two types of indium-tin oxide films, rough and smooth, with an average grain size of 434 and 71 nm, respectively, were deposited by spray pyrolysis chemical vapor deposition. Using both these films, we fabricated glare tunable transparent electrochemical devices exhibiting reversible optical changes between transparent, mirror, and black states, without any treatments. Under zero bias conditions, the transmittance of the transparent state reached 81.1% at 700 nm. With a bias of -2.5 V, the reflectance of the mirror state reached 82.0% at 700 nm. The total transmittances in the mirror and black state amounted to 0.6% in the visible range.

  6. Synthesis and characterization of Gd 0.1Ce 0.9O 1.95 thin films by spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Chourashiya, M. G.; Pawar, S. H.; Jadhav, L. D.

    2008-03-01

    The Gd doped ceria (CGO) in thin layers is of great interest for low temperature operation. In the present investigation, we report on the use of spray pyrolysis technique for the synthesis of CGO thin films. The process parameters were optimized for synthesizing Gd 0.1Ce 0.9O 1.95 films. Films were characterized by XRD, EDS, SEM, and AFM and are observed to be phase pure and dense with surface roughness of the order of ˜5 nm. The d.c. conductivity was also measured and is observed to be ˜0.5 S/cm at 623 K.

  7. Direct Preparation of Fine Powders of the 80 K Superconducting Phase in the Bi-Ca-Sr-Cu-O System by Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Tohge, Noboru; Tatsumisago, Masahiro; Minami, Tsutomu; Okuyama, Kikuo; Arai, Kouji; Kousaka, Yasuo

    1989-07-01

    Submicron powders of the 80 K superconducting phase in the Bi-Ca-Sr-Cu-O system have been directly prepared by the spray pyrolysis of aqueous solutions of corresponding metal nitrates, Bi:Ca:Sr:Cu=1:1:1:2. The powders obtained were spheres with uniformly distributed diameters below 1 μm. The crystalline phase of these powders was found to greatly depend on the oxygen partial pressure in the carrier gas as well as the decomposition temperature. The preparation conditions for the 80 K superconducting phase were examined.

  8. Tailoring of optical band gap by varying Zn content in Cd1-xZnxS thin films prepared by spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Kumar, Vipin; Sharma, D. K.; Agrawal, Sonalika; Sharma, Kapil K.; Dwivedi, D. K.; Bansal, M. K.

    2016-05-01

    Cd1-XZnXS thin films (X = 0.2, 0.4, 0.6, 0.8) have been grown on glass substrate by spray pyrolysis technique using equimolar concentration aqueous solution of cadmium chloride, zinc acetate and thiourea. Prepared thin films have been characterized by UV-VIS spectrophotometer. The optical band gap of the films has been studied by transmission spectra in wavelength range 325-600nm. It has been observed that optical band gap increases with increasing zinc concentration. The optical band gap of these thin films varies from 2.59 to 3.20eV with increasing Zn content.

  9. Determination of cadmium in water samples by fast pyrolysis-chemical vapor generation atomic fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Zhang, Jingya; Fang, Jinliang; Duan, Xuchuan

    2016-08-01

    A pyrolysis-vapor generation procedure to determine cadmium by atomic fluorescence spectrometry has been established. Under fast pyrolysis, cadmium ion can be reduced to volatile cadmium species by sodium formate. The presence of thiourea enhanced the efficiency of cadmium vapor generation and eliminated the interference of copper. The possible mechanism of vapor generation of cadmium was discussed. The optimization of the parameters for pyrolysis-chemical vapor generation, including pyrolysis temperature, amount of sodium formate, concentration of hydrochloric acid, and carrier argon flow rate were carried out. Under the optimized conditions, the absolute and concentration detection limits were 0.38 ng and 2.2 ng ml- 1, respectively, assuming that 0.17 ml of sample was injected. The generation efficiency of was 28-37%. The method was successfully applied to determine trace amounts of cadmium in two certified reference materials of Environmental Water (GSB07-1185-2000 and GSBZ 50009-88). The results were in good agreement with the certified reference values.

  10. Chemical and ecotoxicological properties of three bio-oils from pyrolysis of biomasses.

    PubMed

    Campisi, Tiziana; Samorì, Chiara; Torri, Cristian; Barbera, Giuseppe; Foschini, Anna; Kiwan, Alisar; Galletti, Paola; Tagliavini, Emilio; Pasteris, Andrea

    2016-10-01

    In view of the potential use of pyrolysis-based technologies, it is crucial to understand the environmental hazards of pyrolysis-derived products, in particular bio-oils. Here, three bio-oils were produced from fast pyrolysis of pine wood and intermediate pyrolysis of corn stalk and poultry litter. They were fully characterized by chemical analysis and tested for their biodegradability and their ecotoxicity on the crustacean Daphnia magna and the green alga Raphidocelis subcapitata. These tests were chosen as required by the European REACH regulation. These three bio-oils were biodegradable, with 40-60% of biodegradation after 28 days, and had EC50 values above 100mgL(-1) for the crustacean and above 10mgL(-1) for the alga, showing low toxicity to the aquatic life. The toxic unit approach was applied to verify whether the observed toxicity could be predicted from the data available for the substances detected in the bio-oils. The predicted values largely underestimated the experimental values.

  11. Improved electrical, optical, and structural properties of undoped ZnO thin films grown by water-mist-assisted spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Martínez Pérez, L.; Aguilar-Frutis, M.; Zelaya-Angel, O.; Muñoz Aguirre, N.

    2006-08-01

    Undoped ZnO thin films were prepared using the ultrasonic spray pyrolysis deposition technique with zinc acetylacetonate dissolved in N,N-dimethylformamide as the source materials solution. The addition of water mist in a parallel flux to the spray solution stream was also used during deposition of the films. The addition of water mist improved the electrical characteristics of the ZnO films. Fresh ZnO samples were then thermally annealed in a H2 reducing atmosphere. X-ray diffraction patterns show mainly the wurzite crystalline ZnO phase in the films. An electrical resistivity ( ) of around 2.7 × 10-2 cm was measured at room temperature for the best undoped ZnO film. is approximately one order of magnitude lower than the resistivities found in undoped ZnO films obtained by means of similar non-vacuum deposition techniques.

  12. Characterization of deposited CdS thin films by Spray Pyrolysis method and used in Cd/CdS/p-Si/Al structure

    NASA Astrophysics Data System (ADS)

    Özakın, Oǧuzhan; Aktaş, Şeydanur; Güzeldir, Betül; Saǧlam, Mustafa

    2017-04-01

    In our study, as p-type crystalline Si substrate was used. Omic contact was performed by evaporating Al metal on the matt surface of crystal. On the other surface of it CdS thin film were enlarged with the technique of Spray Pyrolysis. Structural characteristics of the grown thin film was examined SEM and EDAX image. When examining SEM image of CdS thin film were totally covered the p-Si crystal surface of it was nearly homogeneous and The EDAX spectra showed that the expected different ratios metal percent exist in the alloys, approximately. On the CdS films whose surface features were investigated, at 10-7 torr pressure was obtained Cd/CdS/p-Si/Al sandwich structure by evaporating Cd. Firstly, the I-V (current-voltage) characteristics on 80K between 320K at room temperature of this structure was measured. I-V characteristics of the examined at parameters diodes calculation, Thermionic Emission, were used. The characteristic parameters such as barrier height and ideality factor of this structure have been calculated from the forward bias I-V characteristics. Consequently, it was seen that CdS thin film grown on p-Si semiconductor will be used confidently in Cd/p-Si metal-semiconductor contacts thanks to Spray Pyrolysis method.

  13. Spray pyrolysis-deposited nanoengineered TiO2 thick films for ultra-high areal and volumetric capacity lithium ion battery applications

    NASA Astrophysics Data System (ADS)

    Haridas, Anupriya K.; Gangaja, Binitha; Srikrishnarka, Pillalamarri; Unni, Gautam E.; Nair, A. Sreekumaran; Nair, Shantikumar V.; Santhanagopalan, Dhamodaran

    2017-03-01

    Energy storage technologies are sensitively dependent on electrode film quality, thickness and process scalability. In Li-ion batteries, using additive-free titania (TiO2) as electrodes, we sought to show the potential of spray pyrolysis-deposited nanoengineered films with thicknesses up to 135 μm exhibiting ultra-high areal capacities. Detailed electron microscopic characterization indicated that the achieved thick films are composed of highly crystalline anatase TiO2 particles with sizes on the order of 10-12 nm and porous as well. A 135 μm thick film yielded ultra-high areal and volumetric capacities of 3.7 mAh cm-2 and 274 mAh cm-3, respectively, at 1C rate. Also the present work recorded high Coulombic efficiency and good cycling stability. The best previously achieved capacities for additive-free TiO2 films have been less than 0.25 mAh cm-2 and With additives, best reported areal capacity in the literature has been 2.5 mAh cm-2 at 1C rate, but only with electrode thickness as high as 1400 μm. Formation of through-the-thickness percolation of Ti3+ conductive network upon lithiation contributed substantially for the superior performance. Spray pyrolysis deposition of nanoparticulate TiO2 electrodes have the potential to yield volumetric capacities an order of magnitude higher than the other processes previously reported without sacrificing performance and process scalability.

  14. One-Pot Synthesis of CoSex -rGO Composite Powders by Spray Pyrolysis and Their Application as Anode Material for Sodium-Ion Batteries.

    PubMed

    Park, Gi Dae; Kang, Yun Chan

    2016-03-14

    A simple one-pot synthesis of metal selenide/reduced graphene oxide (rGO) composite powders for application as anode materials in sodium-ion batteries was developed. The detailed mechanism of formation of the CoSe(x)-rGO composite powders that were selected as the first target material in the spray pyrolysis process was studied. The crumple-structured CoSe(x)-rGO composite powders prepared by spray pyrolysis at 800 °C had a crystal structure consisting mainly of Co0.85 Se with a minor phase of CoSe2. The bare CoSe(x) powders prepared for comparison had a spherical shape and hollow structure. The discharge capacities of the CoSe(x)-rGO composite and bare CoSe(x) powders in the 50th cycle at a constant current density of 0.3 A g(-1) were 420 and 215 mA h g(-1), respectively, and their capacity retentions measured from the second cycle were 80 and 46%, respectively. The high structural stability of the CoSe(x)-rGO composite powders for repeated sodium-ion charge and discharge processes resulted in superior sodium-ion storage properties compared to those of the bare CoSe(x) powders.

  15. Delicate Structural Control of Si-SiOx-C Composite via High-Speed Spray Pyrolysis for Li-Ion Battery Anodes.

    PubMed

    Lee, Seung Jong; Kim, Hye Jin; Hwang, Tae Hoon; Choi, Sunghun; Park, Sung Hyeon; Deniz, Erhan; Jung, Dae Soo; Choi, Jang Wook

    2017-03-08

    Despite the high theoretical capacity, silicon (Si) anodes in lithium-ion batteries have difficulty in meeting the commercial standards in various aspects. In particular, the huge volume change of Si makes it very challenging to simultaneously achieve high initial Coulombic efficiency (ICE) and long-term cycle life. Herein, we report spray pyrolysis to prepare Si-SiOx composite using an aqueous precursor solution containing Si nanoparticles, citric acid, and sodium hydroxide (NaOH). In the precursor solution, Si nanoparticles are etched by NaOH with the production of [SiO4](4-). During the dynamic course of spray pyrolysis, [SiO4](4-) transforms to SiOx matrix and citric acid decomposes to carbon surface layer with the assistance of NaOH that serves as a decomposition catalyst. As a result, a Si-SiOx composite, in which Si nanodomains are homogeneously embedded in the SiOx matrix with carbon surface layer, is generated by a one-pot process with a residence time of only 3.5 s in a flow reactor. The optimal composite structure in terms of Si domain size and Si-to-O ratio exhibited excellent electrochemical performance, such as reversible capacity of 1561.9 mAh g(-1) at 0.06C rate and ICE of 80.2% and 87.9% capacity retention after 100 cycles at 1C rate.

  16. Variation in Miscanthus chemical composition and implications for conversion by pyrolysis and thermo-chemical bio-refining for fuels and chemicals.

    PubMed

    Hodgson, E M; Nowakowski, D J; Shield, I; Riche, A; Bridgwater, A V; Clifton-Brown, J C; Donnison, I S

    2011-02-01

    Different species and genotypes of Miscanthus were analysed to determine the influence of genotypic variation and harvest time on cell wall composition and the products which may be refined via pyrolysis. Wet chemical, thermo-gravimetric (TGA) and pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) methods were used to identify the main pyrolysis products and determine the extent to which genotypic differences in cell wall composition influence the range and yield of pyrolysis products. Significant genotypic variation in composition was identified between species and genotypes, and a clear relationship was observed between the biomass composition, yields of pyrolysis products, and the composition of the volatile fraction. Results indicated that genotypes other than the commercially cultivated Miscanthus x giganteus may have greater potential for use in bio-refining of fuels and chemicals and several genotypes were identified as excellent candidates for the generation of genetic mapping families and the breeding of new genotypes with improved conversion quality characteristics. Copyright © 2010 Elsevier Ltd. All rights reserved.

  17. The pyrolysis of 2-methylfuran: a quantum chemical, statistical rate theory and kinetic modelling study.

    PubMed

    Somers, Kieran P; Simmie, John M; Metcalfe, Wayne K; Curran, Henry J

    2014-03-21

    Due to the rapidly growing interest in the use of biomass derived furanic compounds as potential platform chemicals and fossil fuel replacements, there is a simultaneous need to understand the pyrolysis and combustion properties of such molecules. To this end, the potential energy surfaces for the pyrolysis relevant reactions of the biofuel candidate 2-methylfuran have been characterized using quantum chemical methods (CBS-QB3, CBS-APNO and G3). Canonical transition state theory is employed to determine the high-pressure limiting kinetics, k(T), of elementary reactions. Rice-Ramsperger-Kassel-Marcus theory with an energy grained master equation is used to compute pressure-dependent rate constants, k(T,p), and product branching fractions for the multiple-well, multiple-channel reaction pathways which typify the pyrolysis reactions of the title species. The unimolecular decomposition of 2-methylfuran is shown to proceed via hydrogen atom transfer reactions through singlet carbene intermediates which readily undergo ring opening to form collisionally stabilised acyclic C5H6O isomers before further decomposition to C1-C4 species. Rate constants for abstraction by the hydrogen atom and methyl radical are reported, with abstraction from the alkyl side chain calculated to dominate. The fate of the primary abstraction product, 2-furanylmethyl radical, is shown to be thermal decomposition to the n-butadienyl radical and carbon monoxide through a series of ring opening and hydrogen atom transfer reactions. The dominant bimolecular products of hydrogen atom addition reactions are found to be furan and methyl radical, 1-butene-1-yl radical and carbon monoxide and vinyl ketene and methyl radical. A kinetic mechanism is assembled with computer simulations in good agreement with shock tube speciation profiles taken from the literature. The kinetic mechanism developed herein can be used in future chemical kinetic modelling studies on the pyrolysis and oxidation of 2-methylfuran

  18. Excellent Li-ion storage performances of hierarchical SnO-SnO2 composite powders and SnO nanoplates prepared by one-pot spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Kim, Jung Hyun; Jeon, Kyung Min; Park, Jin-Sung; Kang, Yun Chan

    2017-08-01

    Hierarchical-structured SnO-SnO2 composite powders and SnO nanoplates with some SnO2 nanorods are prepared by one-pot spray pyrolysis. Dicyandiamide dissolved in the spray solution plays a key role in the preparation of the hierarchical-structured SnO-SnO2 composite powder and SnO nanoplates. The hierarchical-structured SnO-SnO2 composite powders, in which the SnO nanoplates are trapped in the porous SnO2 nanosphere, are prepared by spray pyrolysis at 800 °C. Sufficient conversion of the porous SnO2 nanospheres to SnO at 900 °C results in aggregation-free SnO2 nanoplates. SnO2 nanorods with a spherical nanodroplet at the tip are formed by Ostwald ripening. The hierarchical-structured SnO-SnO2 composite powder having high structural stability during repeated lithium alloying and dealloying reactions, shows superior discharge capacities and rate performances for lithium-ion storage compared to those of the dense-structured SnO2 powders. The discharge capacities of the hierarchical-structured SnO-SnO2 composite powders, SnO nanoplates with SnO2 nanorods, and dense-structured SnO2 powders at a current density of 1 A g-1 for the 300th cycle are 561, 504, and 416 mA h g-1, respectively. The SnO nanoplates with SnO2 nanorods and hierarchical-structured SnO-SnO2 powders deliver high reversible discharge capacities of 433 and 379 mA h g-1 at an extremely high current density of 10 A g-1, respectively.

  19. Concepts of risk assesment of complex chemical mixtures in laser pyrolysis fumes

    NASA Astrophysics Data System (ADS)

    Weber, Lothar W.; Meier, Thomas H.

    1996-01-01

    Laser-tissue interaction may generate by energy absorption a complex mixture of gaseous, volatile, semi-volatile and particular substances. At the time about 150 different components are known from IR-laser interaction with different organ tissues like liver, fat, muscle and skin. The laser-tissue interaction process thereby is dominated by heating processes, which is confirmed by the similarity of formed chemical products in comparison with conventional cooking processes for food preparation. With the identified chemical substances and relative amounts in backmind a walk along the think path of risk assessment with special reference to pyrolysis products is given. The main way of intake of pyrolysis products is the inhalative one, which results from the fine aerosols formed and the high spreading energy out of the irradiated source. The liberated amounts of irritative chemicals as (unsaturated) aldehydes, heterocycles of bad odor and possibly cancerogenic acting substances relates to some (mu) g/g of laser vaporized tissue. With regard to this exposure level in a hypothetic one cubic meter volume the occupational limit settings are far away. Even indoor air exposure levels are in nearly all cases underwent, for the content of bad smelling substances forces an effective ventilation. Up to now no laser typical chemical substance could be identified, which was not elsewhere known by frying or baking processes of meat, food or familiar. Starting with the GRAS concept of 1957 the process of risk assessment by modified food products and new ingredients is still improofing. The same process of risk assessment is governing the laser pyrolysis products of mammalian tissues. By use of sufficient suction around the laser tissue source the odor problems as well as the toxicological problems could be solved.

  20. The effect of different chemical treatments, pyrolysis conditions and feedstocks on the redox properties of biochar.

    NASA Astrophysics Data System (ADS)

    Chacón, Francisco Javier; Cayuela, María Luz; Roig, Asunción; Ángel Sánchez-Monedero, Miguel

    2017-04-01

    Pyrogenic carbonaceous materials can have a role in several biogeochemical redox reactions as electron transfer catalysts. Low N2O emissions in biochar amended soils can be related to its ability to act as an "electron shuttle", facilitating the transport of electrons to soil denitrifying microorganisms. Modifying biochar redox properties could be an interesting approach to regulate this effect. In this work we propose several methods for the development of biochars from slow pyrolysis with altered electrochemical properties. To improve its electron exchange capacity we aimed to: 1) Increase the number of redox active functional groups in biochar. Several pyrolysis conditions and chemical treatments (KOH, H3PO4 and H2O2) were tested. 2) Raise the fraction of redox active mineral in biochar. The presence of Fe and Mn-based minerals in biochar could also catalyze redox reactions in soil associated with the nitrogen cycle. Different additives (FeCl3, KMnO4 and clay) were combined with the feedstock before the pyrolysis process. Results of their ability to modify biochar redox properties, measured by mediated electrochemical analysis, are presented. Additionally, we characterized biochars produced from different feedstocks to assess how their lignin, holocellulose and ash composition affects these properties. Analytical issues arising from the difficulty of measuring the electron exchange capacity of biochar will also be discussed.

  1. Ternary Porous Sulfur/Dual-Carbon Architectures for Lithium/Sulfur Batteries Obtained Continuously and on a Large Scale via an Industry-Oriented Spray-Pyrolysis/Sublimation Method.

    PubMed

    Liang, Xin; Kaiser, Mohammad Rejaul; Konstantinov, Konstantin; Tandiono, Richard; Wang, Zhaoxiang; Chen, Chunhua; Liu, Hua-Kun; Dou, Shi-Xue; Wang, Jiazhao

    2016-09-28

    Ternary composites with porous sulfur/dual-carbon architectures have been synthesized by a single-step spray-pyrolysis/sublimation technique, which is an industry-oriented method that features continuous fabrication of products with highly developed porous structures without the need for any further treatments. A double suspension of commercial sulfur and carbon scaffolding particles was dispersed in ethanol/water solution and sprayed at 180 °C using a spray pyrolysis system. In the resultant composites, the sulfur particles were subjected to an ultrashort sublimation process, leading to the development of a highly porous surface, and were meanwhile coated with amorphous carbon, obtained through the pyrolysis of the ethanol, which acts as an adhesive interface to bind together the porous sulfur with the scaffolding carbon particles, to form a ternary composite architecture. This material has an effective conducting-carbon/sulfur-based matrix and interconnected open pores to reduce the diffusion paths of lithium ions, buffer the sulfur volumetric expansion, and absorb electrolyte and polysulfides. Because of the unique chemistry and the structure, the composites show stable cycling performance for 200 cycles and good rate capability of 520 mAh g(-1) at 2 C. This advanced spray-pyrolysis/sublimation method is easy to scale up and shows great potential for commercialization of lithium/sulfur batteries.

  2. The influence of concentration on the morphology of TiO2 thin films prepared by spray pyrolysis for electrochemical study

    NASA Astrophysics Data System (ADS)

    Fugare, B. Y.; Lokhande, B. J.

    2017-06-01

    In the nanoscale architecture, expected morphology plays an important role in the fabrication of supercapacitive devices due to their highly porous properties. Herein, a well-defined rutile TiO2 architecture was successfully prepared by spray pyrolysis technique (SPT), by changing the concentration of the spraying solution from 0.01 to 0.1 M at 723 K deposition temperature onto stainless steel substrates. The thermal decomposition behavior of the precursor is analyzed using thermogravimetric analyzer. As-deposited thin film electrodes exhibits rutile tetragonal crystalline structure confirmed using XRD. FT-IR study indicate the presence of Ti=O stretching vibration in the range 400-1000 cm-1. The obtained nanostructures merely changes by changing the concentration of spraying solution and process parameters as strongly evidenced using SEM. TEM image and SAED pattern confirms the formation of nanorods and rutile tetragonal structure of TiO2. EDAX confirms formation of pristine TiO2. Wettability of samples shows angle of contact changes by changing the sample thickness and surface roughness of the samples. Optimized electrode shows maximum specific capacitance 273.84 F/g at 2 mV/s in 1 M KOH. Maximum values of specific energy (SE), specific power (SP) and efficiency as observed using galvanostatic charge-discharge are 04.32 Wh/Kg, 70.27 KW/Kg and 90.37%, respectively.

  3. Electrical Characteristics and Preparation of (Ba0.5Sr0.5)TiO3 Films by Spray Pyrolysis and Rapid Thermal Annealing

    NASA Astrophysics Data System (ADS)

    Koo, Horng-Show; Chen, Mi; Ku, Hong-Kou; Kawai, Tomoji

    2007-04-01

    Functional films of (Ba0.5Sr0.5)TiO3 on Pt (1000 Å)/Ti (100 Å)/SiO2 (2000 Å)/Si substrates are prepared by spray pyrolysis and subsequently rapid thermal annealing. Barium nitrate, strontium nitrate and titanium isopropoxide are used as starting materials with ethylene glycol as solvent. For (Ba0.5Sr0.5)TiO3 functional thin film, thermal characteristics of the precursor powder scratched from as-sprayed films show a remarkable peak around 300-400 °C and 57.7% weight loss up to 1000 °C. The as-sprayed precursor film with coffee-like color and amorphous-like phase is transformed into the resultant film with white, crystalline perovskite phase and characteristic peaks (110) and (100). The resultant films show correspondent increases of dielectric constant, leakage current and dissipation factor with increasing annealing temperatures. The dielectric constant is 264 and tangent loss is 0.21 in the resultant films annealed at 750 °C for 5 min while leakage current density is 1.5× 10-6 A/cm2 in the film annealed at 550 °C for 5 min.

  4. Effects of Concentration and Substrate Type on Structure and Conductivity of p-Type CuS Thin Films Grown by Spray Pyrolysis Deposition

    NASA Astrophysics Data System (ADS)

    Sabah, Fayroz A.; Ahmed, Naser M.; Hassan, Z.

    2017-01-01

    Copper sulphide (CuS) thin films were grown upon Ti, indium tin oxide (ITO), and glass substrates by using spray pyrolysis deposition at 200°C. The films exhibited good adhesion compared to chemical bath deposition. CuCl2·2H2O and Na2S2O3·5H2O precursors were used as Cu2+ and S2- sources, respectively. Two concentrations (i.e., 0.2 M and 0.4 M) were selected in this study. X-ray diffraction analysis reveals that the films with 0.2 M showed only the formation of a covellite CuS phase having a hexagonal crystal structure with diffraction peaks of low intensity. For 0.4 M concentration, in addition to the covellite CuS phase, chalcocite Cu2S phase having a hexagonal crystal structure also appeared with relatively higher intensity peaks for all thin films. Field-emission scanning electron microscopy observations showed the formation of small grains for 0.2 M, whereas a mixture of grains with square-like shape and nanoplates were formed for 0.4 M. Depending on the 0.2 M and 0.4 M thin films thicknesses (3.2 μm and 4 μm, respectively), the band gap energy was obtained from optical measurements to be approximately 2.64 eV for 0.2 M (pure CuS phase), which slightly decreased up to 2.56 eV for 0.4 M concentration. Hall effect measurements showed that all grown films are p-type. The 0.2 M film exhibited much lower sheet resistance ( R sh = 33.96 Ω/Sq-55.70 Ω/Sq) compared to 0.4 M film ( R sh = 104.33 Ω/Sq-466.6 Ω/Sq). Moreover, for both concentrations, the films deposited onto ITO substrate showed the lowest sheet resistance ( R sh = 33.96 Ω/Sq-104.33 Ω/Sq).

  5. Flash Vacuum Pyrolysis - Techniques and Reactions.

    PubMed

    Wentrup, Curt

    2017-07-04

    While pyrolysis reactions have been performed since ancient times and been crucial for the invention of several technologies, the methodology now commonly known as flash vacuum pyrolysis, FVP (or flash vacuum thermolysis, FVT) had its early beginnings in the 1940s and1950s, mainly through mass spectrometric detection of pyrolytically formed free radicals. In the 1960s many organic chemists started performing FVP experiments with the purpose of isolating new and interesting compounds and understanding pyrolysis processes. Meanwhile, many different types of apparatus and techniques have been developed, and it is the purpose of this review to present the most important methods as well as a survey of typical reactions and observations that can be achieved with the various techniques. This includes preparative FVP, chemical trapping reactions, matrix isolation and low temperature spectroscopy of reactive intermediates and unstable molecules, the use of online mass, photoelectron, microwave and millimeterwave spectroscopies, gas-phase laser pyrolysis, pulsed pyrolysis with supersonic jet expansion, very low pressure pyrolysis for kinetic investigations, solution-spray and falling-solid FVP for involatile compounds, and pyrolysis over solid supports and reagents. Moreover, the combination of FVP with matrix isolation and photochemistry is a powerful tool for investigations of reaction mechanism. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Analytical pyrolysis vs. classical wet chemical analysis to assess the decay of archaeological waterlogged wood.

    PubMed

    Lucejko, Jeannette J; Zborowska, Magdalena; Modugno, Francesca; Colombini, Maria P; Prądzyński, Włodzimierz

    2012-10-01

    The macromolecular complexity of wood limits the possibility of obtaining complete chemical information on its alteration in archaeological objects. This paper compares the results obtained in the characterisation of the components of archaeological wood by a classical wet chemical method and by an instrumental method based on pyrolysis in presence of hexamethyldisilazane coupled with gas chromatography/mass spectrometry, Py(HMDS)-GC/MS. We compare the results obtained with the two methods quantitatively. This enables us to evaluate the efficiency of Py(HMDS)-GC/MS in assessing the chemical composition and the state of conservation of degraded wood. The material analysed consisted of reference sound wood and waterlogged wood from the Żółte historical site, located on a small island on Lake Zarańskie in Poland. The samples are from the remains of settlements dating to a period between the 9th and the 12th centuries AD. The results obtained by Py(HMDS)-GC/MS analysis are consistent in the determination of the level of degradation of archaeological wood with the results obtained using traditional techniques. The pyrolysis method is faster, reproducible, and reveals not only the amount but also the quality of the wood constituents, needing a much smaller sample. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Rapid analysis of the chemical composition of agricultural fibers using near infrared spectroscopy and pyrolysis molecular beam mass spectrometry

    Treesearch

    Stephen S. Kelley; Roger M. Rowell; Mark Davis; Cheryl K. Jurich; Rebecca Ibach

    2004-01-01

    The chemical composition of a variety of agricultural biomass samples was analyzed with near infrared spectroscopy and pyrolysis molecular beam mass spectroscopy. These samples were selected from a wide array of agricultural residue samples and included residues that had been subjected to a variety of di2erent treatments including solvent extractions and chemical...

  8. Processing and synthesis of multi-metallic nano oxide ceramics via liquid-feed flame spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Azurdia, Jose Antonio

    The liquid-feed flame spray pyrolysis (LF-FSP) process aerosolizes metal-carboxylate precursors dissolved in alcohol with oxygen and combusts them at >1500°C. The products are quenched rapidly (˜10s msec) to < 400°C. By selecting the appropriate precursor mixtures, the compositions of the resulting oxide nanopowders can be tailored easily, which lends itself to combinatorial studies of systems facilitating material property optimization. The resulting nanopowders typically consist of single crystal particles with average particle sizes (APS) < 35 nm, specific surface areas (SSA) of 20-60 m2/g and spherical morphology. LF-FSP provides access to novel single phase nanopowders, known phases at compositions outside their published phase diagrams, intimate mixing at nanometer length scales in multi metallic oxide nanopowders, and control of stoichiometry to ppm levels. The materials produced may exhibit unusual properties including structural, catalytic, and photonic ones and lower sintering temperatures. Prior studies used LF-FSP to produce MgAl2O4 spinel for applications in transparent armor and IR radomes. In these studies, a stable spinel structure with a (MgO)0.1(Al2O3)0.9 composition well outside the known phase field was observed. The work reported here extends this observation to two other spinel systems: Al2O3-NiO, Al2O3-CoOx; followed by three series of transition metal binary oxides, NiO-CoO, NiO-MoO3, NiO-CuO. The impetus to study spinels derives both from the fact that a number of them are known transparent ceramics, but also others offer high SSAs coupled with unusual phases that suggest potentially novel catalytic materials. Because LF-FSP provides access to any composition, comprehensive studies of the entire tie-lines were conducted rather than just compositions of value for catalytic applications. Initial efforts established baseline properties for the nano aluminate spinels, then three binary transition metal oxide sets (Ni-Co, Ni-Mo and Ni

  9. Integrated supply chain design for commodity chemicals production via woody biomass fast pyrolysis and upgrading.

    PubMed

    Zhang, Yanan; Hu, Guiping; Brown, Robert C

    2014-04-01

    This study investigates the optimal supply chain design for commodity chemicals (BTX, etc.) production via woody biomass fast pyrolysis and hydroprocessing pathway. The locations and capacities of distributed preprocessing hubs and integrated biorefinery facilities are optimized with a mixed integer linear programming model. In this integrated supply chain system, decisions on the biomass chipping methods (roadside chipping vs. facility chipping) are also explored. The economic objective of the supply chain model is to maximize the profit for a 20-year chemicals production system. In addition to the economic objective, the model also incorporates an environmental objective of minimizing life cycle greenhouse gas emissions, analyzing the trade-off between the economic and environmental considerations. The capital cost, operating cost, and revenues for the biorefinery facilities are based on techno-economic analysis, and the proposed approach is illustrated through a case study of Minnesota, with Minneapolis-St. Paul serving as the chemicals distribution hub. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Ionization potentials of transparent conductive indium tin oxide films covered with a single layer of fluorine-doped tin oxide nanoparticles grown by spray pyrolysis deposition

    SciTech Connect

    Fukano, Tatsuo; Motohiro, Tomoyoshi; Ida, Takashi; Hashizume, Hiroo

    2005-04-15

    Indium tin oxide (ITO) films deposited with single layers of monodispersive fluorine-doped tin oxide (FTO) nanoparticles of several nanometers in size were grown on glass substrates by intermittent spray pyrolysis deposition using conventional atomizers. These films have significantly higher ionization potentials than the bare ITO and FTO films grown using the same technique. The ITO films covered with FTO particles of 7 nm in average size show an ionization potential of 5.01 eV, as compared with {approx}4.76 and {approx}4.64 eV in ITO and FTO films, respectively, which decreases as the FTO particle size increases. The ionization potentials are practically invariant against oxidation and reduction treatments, promising a wide application of the films to transparent conducting oxide electrodes in organic electroluminescent devices and light-emitting devices of high efficiencies.

  11. Tailoring of optical band gap by varying Zn content in Cd{sub 1-x}Zn{sub x}S thin films prepared by spray pyrolysis method

    SciTech Connect

    Kumar, Vipin Sharma, D. K.; Agrawal, Sonalika; Sharma, Kapil K.; Dwivedi, D. K.; Bansal, M. K.

    2016-05-06

    Cd{sub 1-X}Zn{sub X}S thin films (X = 0.2, 0.4, 0.6, 0.8) have been grown on glass substrate by spray pyrolysis technique using equimolar concentration aqueous solution of cadmium chloride, zinc acetate and thiourea. Prepared thin films have been characterized by UV-VIS spectrophotometer. The optical band gap of the films has been studied by transmission spectra in wavelength range 325-600nm. It has been observed that optical band gap increases with increasing zinc concentration. The optical band gap of these thin films varies from 2.59 to 3.20eV with increasing Zn content.

  12. Structural and optical properties of nanocrystalline pure and indium doped tin oxide powders synthesized in a single step by flame spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Silvister Raju, M. J.; Bhattacharya, S. S.

    2017-07-01

    Phase pure tin oxide (SnO2) and indium doped SnO2 nanocrystalline powders were synthesized in a single step by a flame spray pyrolysis method. The as-synthesized powders were characterized by standard techniques of x-ray diffraction, scanning and transmission electron microscopy, x-ray photoelectron spectroscopy and absorption spectroscopy. Using x-ray diffraction, it was established that the powders had the rutile (cassiterite) structure with tetragonal unit cells in the space group P42/mnm. Using the Rietveld refinement method, structural analysis was carried out in order to obtain the lattice parameters, volume and density. X-ray photoelectron spectra confirmed the presence of indium in the doped samples. Absorption spectra revealed that the powders were transparent to the visible spectrum with a sharp absorption below 350 nm. Energy bandgaps, estimated by Tauc plots, established that increasing the doping concentration reduced the bandgap.

  13. The Effect of Film Composition on the Texture and Grain Size of CuInS2 Prepared by Spray Pyrolysis

    NASA Technical Reports Server (NTRS)

    Jin, Michael H.-C.; Banger, Kulbinder K.; Harris, Jerry D.; Hepp, Aloysius F.

    2003-01-01

    CuInS2 was deposited by spray pyrolysis using single-source precursors synthesized in-house. Films with either (112) or (204/220) preferred orientation always showed Cu-rich and In-rich composition respectively. The In-rich (204/220)-oriented films always contained a secondary phase evaluated as an In-rich compound, and the hindrance of (112)-oriented grain growth was confirmed by glancing angle X-ray diffraction. In conclusion, only the Cu-rich (112)-oriented films with dense columnar grains can be prepared without the secondary In-rich compound. The effect of extra Cu on the grain size and the solar cell results will be also presented.

  14. Ti K-edge X-ray absorption spectra of spray pyrolysis synthesized TiO2-x and TiO2-x Nx thin films

    NASA Astrophysics Data System (ADS)

    Sahoo, Madhusmita; Yadav, Ashok Kumar; Jha, S. N.; Bhattacharyya, Dibyendu; Mathews, Tom; Dash, S.

    2017-05-01

    Oxygen deficient TiO2 and N-TiO2 anatase thin films were synthesized by employing a two step process. First TiO2 and N-TiO2 films were synthesized by using a cost effective spray pyrolysis method. Subsequently, these films were reduced under H2 to create oxygen vacancies. Formation of oxygen vacancies was confirmed by using synchrotron source X-ray Absorption Spectroscopy (XAS). Effect of oxygen vacancies on electronic and structural properties were deduced from the near edge and extended region analysis of the X-ray absorption spectra. It is inferred that reduction time plays a crucial role in creating oxygen vacancies and number of oxygen vacancies increases with increase in reduction time. Substrate effect was delineated by using Si and FTO (Fluorine doped tin oxide coated glass) as substrates for film deposition.

  15. High electron mobility thin-film transistors based on Ga{sub 2}O{sub 3} grown by atmospheric ultrasonic spray pyrolysis at low temperatures

    SciTech Connect

    Thomas, Stuart R. E-mail: thomas.anthopoulos@imperial.ac.uk; Lin, Yen-Hung; Faber, Hendrik; Anthopoulos, Thomas D. E-mail: thomas.anthopoulos@imperial.ac.uk; Adamopoulos, George; Sygellou, Labrini; Stratakis, Emmanuel; Pliatsikas, Nikos; Patsalas, Panos A.

    2014-09-01

    We report on thin-film transistors based on Ga{sub 2}O{sub 3} films grown by ultrasonic spray pyrolysis in ambient atmosphere at 400–450 °C. The elemental, electronic, optical, morphological, structural, and electrical properties of the films and devices were investigated using a range of complementary characterisation techniques, whilst the effects of post deposition annealing at higher temperature (700 °C) were also investigated. Both as-grown and post-deposition annealed Ga{sub 2}O{sub 3} films are found to be slightly oxygen deficient, exceptionally smooth and exhibit a wide energy bandgap of ∼4.9 eV. Transistors based on as-deposited Ga{sub 2}O{sub 3} films show n-type conductivity with the maximum electron mobility of ∼2 cm{sup 2}/V s.

  16. Comparison of carrier transport mechanism under UV/Vis illumination in an AZO photodetector and an AZO/p-Si heterojunction photodiode produced by spray pyrolysis

    SciTech Connect

    Shasti, M.; Mortezaali, A. Dariani, R. S.

    2015-01-14

    In this study, Aluminum doped Zinc Oxide (AZO) layer is deposited on p-type silicon (p-Si) by spray pyrolysis method to fabricate ultraviolet-visible (UV/Vis) photodetector as Al doping process can have positive effect on the photodetector performance. Morphology, crystalline structure, and Al concentration of AZO layer are investigated by SEM, XRD, and EDX. The goal of this study is to analyze the mechanism of carrier transport by means of current-voltage characteristics under UV/Vis illumination in two cases: (a) electrodes connected to the surface of AZO layer and (b) electrodes connected to cross section of heterojunction (AZO/p-Si). Measurements indicate that the AZO/p-Si photodiode exhibits a higher photocurrent and lower photoresponse time under visible illumination with respect to AZO photodetector; while under UV illumination, the above result is inversed. Besides, the internal junction field of AZO/p-Si heterojunction plays an important role on this mechanism.

  17. The comparison of chemical liquid deposition and acid dealumination modified ZSM-5 for catalytic pyrolysis of pinewood using pyrolysis-gas chromatography/mass spectrometry.

    PubMed

    Zhang, Huiyan; Shao, Shanshan; Luo, Mengmeng; Xiao, Rui

    2017-11-01

    Catalyst deactivation is the main reason for low petrochemical yield in catalytic fast pyrolysis (CFP) of biomass. ZSM-5 catalysts modified by chemical liquid deposition (CLD) and acid dealumination (AD) were prepared to improve petrochemical yields for CFP of pinewood. The results showed that CLD by SiO2 led to the coverage of strong acid sites, while AD favored the removal of superficial acid sites. CFP of pinewood showed that the relative area ratio of BTX was boosted by 37.2% and 30.4% over modified ZSM-5 catalysts by CLD and AD, respectively. The yield of indenes and naphthalenes which were important precursors of heavy coke decreased sharply. Considering environmental cost and catalytic performance, CLD seems to be a preferable modification method over ZSM-5 in the catalytic pyrolysis of biomass for petrochemicals. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. Superheated steam pyrolysis of biomass elemental components and Sugi (Japanese cedar) for fuels and chemicals.

    PubMed

    Sagehashi, Masaki; Miyasaka, Noritaka; Shishido, Hiromu; Sakoda, Akiyoshi

    2006-07-01

    To develop a novel noncatalytic biomass refinery process that can be used as a portable process, superheated steam pyrolysis was investigated to produce both carbonized solid fuels and chemicals using a large-scale reactor. Individual biomass components and native biomass (Sugi, Japanese cedar) were pyrolyzed. Between 150 and 400 degrees C, the vaporizing fractions of cellulose, xylan, and kraft lignin were summarized using a numerical model. Cellulose was converted to glycolaldehyde, furfural, 5-hydroxymethyl furfural and levoglucosan, whereas xylan was converted to glycolaldehyde, furfural, and acetic acid. Kraft lignin produced a slight yield of phenol and guaiacol. The total vaporization fraction of Sugi and its vaporizing rate were explained sufficiently using a numerical model based on the weighted average of the vaporizing properties of the individual components. However, the yields of phenol, guaiacol, and acetic acid were underestimated, while the yields of furfurals and levoglucosan were overestimated. Possible synergetic effects among chemicals in the superheated steam pyrolysis of native biomass were also discussed.

  19. Effect of the substrate temperature on the physical properties of molybdenum tri-oxide thin films obtained through the spray pyrolysis technique

    SciTech Connect

    Martinez, H.M.; Torres, J.; Lopez Carreno, L.D.; Rodriguez-Garcia, M.E.

    2013-01-15

    Polycrystalline molybdenum tri-oxide thin films were prepared using the spray pyrolysis technique; a 0.1 M solution of ammonium molybdate tetra-hydrated was used as a precursor. The samples were prepared on Corning glass substrates maintained at temperatures ranging between 423 and 673 K. The samples were characterized through micro Raman, X-ray diffraction, optical transmittance and DC electrical conductivity. The species MoO{sub 3} (H{sub 2}O){sub 2} was found in the sample prepared at a substrate temperature of 423 K. As the substrate temperature rises, the water disappears and the samples crystallize into {alpha}-MoO{sub 3}. The optical gap diminishes as the substrate temperature rises. Two electrical transport mechanisms were found: hopping under 200 K and intrinsic conduction over 200 K. The MoO{sub 3} films' sensitivity was analyzed for CO and H{sub 2}O in the temperature range 160 to 360 K; the results indicate that CO and H{sub 2}O have a reduction character. In all cases, it was found that the sensitivity to CO is lower than that to H{sub 2}O. - Highlights: Black-Right-Pointing-Pointer A low cost technique is used which produces good material. Black-Right-Pointing-Pointer Thin films are prepared using ammonium molybdate tetra hydrated. Black-Right-Pointing-Pointer The control of the physical properties of the samples could be done. Black-Right-Pointing-Pointer A calculation method is proposed to determine the material optical properties. Black-Right-Pointing-Pointer The MoO{sub 3} thin films prepared by spray pyrolysis could be used as gas sensor.

  20. Facile spray-drying/pyrolysis synthesis of core-shell structure graphite/silicon-porous carbon composite as a superior anode for Li-ion batteries

    NASA Astrophysics Data System (ADS)

    Li, Min; Hou, Xianhua; Sha, Yujing; Wang, Jie; Hu, Shejun; Liu, Xiang; Shao, Zongping

    2014-02-01

    A silicon/graphite/amorphous carbon (Si/C) composite with a low silicon content in a core-shell structure has been easily synthesized using a simple method based on spray drying in combination with a subsequent pyrolysis process; natural graphite serves as the core, and silicon nanoparticles, which filled in the porous carbon matrix formed from the pyrolysis of citric acid and pitch precursors, serve as the shell. The combination of the core-shell structure for the composite and porous carbon-coating layer accommodates the large volume change of the silicon during the lithium intercalation/extraction process, thus stabilizing the electrode structure during discharge/charge cycles. As an anode material, the as-obtained Si/C composite demonstrates high capacity and excellent cycle stability. An initial specific discharge capacity of approximately 723.8 mAh g-1 and a reversible specific capacity of approximately 600 mAh g-1 after 100 cycles at a constant density of 100 mA g-1 are reached, about two times the values for graphite. Due to the simple synthesis process and the excellent performance of the resulted electrode, great commercial potential is envisioned.

  1. Pyrolysis of triglyceride materials for the production of renewable fuels and chemicals.

    PubMed

    Maher, K D; Bressler, D C

    2007-09-01

    Conversion of vegetable oils and animal fats composed predominantly of triglycerides using pyrolysis type reactions represents a promising option for the production of renewable fuels and chemicals. The purpose of this article was to collect and review literature on the thermo-chemical conversion of triglyceride based materials. The literature was divided and discussed as (1) direct thermal cracking and (2) combination of thermal and catalytic cracking. Typically, four main catalyst types are used including transition metal catalysts, molecular sieve type catalysts, activated alumina, and sodium carbonate. Reaction products are heavily dependant on the catalyst type and reaction conditions and can range from diesel like fractions to gasoline like fractions. Research in this area is not as advanced as bio-oil and bio-diesel research and there is opportunity for further study in the areas of reaction optimization, detailed characterization of products and properties, and scale-up.

  2. Effects of chemical form of sodium on the product characteristics of alkali lignin pyrolysis.

    PubMed

    Guo, Da-liang; Yuan, Hong-you; Yin, Xiu-li; Wu, Chuang-zhi; Wu, Shu-bin; Zhou, Zhao-qiu

    2014-01-01

    The effects of Na as organic bound form or as inorganic salts form on the pyrolysis products characteristics of alkali lignin were investigated by using thermogravimetric analyzer coupled with Fourier transform infrared spectrometry (TG-FTIR), tube furnace and thermo-gravimetric analyzer (TGA). Results of TG-FTIR and tube furnace indicated that the two chemical forms Na reduced the releasing peak temperature of CO and phenols leading to the peak temperature of the maximum mass loss rate shifted to low temperature zone. Furthermore, organic bound Na obviously improved the elimination of alkyl substituent leading to the yields of phenol and guaiacol increased, while inorganic Na increased the elimination of phenolic hydroxyl groups promoting the formation of ethers. It was also found the two chemical forms Na had different effects on the gasification reactivity of chars. For inorganic Na, the char conversion decreased with increasing the char forming temperature, while organic bound Na was opposite.

  3. Chemical Synthesis Accelerated by Paper Spray: The Haloform Reaction

    ERIC Educational Resources Information Center

    Bain, Ryan M.; Pulliam, Christopher J.; Raab, Shannon A.; Cooks, R. Graham

    2016-01-01

    In this laboratory, students perform a synthetic reaction in two ways: (i) by traditional bulk-phase reaction and (ii) in the course of reactive paper spray ionization. Mass spectrometry (MS) is used both as an analytical method and a means of accelerating organic syntheses. The main focus of this laboratory exercise is that the same ionization…

  4. Chemical Synthesis Accelerated by Paper Spray: The Haloform Reaction

    ERIC Educational Resources Information Center

    Bain, Ryan M.; Pulliam, Christopher J.; Raab, Shannon A.; Cooks, R. Graham

    2016-01-01

    In this laboratory, students perform a synthetic reaction in two ways: (i) by traditional bulk-phase reaction and (ii) in the course of reactive paper spray ionization. Mass spectrometry (MS) is used both as an analytical method and a means of accelerating organic syntheses. The main focus of this laboratory exercise is that the same ionization…

  5. Raman spectroscopy of Cu-Sn-S ternary compound thin films prepared by the low-cost spray-pyrolysis technique.

    PubMed

    Brus, Viktor V; Babichuk, Ivan S; Orletskyi, Ivan G; Maryanchuk, Pavlo D; Yukhymchuk, Volodymyr O; Dzhagan, Volodymyr M; Yanchuk, Igor B; Solovan, Mykhailo M; Babichuk, Iryna V

    2016-04-20

    Cu-Sn-S (CTS) thin films were deposited onto bare and molybdenum (Mo) coated glass substrates by means of the spray pyrolysis technique under different conditions. The CTS thin films obtained are shown, by means of Raman spectroscopy, to consist of two main phases: Cu2SnS3 and Cu3SnS4 as well as of the secondary phase of Cu2-xS. The electrical conductivity of the spray-deposited p-type CTS thin films under investigation is determined by two shallow acceptor levels: Ev+0.07  eV at T<334  K and Ev+0.1  eV at T>334  K. The material of the CTS thin films was established to be a direct-band semiconductor with the bandgap Eg=1.89  eV. The SEM and x-ray energy dispersive analysis show the surface and cross section of the CTS thin film deposited onto molybdenum-coated glass ceramics substrate with the actual atomic ratios of Cu:Sn:S being 2.9:1:2.64, which is in good agreement with the Raman spectra. Also, a small content of residual Cl atoms was found in the CTS thin films under investigation as the by-product of the pyrolytic reactions.

  6. Aromatic chemicals by iron-catalyzed hydrotreatment of lignin pyrolysis vapor.

    PubMed

    Olcese, Roberto Nicolas; Lardier, George; Bettahar, Mohammed; Ghanbaja, Jaafar; Fontana, Sébastien; Carré, Vincent; Aubriet, Frédéric; Petitjean, Dominique; Dufour, Anthony

    2013-08-01

    Lignin is a potential renewable material for the production of bio-sourced aromatic chemicals. We present the first hydrotreatment of lignin pyrolysis vapors, before any condensation, using inexpensive and sustainable iron-silica (Fe/SiO2 ) and iron-activated carbon (Fe/AC) catalysts. Lignin pyrolysis was conducted in a tubular reactor and vapors were injected in a fixed bed of catalysts (673 K, 1 bar) with stacks to investigate the profile of coke deposit. More than 170 GC-analyzable compounds were identified by GCxGC (heart cutting)/flame ionization detector mass spectrometry. Lignin oligomers were analyzed by very high resolution mass spectrometry, called the "petroleomic" method. They are trapped by the catalytic fixed bed and, in particular, by the AC. The catalysts showed a good selectivity for the hydrodeoxygenation of real lignin vapors to benzene, toluene, xylenes, phenol, cresols, and alkyl phenols. The spent catalysts were characterized by temperature-programmed oxidation, transmission electron microscopy (TEM), and N2 sorption. Micropores in the Fe/AC catalyst are completely plugged by coke deposits, whereas the mesoporous structure of Fe/SiO2 is unaffected. TEM images reveal two different types of coke deposit: 1) catalytic coke deposited in the vicinity of iron particles and 2) thermal coke (carbonaceous particles ≈1 μm in diameter) formed from the gas-phase growth of lignin oligomers.

  7. Physico-chemical properties of chars obtained in the co-pyrolysis of waste mixtures.

    PubMed

    Bernardo, M; Lapa, N; Gonçalves, M; Mendes, B; Pinto, F; Fonseca, I; Lopes, H

    2012-06-15

    The present work aims to perform a multistep upgrading of chars obtained in the co-pyrolysis of PE, PP and PS plastic wastes, pine biomass and used tires. The quality of the upgraded chars was evaluated by measuring some of their physico-chemical properties in order to assess their valorisation as adsorbents' precursors. The crude chars were submitted to a sequential solvent extraction with organic solvents of increasing polarity (hexane, mixture 1:1 v/v hexane:acetone and acetone) followed by an acidic demineralization procedure with 1M HCl solution. The results obtained showed that the upgrading treatment allow the recovery of 63-81% of the pyrolysis oils trapped in the crude chars and a reduction in the char's ash content in the range of 64-86%. The textural and adsorption properties of the upgraded chars were evaluated and the results indicate that the chars are mainly mesoporous and macroporous materials, with adsorption capacities in the range of 3.59-22.2 mg/g for the methylene blue dye. The upgrading treatment allowed to obtain carbonaceous materials with quality to be reused as adsorbents or as precursors for activated carbon.

  8. Catalytic pyrolysis-gc/ms of spirulina: evaluation of a highly proteinaceous biomass source for production of fuels and chemicals

    USDA-ARS?s Scientific Manuscript database

    Pyrolysis of microalgae offers a pathway towards the production of compounds derived from the thermal decomposition of triglycerides, proteins as well as lignocelluloses and their combinations thereof. When catalytically induced, this could lead to the production of fuels and chemicals including aro...

  9. Pretreatment of empty palm fruit bunch for production of chemicals via catalytic pyrolysis.

    PubMed

    Misson, Mailin; Haron, Roslindawati; Kamaroddin, Mohd Fadhzir Ahmad; Amin, Nor Aishah Saidina

    2009-06-01

    The effect of chemical pretreatments using NaOH, H(2)O(2), and Ca(OH)(2) on Empty Palm Fruit Bunches (EPFB) to degrade EPFB lignin before pyrolysis was investigated. Spectrophotometer analysis proved consecutive addition of NaOH and H(2)O(2) decomposed almost 100% of EPFB lignin compared to 44% for the Ca(OH)(2), H(2)O(2) system while NaOH and Ca(OH)(2) used exclusively could not alter lignin much. Next, the pretreated EPFB was catalytically pyrolyzed. Experimental results indicated the phenolic yields over Al-MCM-41 and HZSM-5 catalysts were 90 wt% and 80 wt%, respectively compared to 67 wt% yield for the untreated sample under the same set of conditions. Meanwhile, the experiments with HY zeolite yielded 70 wt% phenols.

  10. A review of catalytic microwave pyrolysis of lignocellulosic biomass for value-added fuel and chemicals.

    PubMed

    Morgan, Hervan Marion; Bu, Quan; Liang, Jianghui; Liu, Yujing; Mao, Hanping; Shi, Aiping; Lei, Hanwu; Ruan, Roger

    2017-04-01

    Lignocellulosic biomass is an abundant renewable resource and can be efficiently converted into bio-energy by a bio-refinery. From the various techniques available for biomass thermo-chemical conversion; microwave assisted pyrolysis (MAP) seems to be the very promising. The principles of microwave technology were reviewed and the parameters for the efficient production of bio-oil using microwave technology were summarized. Microwave technology by itself cannot efficiently produce high quality bio-oil products, catalysts are used to improve the reaction conditions and selectivity for valued products during MAP. The catalysts used to optimize MAP are revised in the development of this article. The origins for bio-oils that are phenol rich or hydrocarbon rich are reviewed and their experimental results were summarized. The kinetics of MAP is discussed briefly in the development of the article. Future prospects and scientific development of MAP are also considered in the development of this article.

  11. Pyrolysis behaviors and kinetics of refining and chemicals wastewater, lignite and their blends through TGA.

    PubMed

    Mu, Lin; Chen, Jianbiao; Yin, Hongchao; Song, Xigeng; Li, Aimin; Chi, Xiao

    2015-03-01

    Co-pyrolysis behaviors of refining and chemicals wastewater solid (RS) and Huolinhe lignite (HL) were investigated via thermogravimetric analysis (TGA). The thermal degradation process of RS and the blends proceeded in three stages, while two stages for HL. The increased percentage of RS in the blends reduced the characteristic temperature (Ti, Tp, Tf) and residual mass (Mr), while raised the characteristic reaction rate (Rp, Rv) and comprehensive devolatilization parameter (D). The results indicated that there existed some inhibitive interactions between RS and HL. The activation energies were calculated by using the Friedman and Starink method. The activation energy of RS increased first and then decreased with conversion degree, and the variation wasn't as great as that of the blends and lignite. No matter which conversion degree is, the activation energy decreased with the percentage of RS in the blends increasing. The minimum value was obtained by blending 75wt.% RS. Copyright © 2014 Elsevier Ltd. All rights reserved.

  12. Ab initio quantum chemical and kinetic modeling study of the pyrolysis kinetics of pyrrole

    SciTech Connect

    Martoprawiro, M.; Bacskay, G.B.; Mackie, J.C.

    1999-05-20

    The five-membered heterocyclic pyrrole moiety is an important structure in coals and derived tars, and the thermal decomposition reactions of pyrrole are important for production of precursors of the oxides of nitrogen, NO{sub x}, in the combustion of coals. The kinetics of pyrolysis of pyrrole have been investigated theoretically by ab initio quantum chemical techniques and by detailed chemical kinetic modeling of previously reported experimental results. The overall kinetics can be successfully modeled by a 117 step kinetic model that gives good agreement with temperature profiles of major products and also provides an acceptable fit for minor products. The thermochemistry and rate parameters of a number of key reactions have been obtained by ab initio calculations carried out at CASSCF, CASPT2, and G2(MP2) levels of theory. Several reaction pathways were investigated. The major product, HCN, arises principally from a hydrogen migration in pyrrole to form a cyclic carbene with the NH bond intact. Ring scission of this carbene leads to an allenic imine precursor of HCN and propyne. This is the decomposition pathway of lowest energy. Pyrolysis is preceded by the facile tautomerization of pyrrole to 2H-pyrrolenine. The latter can undergo CN fission to form an open chain biradical species, which is the precursor of the butenenitrile isomeric products, cis- and trans-crotononitrile and allyl cyanide. The biradical can also undergo facile H-fission to form cyanoallyl radical, which is an important precursor of acetylene, acetonitrile, and acrylonitrile, H{sub 2} also arises principally from H-fission of the biradical.

  13. CuS p-type thin film characterization deposited on Ti, ITO and glass substrates using spray pyrolysis deposition (SPD) for light emitting diode (LED) application

    SciTech Connect

    Sabah, Fayroz A.; Ahmed, Naser M. Hassan, Z. Azzez, Shrook A.; Rasheed, Hiba S.; Al-Hazim, Nabeel Z.

    2016-07-06

    The copper sulphide (CuS) thin films were grown with good adhesion by spray pyrolysis deposition (SPD) on Ti, ITO and glass substrates at 200 °C. The distance between nozzle and substrate is 30 cm. The composition was prepared by mixing copper chloride CuCl{sub 2}.2H{sub 2}O as a source of Cu{sup 2+} and sodium thiosulfate Na{sub 2}S{sub 2}O{sub 3}.5H{sub 2}O as a source of and S{sup 2−}. Two concentrations (0.2 and 0.4 M) were used for each CuCl{sub 2} and Na{sub 2}S{sub 2}O{sub 3} to be prepared and then sprayed (20 ml). The process was started by spraying the solution for 3 seconds and after 10 seconds the cycle was repeated until the solution was sprayed completely on the hot substrates. The structural characteristics were studied using X-ray diffraction; they showed covellite CuS hexagonal crystal structure for 0.2 M concentration, and covellite CuS hexagonal crystal structure with two small peaks of chalcocite Cu{sub 2}S hexagonal crystal structure for 0.4 M concentration. Also the surface and electrical characteristics were investigated using Field Emission Scanning Electron Microscopy (FESEM) and current source device, respectively. The surface study for the CuS thin films showed nanorods to be established for 0.2 M concentration and mix of nanorods and nanoplates for 0.4 M concentration. The electrical study showed ohmic behavior and low resistivity for these films. Hall Effect was measured for these thin films, it showed that all samples of CuS are p- type thin films and ensured that the resistivity for thin films of 0.2 M concentration was lower than that of 0.4 M concentration; and for the two concentrations CuS thin film deposited on ITO had the lowest resistivity. This leads to the result that the conductivity was high for CuS thin film deposited on ITO substrate, and the conductivity of the three thin films of 0.2 M concentration was higher than that of 0.4 M concentration.

  14. CuS p- type thin film characterization deposited on Ti, ITO and glass substrates using spray pyrolysis deposition (SPD) for light emitting diode (LED) application

    NASA Astrophysics Data System (ADS)

    Sabah, Fayroz A.; Ahmed, Naser M.; Hassan, Z.; Rasheed, Hiba S.; Azzez, Shrook A.; Al-Hazim, Nabeel Z.

    2016-07-01

    The copper sulphide (CuS) thin films were grown with good adhesion by spray pyrolysis deposition (SPD) on Ti, ITO and glass substrates at 200 °C. The distance between nozzle and substrate is 30 cm. The composition was prepared by mixing copper chloride CuCl2.2H2O as a source of Cu2+ and sodium thiosulfate Na2S2O3.5H2O as a source of and S2-. Two concentrations (0.2 and 0.4 M) were used for each CuCl2 and Na2S2O3 to be prepared and then sprayed (20 ml). The process was started by spraying the solution for 3 seconds and after 10 seconds the cycle was repeated until the solution was sprayed completely on the hot substrates. The structural characteristics were studied using X-ray diffraction; they showed covellite CuS hexagonal crystal structure for 0.2 M concentration, and covellite CuS hexagonal crystal structure with two small peaks of chalcocite Cu2S hexagonal crystal structure for 0.4 M concentration. Also the surface and electrical characteristics were investigated using Field Emission Scanning Electron Microscopy (FESEM) and current source device, respectively. The surface study for the CuS thin films showed nanorods to be established for 0.2 M concentration and mix of nanorods and nanoplates for 0.4 M concentration. The electrical study showed ohmic behavior and low resistivity for these films. Hall Effect was measured for these thin films, it showed that all samples of CuS are p- type thin films and ensured that the resistivity for thin films of 0.2 M concentration was lower than that of 0.4 M concentration; and for the two concentrations CuS thin film deposited on ITO had the lowest resistivity. This leads to the result that the conductivity was high for CuS thin film deposited on ITO substrate, and the conductivity of the three thin films of 0.2 M concentration was higher than that of 0.4 M concentration.

  15. Spraying chicken skin with selected chemicals to reduce attached Salmonella typhimurium.

    PubMed

    Xiong, H; Li, Y; Slavik, M F; Walker, J T

    1998-03-01

    Aqueous solutions of 5% and 10% trisodium phosphate (TSP), 0.1% and 0.5% cetylpyridinium chloride (CPC), 1% and 2% lactic acid (LA), and 0.1% and 0.5% grapefruit seed extract (DF-100) were evaluated in prechill spraying for reducing Salmonella typhimurium attached on chicken skins. Chicken skins were inoculated with S. typhimurium and then sprayed with the selected chemical solutions for 30 sec at 206 kPa and 20 degrees C. After chemical spraying, the skins were rinsed by spraying tap water for 30 sec. Each skin was stomached in buffered peptone water (BPW) for 1 min. The stomaching water was then diluted serially, inoculated onto both xylose lysine tergitol (XLT4) agar and Aerobic Plate Count (APC) Petrifilm, and incubated for 24 hr at 37 degrees C. The results showed that the numbers of Salmonella on the chicken skins after the chemical spraying were significantly lower than those without spray (P < 0.05). The CPC reduced Salmonella by 1.5 to 1.9 log10. TSP resulted in a 2.1 to 2.2 log10 reduction of Salmonella and DF-100 produced a 1.6 to 1.8 log10 reduction of Salmonella. The LA had a number of Salmonella with a 2.2 log10 reduction. The 0.5% CPC resulted a significantly greater reduction in Salmonella than 0.1% CPC. There were no significant differences in Salmonella reduction between different concentrations of the other three chemicals.

  16. Chemical and mineralogical evaluation of slag products derived from the pyrolysis/melting treatment of MSW

    SciTech Connect

    Saffarzadeh, Amirhomayoun . E-mail: a_saffarzadeh@yahoo.com; Shimaoka, Takayuki; Motomura, Yoshinobu; Watanabe, Koichiro

    2006-07-01

    This paper provides the results of studies on the characteristics of novel material derived from pyrolysis/melting treatment of municipal solid waste in Japan. Slag products from pyrolysis/melting plants were sampled for the purpose of detailed phase analysis and characterization of heavy metal-containing phases using optical microscopy, electron probe microanalysis (EPMA), XRF and XRD. The study revealed that the slag material contains glass (over 95%), oxide and silicate minerals (spinel, melilite, pseudowollastonite), as well as individual metallic inclusions as the major constituents. A distinct chemical diversity was discovered in the interstitial glass in terms of silica content defined as low and high silica glass end members. Elevated concentrations of Zn, Cr, Cu, Pb and Ba were recorded in the bulk composition. Cu, Pb and Ba behave as incompatible elements since they have been markedly characterized as part of polymetallic alloys and insignificantly sulfides in the form of spherical metallic inclusions associated with tracer amounts of other elements such as Sb, Sn, Ni, Zn, Al, P and Si. In contrast, an appreciable amount of Zn is retained by zinc-rich end members of spinel and partially by melilite and silica glass. Chromium exhibits similar behavior, and is considerably held by Cr-rich spinel. The intense incorporation of Zn and Cr into spinel indicates the very effective enrichment of these two elements into phases more environmentally resistant than glass. There was no evidence, however, that Cu and Pb enter into the structure of the crystalline silicates or oxides that may lead to their easier leachability upon exposure to the environment.

  17. Chemical and mineralogical evaluation of slag products derived from the pyrolysis/melting treatment of MSW.

    PubMed

    Saffarzadeh, Amirhomayoun; Shimaoka, Takayuki; Motomura, Yoshinobu; Watanabe, Koichiro

    2006-01-01

    This paper provides the results of studies on the characteristics of novel material derived from pyrolysis/melting treatment of municipal solid waste in Japan. Slag products from pyrolysis/melting plants were sampled for the purpose of detailed phase analysis and characterization of heavy metal-containing phases using optical microscopy, electron probe microanalysis (EPMA), XRF and XRD. The study revealed that the slag material contains glass (over 95%), oxide and silicate minerals (spinel, melilite, pseudowollastonite), as well as individual metallic inclusions as the major constituents. A distinct chemical diversity was discovered in the interstitial glass in terms of silica content defined as low and high silica glass end members. Elevated concentrations of Zn, Cr, Cu, Pb and Ba were recorded in the bulk composition. Cu, Pb and Ba behave as incompatible elements since they have been markedly characterized as part of polymetallic alloys and insignificantly sulfides in the form of spherical metallic inclusions associated with tracer amounts of other elements such as Sb, Sn, Ni, Zn, Al, P and Si. In contrast, an appreciable amount of Zn is retained by zinc-rich end members of spinel and partially by melilite and silica glass. Chromium exhibits similar behavior, and is considerably held by Cr-rich spinel. The intense incorporation of Zn and Cr into spinel indicates the very effective enrichment of these two elements into phases more environmentally resistant than glass. There was no evidence, however, that Cu and Pb enter into the structure of the crystalline silicates or oxides that may lead to their easier leachability upon exposure to the environment.

  18. Mass production of chemicals from biomass-derived oil by directly atmospheric distillation coupled with co-pyrolysis

    PubMed Central

    Zhang, Xue-Song; Yang, Guang-Xi; Jiang, Hong; Liu, Wu-Jun; Ding, Hong-Sheng

    2013-01-01

    Production of renewable commodity chemicals from bio-oil derived from fast pyrolysis of biomass has received considerable interests, but hindered by the presence of innumerable components in bio-oil. In present work, we proposed and experimentally demonstrated an innovative approach combining atmospheric distillation of bio-oil with co-pyrolysis for mass production of renewable chemicals from biomass, in which no waste was produced. It was estimated that 51.86 wt.% of distillate just containing dozens of separable organic components could be recovered using this approach. Ten protogenetic and three epigenetic compounds in distillate were qualitatively identified by gas chromatography/mass spectrometry and quantified by gas chromatography. Among them, the recovery efficiencies of acetic acid, propanoic acid, and furfural were all higher than 80 wt.%. Formation pathways of the distillate components in this process were explored. This work opens up a fascinating prospect for mass production of chemical feedstock from waste biomass. PMID:23350028

  19. Mass production of chemicals from biomass-derived oil by directly atmospheric distillation coupled with co-pyrolysis

    NASA Astrophysics Data System (ADS)

    Zhang, Xue-Song; Yang, Guang-Xi; Jiang, Hong; Liu, Wu-Jun; Ding, Hong-Sheng

    2013-01-01

    Production of renewable commodity chemicals from bio-oil derived from fast pyrolysis of biomass has received considerable interests, but hindered by the presence of innumerable components in bio-oil. In present work, we proposed and experimentally demonstrated an innovative approach combining atmospheric distillation of bio-oil with co-pyrolysis for mass production of renewable chemicals from biomass, in which no waste was produced. It was estimated that 51.86 wt.% of distillate just containing dozens of separable organic components could be recovered using this approach. Ten protogenetic and three epigenetic compounds in distillate were qualitatively identified by gas chromatography/mass spectrometry and quantified by gas chromatography. Among them, the recovery efficiencies of acetic acid, propanoic acid, and furfural were all higher than 80 wt.%. Formation pathways of the distillate components in this process were explored. This work opens up a fascinating prospect for mass production of chemical feedstock from waste biomass.

  20. Production and characterization of submicron hematite (α−Fe{sub 2}O{sub 3}) particles by ultrasonic spray pyrolysis method

    SciTech Connect

    Kırcı, Burak; Ebin, Burçak; Gürmen, Sebahattin

    2013-12-16

    The ultrasonic spray pyrolysis (USP) method has been used to prepare submicron hematite (α−Fe{sub 2}O{sub 3}) particles using two different industrial pickling solutions of iron chloride (41 g/L FeCl{sub 2} and 54 g/L FeCl{sub 3}) Particles were obtained by thermal decomposition of generated aerosols from precursor solutions using 1.7 MHz ultrasonic atomizer. Reaction temperature was set up at 800 °C and aerosol droplets were carried into the heated zone by 0.7 L/min air flow rate. X-Ray Diffraction (XRD) studies were used to determine the crystal structure and crystallite size of the particles. Results indicate that patterns correspond to hematite phase with rhombohedral crystal structure (space group: R3c). The crystallite sizes of particles prepared from FeCl{sub 2} and FeCl{sub 3} solutions that were calculated from Scherrer equation are 59 and 33 nm, respectively. Scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS) investigations give detailed information about particle size, morphology and composition. SEM micrographs show that hematite nanoparticles aggregate and formed spherical secondary particles in submicron range.

  1. Physical properties of Zn doped TiO2 thin films with spray pyrolysis technique and its effects in antibacterial activity.

    PubMed

    Arunachalam, A; Dhanapandian, S; Manoharan, C; Sivakumar, G

    2015-03-05

    Zinc doped Titanium dioxide (TiO2: Zn) thin films were deposited onto glass substrates by the spray pyrolysis technique with the substrate temperature 450°C. The structural, optical, photoluminescence (PL) properties and morphological studies were investigated for the films deposited with various doping concentration (0, 2, 4, 6 and 8at.%) of zinc. The results of X-ray diffraction (XRD) had shown the presence of anatase peak with a strong orientation along (101) plane at 8at.% of Zn-doped TiO2 film. Scanning electron microscopy (SEM) study showed the uniform distribution of grains with porous nature. Atomic force microscopy (AFM) observations indicated the tetragonal shape at 8at.% of Zn-doped TiO2 with the particle size and decrease in surface roughness. The emission at 398nm was observed at the 8at.% of Zn-doped TiO2 thin film. The carrier concentration and Hall mobility was increased with doping. The antibacterial activity was highly yielded for the Zn-doped TiO2 thin films.

  2. Facile Spray Pyrolysis Synthesis of Yolk-shell Earth-abundant Elemental NiFe-based Nanohybrid Electrocatalysts for Full Water Splitting.

    PubMed

    Wen, Zhenhai; Li, Hao; Ci, Suqin; Zhang, Mengtian; Chen, Junxiang; Lai, Keyuan

    2017-08-28

    It is critical while remains a daunting challenge in the development of high-activity electrocatalysts for water splitting that comprise only inexpensive, earth-abundant elements. In this work, the preparation of yolk-shell Ni3Fe/Ni3FeN was developed by a possible scale-up method using spray pyrolysis technique. The yolk-shell Ni3Fe/Ni3FeN presents excellent catalytic activity for OER and HER with overpotentials of 268 mV and 166 mV at 10 mA cm-2, respectively, and bears a prominent electrochemical durability. The overall water splitting on the electrolyzer with yolk-shell Ni3Fe/Ni3FeN as cathode and anode only requires a cell voltage of 1.62 V to reach current density of 10 mA cm-2. The present research not only proposes a new route in synthesizing advanced functional electrocatalysts for overall water splitting but also shed light on its potential commercial application. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Effect of fuel rate and annealing process of LiFePO{sub 4} cathode material for Li-ion batteries synthesized by flame spray pyrolysis method

    SciTech Connect

    Halim, Abdul; Setyawan, Heru; Machmudah, Siti; Nurtono, Tantular; Winardi, Sugeng

    2014-02-24

    In this study the effect of fuel rate and annealing on particle formation of LiFePO{sub 4} as battery cathode using flame spray pyrolysis method was investigated numerically and experimentally. Numerical study was done using ANSYS FLUENT program. In experimentally, LiFePO{sub 4} was synthesized from inorganic aqueous solution followed by annealing. LPG was used as fuel and air was used as oxidizer and carrier gas. Annealing process attempted in inert atmosphere at 700°C for 240 min. Numerical result showed that the increase of fuel rate caused the increase of flame temperature. Microscopic observation using Scanning Electron Microscopy (SEM) revealed that all particles have sphere and polydisperse. Increasing fuel rate caused decreasing particle size and increasing particles crystallinity. This phenomenon attributed to the flame temperature. However, all produced particles still have more amorphous phase. Therefore, annealing needed to increase particles crystallinity. Fourier Transform Infrared (FTIR) analysis showed that all particles have PO4 function group. Increasing fuel rate led to the increase of infrared spectrum absorption corresponding to the increase of particles crystallinity. This result indicated that phosphate group vibrated easily in crystalline phase. From Electrochemical Impedance Spectroscopy (EIS) analysis, annealing can cause the increase of Li{sup +} diffusivity. The diffusivity coefficient of without and with annealing particles were 6.84399×10{sup −10} and 8.59888×10{sup −10} cm{sup 2} s{sup −1}, respectively.

  4. The effect of substrate heating temperature upon spray pyrolysis process on the morphological and functional properties of fluorine tin oxide conducting glass

    NASA Astrophysics Data System (ADS)

    Fikri, Dahlin; Yuwono, Akhmad Herman; Sofyan, Nofrijon; Arini, Tri; Lalasari, Latifa Hanum

    2017-03-01

    Transparent conductive oxide (TCO) is one of the main components in the dye sensitized solar cell (DSSC), a device which is developed as one of renewable energy sources that has high potential to substitute fossil fuel. Among all TCO glasses, fluorine-doped tin oxide (FTO) has the biggest potential to be developed. The purpose of this research is aimed at finding an optimum substrate temperature during spray pyrolysis process in order to obtain FTO substrates with the desired characteristics. For this purpose, soda lime glasses were deposited with a mixture of tin and fluorine doping precursors using a special modified ultrasonic nebulizer with a variation in substrate heating temperature of 250, 300, 350, 400, and 450°C. All the fabricated samples were characterized by using x-ray diffraction (XRD), UV-Vis spectrometry, scanning electron microscope (SEM), and digital multimeter. On the basis of investigation, the best result was obtained in the substrate heated at 300 °C, providing an electrical resistance of 8 ohm/sq and optical transmittance of 74%. This research creates a chance for the next fabrication of TCO glass with desired properties using simple-low cost facilities.

  5. Preparation and characterization of Cu2SnS3 ternary semiconductor nanostructures via the spray pyrolysis technique for photovoltaic applications

    NASA Astrophysics Data System (ADS)

    Adelifard, Mehdi; Bagheri Mohagheghi, Mohamad Mehdi; Eshghi, Hosein

    2012-03-01

    Thin films of Cu2SnS3 have been deposited by the spray pyrolysis technique. Various Sn/Cu molar ratios (from 0.0 to 1.0) were applied, which allowed the study of the copper tin sulfide phase. Structural, morphological and compositional analyses have been carried out using x-ray diffraction, field emission scanning electron microscopy and energy dispersive spectroscopy. The pure CuS thin film showed the covellite phase with hexagonal crystal structure, and with increasing the Sn/Cu molar ratio, the films grown were crystallized with triclinic Cu2SnS3 ternary phase. Optical measurement analysis showed that the deposited layers have a relatively high absorption coefficient (~105 cm-1) in the visible spectrum, about one order of magnitude higher than in other published reports. Also these layers presented a reduction of about 1 eV in the values of band gap from 2.57 to 1.58 eV with an increment in the Sn/Cu molar ratio from 0.0 to 1.0. The electrical properties studies showed that all these samples are p-type semiconductors and the resistivity decreases with increasing the Sn/Cu molar ratio.

  6. Structural, microstructural, and optical properties of Zn1- x Mg x O thin films grown onto glass substrate by ultrasonic spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Hoggas, K.; Nouveau, Corinne; Djelloul, A.; Bououdina, M.

    2015-08-01

    Pure and doped Zn1- x Mg x O films were deposited onto glass substrate by ultrasonic spray pyrolysis technique. The variation of lattice constant and the blue shift of near-band-edge emission indicate that Zn2+ ions are successfully substituted by Mg2+ ions within ZnO lattice. At higher Mg content ( x ≥ 0.21), a drastic change appears in the morphology, as a result of structural changes from wurtzite (ZnO) structure into a mixture of wurtzite and cubic (MgO) phases. FTIR study indicated the existence of distinct characteristic absorption peaks at ~442 cm-1 for Zn-O stretching mode that shifted toward the red region with the increase in Mg content. In addition to the host phonons of ZnO, one additional band was observed around 523 cm-1, presumably attributed to the Mg-related vibrational mode. The optical constants and thickness of thin films have been determined using experimental transmittance data. The luminescence intensity at 2.63 eV of Zn0.85Mg0.15O thin films was found to be approximately 13 times higher than that of pure ZnO film measured under the same excitation conditions.

  7. H2 Production Under Visible Light Irradiation from Aqueous Methanol Solution on CaTiO3:Cu Prepared by Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Lim, Sung Nam; Song, Shin Ae; Jeong, Yong-Cheol; Kang, Hyun Woo; Park, Seung Bin; Kim, Ki Young

    2017-10-01

    Perovskite-type photocatalysts of CaCu x Ti1- x O3 (0 ≤ x ≤ 0.02) powder were prepared by spray pyrolysis of aqueous solution or aqueous solution with polymeric additive. The effects of the amount of copper ions doped in the photocatalyst and the precursor type on the photocatalytic activity under visible-light irradiation were investigated. The crystal structure, oxidation state, and light adsorption properties of the prepared photocatalysts were analyzed using x-ray diffraction, x-ray photoelectron spectroscopy, and diffuse reflectance spectroscopy, respectively. The doping of copper ions in CaTiO3 allowed visible-light absorption owing to a narrowing of the band gap energy of the host material through the formation of a new donor level for copper ions. Among the doped samples prepared from the aqueous precursor, CaTiO3 doped with 1 mol.% copper ions had the highest hydrogen evolution rate (140.7 μmol g-1 h-1). Notably, the hydrogen evolution rate of the photocatalyst doped with 1 mol.% copper ions prepared from the aqueous precursor with polymeric additive (295.0 μmol g-1 h-1) was two times greater than that prepared from the aqueous precursor, due to the morphology effect.

  8. Photoelectrochemical performances of n-CdS{sub 1-x}Se{sub x} thin films prepared by spray pyrolysis technique

    SciTech Connect

    Yadav, A.A.; Masumdar, E.U.

    2010-08-15

    The CdS{sub 1-x}Se{sub x} (0.0 {<=} x {<=} 1.0) thin films of various compositions have been deposited onto the amorphous and FTO coated glass substrates using a spray pyrolysis technique. An electrode/electrolyte interface has been formed between an n-type CdS{sub 1-x}Se{sub x} (0.0 {<=} x {<=} 1.0) alloyed/mixed type semiconductor and a sulphide/polysulphide redox electrolyte and investigated through the current-voltage, capacitance-voltage and photovoltaic power output characteristics. The dependence of the dark current through the junction and the junction capacitance on the voltage across the junction have been examined and analysed. Upon illumination of the interface with a light of 20 mW/cm{sup 2}, an open-circuit voltage of the order of 335 mV and a short-circuit current of 1.02 mA/cm{sup 2} have been developed (for x = 0.8), which results in energy conversion efficiency and fill factor 0.79% and 0.46% respectively. The magnitudes of the barrier heights at the interfaces have been determined. The significant electrochemical properties have been observed for a cell with electrode composition x = 0.8. (author)

  9. An easy and innovative method based on spray-pyrolysis deposition to obtain high efficiency cathodes for Solid Oxide Fuel Cells

    NASA Astrophysics Data System (ADS)

    dos Santos-Gómez, L.; Porras-Vázquez, J. M.; Martín, F.; Ramos-Barrado, J. R.; Losilla, E. R.; Marrero-López, D.

    2016-07-01

    A novel electrode preparation method based on the spray-pyrolysis deposition of metal nitrate solutions onto a porous electrolyte scaffold is proposed. This method has been proved with different cathode materials, usually used in Solid Oxide Fuel Cells, such as La0.8Sr0.2MnO3-δ and La0.6Sr0.4Co1-xFexO3-δ (x = 0, 0.2, 0.8 and 1). The electrode microstructure is composed by two layers; the inner layer is a porous electrolyte scaffold homogeneously coated by cathode nanoparticles, providing an increased number of triple phase boundary sites for oxygen reduction, whereas, the top layer is formed by only cathode nanoparticles and acts mainly as a current collector. Polarization resistance values as low as 0.07 and 1.0 Ω cm2 at 600 and 450 °C, respectively, are obtained at open circuit voltage. This alternative approach has several advantages with respect to the traditional wet infiltration method for large area electrode fabrication, such as higher reproducibility, shorter preparation time in a single thermal deposition step, and easy implementation at industrial scale as a continuous process.

  10. Structural and magnetic characterization of LiMn{sub 1.825}Cr{sub 0.175}O{sub 4} spinel obtained by ultrasonic spray pyrolysis

    SciTech Connect

    Jugovic, D.; Kusigerski, V.; Mitric, M.; Miljkovic, M.; Makovec, D.; Uskokovic, D.

    2007-03-22

    Quaternary spinel oxide LiMn{sub 1.825}Cr{sub 0.175}O{sub 4} powder was synthesized by using an ultrasonic spray pyrolysis method, without additional annealing. The crystal structure of the as-prepared powder was revealed by X-ray powder diffraction and identified as a single spinel phase with Fd3m space group. The powders had a spherical morphology with extremely smooth surface appearance and densely congested interior structure. Transmission electron microscopy confirmed that the particle consisted by the cohesion of the primary particles. Magnetic measurements performed in DC field in both zero-field-cooled and field-cooled regimes, as well as AC susceptibility experiments, show that system undergoes spin-glass transition at the freezing temperature T {sub f} = 20 K. The value of the effective magnetic moment {mu} {sub eff} = 4.34 {mu} {sub B} obtained from the Curie-Weiss fit in the high temperature region confirms the substitution of Mn{sup 3+} ions with Cr{sup 3+} ions.

  11. Effect of Sb dopant on the structural, optical and electrical properties of SnS thin films by spray pyrolysis technique.

    PubMed

    Santhosh Kumar, K; Manoharan, C; Dhanapandian, S; Gowri Manohari, A

    2013-11-01

    Thin films of antimony doped tin sulphide (SnS:Sb) with different antimony concentrations have been prepared by the spray pyrolysis technique at the substrate temperature of 350°C. The physical properties of the films were studied as a function of increase in antimony dopant concentration (up to 10at.%). The films were characterized by different techniques to study their structural, optical and electrical properties. The X-ray diffraction analysis revealed that the films were polycrystalline in nature and having orthorhombic crystal structure with a preferred orientation in (111) direction. Due to Sb doping, the crystalline quality and the preferential orientation of SnS films were improved up to 6at.% of doping concentration. However, when doping concentration was increased above 6at.%, the crystalline quality and the preferential orientation of SnS films was deteriorated. Atomic force microscopy images revealed that the surface roughness of the films increased due to Sb doping. Optical measurements showed that the band gap values decreased from 1.60eV to 1.15eV with increase in Sb concentration. The photoluminescence spectra displayed that all the samples have an emission peak centered at 760nm. At 6at.% of Sb doping, the film has the lowest resistivity of 2.598×10(-2)Ωcm while the carrier concentration was high. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Spray pyrolysis growth of a high figure of merit, nano-crystalline, p-type transparent conducting material at low temperature

    NASA Astrophysics Data System (ADS)

    Farrell, L.; Norton, E.; O'Dowd, B. J.; Caffrey, D.; Shvets, I. V.; Fleischer, K.

    2015-07-01

    In this letter, we demonstrate a low temperature (≈345 °C) growth method for Cu deficient CuCrO2 performed by spray pyrolysis using metal-organic precursors and a simple air blast nozzle. Smooth films were grown on glass substrates with a highest conductivity of 12 S/cm. The most conductive samples retain transparencies above 55% resulting in a figure of merit as high as 350 μS, which is the best performing p-type transparent conducting material grown by solution methods to date. Remarkably, despite the nano-crystallinity of the films, properties comparable with crystalline CuCrO2 are observed. No postannealing of the films is required in contrast to previous reports on crystalline material. The low processing temperature of this method means that the material can be deposited on flexible substrates. As this is a solution based technique, it is more attractive to industry as physical vapour deposition methods are slow and costly in comparison.

  13. Role of molar concentration in structural, optical and gas sensing performance of anatase phase TiO2 nanofilms: automated nebulizer spray pyrolysis (ANSP) technique

    NASA Astrophysics Data System (ADS)

    Gopala Krishnan, V.; Elango, P.; Ganesan, V.

    2017-07-01

    TiO2 nanofilms were deposited on a glass substrate at 500 °C using automated nebulizer spray pyrolysis. The anatase polycrystalline structure with increased grain size and variations of surfactant planes ( T c) were influenced by molar concentration on XRD study. AFM study shows the average roughness values were increased with increase in molar concentration. A granular domain like microstructure with crack and void-free particle was examined by FESEM. The maximum transmittance 95.5% (529.6 nm) for x = 0.05 M/L, further increment of molar concentration showed the decremented transmittance with red shift absorption edge and the calculated band gap values ( E g = 3.53-3.20 eV) also noted. The gas sensing performances of films were studied with respect to various gas sensing parameters and the ammonia (NH3) gas showed better sensing response ( S max = 89%) at 150 °C for 300 ppm gas concentration against other gases (C2H6O, CH4O, C3H8O and C3H6O).

  14. Preparation and characterizations of electroluminescent p-ZnO : N/n-ZnO : Ga/ITO thin films by spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Panatarani, C.; Fitriyadi, S.; Balasubramanian, N.; Parmar, N. S.; Joni, I. M.

    2016-02-01

    ZnO thin films were fabricated by spray pyrolysis (SP) method with p-ZnO : N/n-ZnO:Ga/ITO structure. The X-ray results show that the deposited films have hexagonal wurtzite structure. The EDS results observed that the composition of Ga in ZnO:Ga and N in ZnO:N was 3.73% and 27.73% respectively. The photoluminescence (PL) with excitation wave length of 260 nm shows that ZnO:Ga and ZnO:N films emitted UV emission at ˜393 and ˜388 nm, respectively and the films resistivity was 7.12 and 12.80 Ohm-cm respectively. The electroluminescence of the p-ZnO : N/n-ZnO:Ga/ITO structure was obtained by applying forward bias of 5 volt with 30 mA current, resulting in a 3.35 volt threshold bias with the peak electroluminescence in UV-blue range.

  15. Physical properties of Zn doped TiO2 thin films with spray pyrolysis technique and its effects in antibacterial activity

    NASA Astrophysics Data System (ADS)

    Arunachalam, A.; Dhanapandian, S.; Manoharan, C.; Sivakumar, G.

    2015-03-01

    Zinc doped Titanium dioxide (TiO2: Zn) thin films were deposited onto glass substrates by the spray pyrolysis technique with the substrate temperature 450 °C. The structural, optical, photoluminescence (PL) properties and morphological studies were investigated for the films deposited with various doping concentration (0, 2, 4, 6 and 8 at.%) of zinc. The results of X-ray diffraction (XRD) had shown the presence of anatase peak with a strong orientation along (1 0 1) plane at 8 at.% of Zn-doped TiO2 film. Scanning electron microscopy (SEM) study showed the uniform distribution of grains with porous nature. Atomic force microscopy (AFM) observations indicated the tetragonal shape at 8 at.% of Zn-doped TiO2 with the particle size and decrease in surface roughness. The emission at 398 nm was observed at the 8 at.% of Zn-doped TiO2 thin film. The carrier concentration and Hall mobility was increased with doping. The antibacterial activity was highly yielded for the Zn-doped TiO2 thin films.

  16. Effects of ultraviolet light on B-doped CdS thin films prepared by spray pyrolysis method using perfume atomizer

    NASA Astrophysics Data System (ADS)

    Novruzov, V. D.; Keskenler, E. F.; Tomakin, M.; Kahraman, S.; Gorur, O.

    2013-09-01

    Boron doped CdS thin films were deposited by spray pyrolysis method using perfume atomizer. The effects of ultraviolet light on the structural, optical and electrical properties of B-doped CdS thin films were investigated as a function of dopant concentration (B/Cd). X-ray diffraction studies showed that all samples were polycrystalline nature with hexagonal structure. It was determined that the preferred orientation of non-illuminated samples changes from (1 0 1) to (0 0 2) with B concentration. The c lattice constant of films decreases from 6.810 Å to 6.661 Å with boron doping. The XRD peak intensity increased with the illumination for almost all the samples. The lattice parameters of B-doped samples remained nearly constant after illumination. It was found that the optical transmittance, photoluminescence spectra, resistivity and carrier concentration of the B-doped samples are stable after the illumination with UV light. Also the effects of UV light on B-doped CdS/Cu2S solar cell were investigated and it was determined that photoelectrical parameters of B-doped solar cell were more durable against the UV light.

  17. High power density cell using nanostructured Sr-doped SmCoO3 and Sm-doped CeO2 composite powder synthesized by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Shimada, Hiroyuki; Yamaguchi, Toshiaki; Suzuki, Toshio; Sumi, Hirofumi; Hamamoto, Koichi; Fujishiro, Yoshinobu

    2016-01-01

    High power density solid oxide electrochemical cells were developed using nanostructure-controlled composite powder consisting of Sr-doped SmCoO3 (SSC) and Sm-doped CeO2 (SDC) for electrode material. The SSC-SDC nano-composite powder, which was synthesized by spray pyrolysis, had a narrow particle size distribution (D10, D50, and D90 of 0.59, 0.71, and 0.94 μm, respectively), and individual particles were spherical, composing of nano-size SSC and SDC fragments (approximately 10-15 nm). The application of the powder to a cathode for an anode-supported solid oxide fuel cell (SOFC) realized extremely fine cathode microstructure and excellent cell performance. The anode-supported SOFC with the SSC-SDC cathode achieved maximum power density of 3.65, 2.44, 1.43, and 0.76 W cm-2 at 800, 750, 700, and 650 °C, respectively, using humidified H2 as fuel and air as oxidant. This result could be explained by the extended electrochemically active region in the cathode induced by controlling the structure of the starting powder at the nano-order level.

  18. Effects of Different Salts on Salt-Assisted Ultrasonic Spray Pyrolysis (SA-USP) Calcination for the Synthesis of Strontium Ferrite.

    PubMed

    Hwang, Tea-Yeon; An, Guk-Hwan; Cho, Jeong-Ho; Kim, Jongryoul; Choa, Yong-Ho

    2015-10-01

    Strontium ferrite (hexaferrite), SrFe12O19, was successfully fabricated in sizes ranging from hundreds of nanometers to several micrometers by salt-assisted ultrasonic spray pyrolysis-calcination using different salt media. All samples were single phases of SrFe12O19 without the intermediate phase, α-Fe2O3, and their morphology was hexagonal. As calcination temperature increased, the size of as-calcined samples and saturation magnetization, Ms, increased while coercivity decreased. The particle size of the obtained nanoparticles varied depending on the salt media and calcination temperatures. The best magnetic properties obtained in this experiment were a coercivity of 6973 Oe with a saturation magnetization of 68.3 emu/g. To the best of our knowledge, these coercivity values are the highest ever obtained. We propose a detailed mechanism explaining the growth of these particles and conclude that the resulting single-domain particle size is about 70 nm, taking into account of factors affecting coercivity in ferrite nano- to micro-sized particles.

  19. Effect of Sn doping on the structural, optical and electrical properties of TiO2 films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Arunachalam, A.; Dhanapandian, S.; Manoharan, C.

    2016-02-01

    In this work, highly oriented pure and Tin-doped Titanium dioxide (Sn-doped TiO2) with porous nature photoelectrodes were deposited on ITO glass plates using spray pyrolysis technique. The XRD pattern revealed the formation of anatase TiO2 with the maximum intensity of (101) plane while doping 6 at% of Sn. The morphological studies depicted the porous nature with the uniform arrangement of small-sized grains. The presence of tin confirmed with the EDX spectra. The size of particles of 13 nm was observed from High Resolution Transmission Electron Microscopy (HR-TEM) analysis. The average transmittance was about 85% for the doped photoelectrode and was observed for the photoelectrode deposited with 6 at% of tin, with decreased energy band gap. The PL study showed the emission peak at 391 nm. The maximum carrier concentration and Hall mobility was observed for the photoelectrode deposited with 6 at% of tin. With these studies, the DSSCs were prepared separately with the dye extracted from Hibiscus Rosasinesis and Hibiscus Surttasinesis and their efficiency was maximum for the DSSC prepared with 6 at% of tin.

  20. Peculiarities in electrical and optical properties of Cu2Zn1- x Mn x SnS4 films obtained by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Orletskii, I. G.; Mar'yanchuk, P. D.; Solovan, M. N.; Maistruk, E. V.; Kozyarskii, D. P.

    2016-03-01

    Thin films of Cu2Zn1- x Mn x SnS4 (0 ≤ x ≤ 1) solid solutions have been obtained for the first time by the spray pyrolysis of aqueous salt solutions (copper, zinc, manganese, and tin chlorides and thiourea) at a temperature of T S = 563 K. The films possess specific electric conductivities within σ ≈ 35-422 Ω-1 cm-1 and optical bandgap width E g op that increases with the manganese content from 1.54 eV ( x = 0) to 2.25 eV ( x = 1). Electrical and optical properties of the obtained films have been studied and analyzed based on a model of polycrystalline materials with grain boundaries. The energy barriers Eb between grains have been determined. The dependence of the bandgap of Cu2Zn1- x Mn x SnS4 (0 ≤ x ≤ 1) solid solutions on the composition has been established using the results of measurements of the optical transmission and absorption coefficients.

  1. Title III section 313 release reporting guidance: Estimating chemical releases from spray application of organic coatings

    SciTech Connect

    Not Available

    1988-01-01

    Spray applicators of organic coatings may be required to report annually any releases to the environment of certain chemicals regulated under Section 313, Title III, of the Superfund Amendments and Reauthorization Act (SARA) of 1986. The document has been developed to assist appliers of organic coatings in the completion of Part III (Chemical Specific Information) of the Toxic Chemical Release Inventory Reporting Form. Included herein is general information on toxic chemicals used and process wastes generated, along with several examples to demonstrate the types of data needed and various methodologies available for estimating releases.

  2. Pyrolysis temperature affects phosphorus transformation in biochar: Chemical fractionation and (31)P NMR analysis.

    PubMed

    Xu, Gang; Zhang, You; Shao, Hongbo; Sun, Junna

    2016-11-01

    Phosphorus (P) recycling or reuse by pyrolyzing crop residue has recently elicited increased research interest. However, the effects of feedstock and pyrolysis conditions on P species have not been fully understood. Such knowledge is important in identifying the agronomic and environmental uses of biochar. Residues of three main Chinese agricultural crops and the biochars (produced at 300°C-600°C) derived from these crops were used to determine P transformations during pyrolysis. Hedley sequential fractionation and (31)P NMR analyses were used in the investigation. Our results showed that P transformation in biochar was significantly affected by pyrolysis temperature regardless of feedstock (Wheat straw, maize straw and peanut husk). Pyrolysis treatment transformed water soluble P into a labile (NaHCO3-Pi) or semi-labile pool (NaOH-Pi) and into a stable pool (Dil. HCl P and residual-P). At the same time, organic P was transformed into inorganic P fractions which was identified by the rapid decomposition of organic P detected with solution (31)P NMR. The P transformation during pyrolysis process suggested more stable P was formed at a higher pyrolysis temperature. This result was also evidenced by the presence of less soluble or stable P species, such as such as poly-P, crandallite (CaAl3(OH)5(PO4)2) and Wavellite (Al3(OH)3(PO4)2·5H2O), as detected by solid-state (31)P NMR in biochars formed at a higher pyrolysis temperature. Furthermore, a significant proportion of less soluble pyrophosphate was identified by solution (2%-35%) and solid-state (8%-53%) (31)P NMR, which was also responsible for the stable P forms at higher pyrolysis temperature although their solubility or stability requires further investigation. Results suggested that a relatively lower pyrolysis temperature retains P availability regardless of feedstock during pyrolysis process. Copyright © 2016. Published by Elsevier B.V.

  3. Characterization of bidisperse magnetorheological fluids utilizing maghemite (γ-Fe2O3) nanoparticles synthetized by flame spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Jönkkäri, I.; Sorvali, M.; Huhtinen, H.; Sarlin, E.; Salminen, T.; Haapanen, J.; Mäkelä, J. M.; Vuorinen, J.

    2017-09-01

    In this study we have used liquid flame spray (LFS) process to synthetize γ-Fe2O3 nanoparticles of two different average sizes. Different sized nanoparticles were generated with two different liquid precursor feed rates in the spray process, higher feed rate resulting in larger nanoparticles with higher saturation magnetization. The nanoparticles were used in bidisperse magnetorheological fluids to substitute 5% of the micron sized carbonyl iron particles. To our knowledge this is the first time particles synthetized by the LFS method have been used in magnetorheological fluids. The bidisperse fluids showed significantly improved sedimentation stability compared to a monodisperse suspension with the same solid concentration. The tradeoff was an increased viscosity without magnetic field. The effect of the nanoparticles on the rheological properties under external magnetic field was modest. Finally, the dynamic oscillatory testing was used to evaluate the structural changes in the fluids under magnetic field. The addition of nanoparticles decreased the elastic portion of the deformation and increased the viscous portion.

  4. A multiple shock tube and chemical kinetic modeling study of diethyl ether pyrolysis and oxidation.

    PubMed

    Yasunaga, K; Gillespie, F; Simmie, J M; Curran, H J; Kuraguchi, Y; Hoshikawa, H; Yamane, M; Hidaka, Y

    2010-09-02

    The pyrolysis and oxidation of diethyl ether (DEE) has been studied at pressures from 1 to 4 atm and temperatures of 900-1900 K behind reflected shock waves. A variety of spectroscopic diagnostics have been used, including time-resolved infrared absorption at 3.39 mum and time-resolved ultraviolet emission at 431 nm and absorption at 306.7 nm. In addition, a single-pulse shock tube was used to measure reactant, intermediate, and product species profiles by GC samplings at different reaction times varying from 1.2 to 1.8 ms. A detailed chemical kinetic model comprising 751 reactions involving 148 species was assembled and tested against the experiments with generally good agreement. In the early stages of reaction the unimolecular decomposition and hydrogen atom abstraction of DEE and the decomposition of the ethoxy radical have the largest influence. In separate experiments at 1.9 atm and 1340 K, it is shown that DEE inhibits the reactivity of an equimolar mixture of hydrogen and oxygen (1% of each).

  5. Physical and Chemical Properties of Bio-Oils From Microwave Pyrolysis of Corn Stover

    NASA Astrophysics Data System (ADS)

    Yu, Fei; Deng, Shaobo; Chen, Paul; Liu, Yuhuan; Wan, Yiqin; Olson, Andrew; Kittelson, David; Ruan, Roger

    This study was aimed to understand the physical and chemical properties of pyrolytic bio-oils produced from microwave pyrolysis of corn stover regarding their potential use as gas turbine and home heating fuels. The ash content, solids content, pH, heating value, minerals, elemental ratio, moisture content, and viscosity of the bio-oils were determined. The water content was approx 15.2 wt%, solids content 0.22 wt%, alkali metal content 12 parts per million, dynamic viscosity 185 mPa·s at 40°C, and gross high heating value 17.5 MJ/kg for a typical bio-oil produced. Our aging tests showed that the viscosity and water content increased and phase separation occurred during the storage at different temperatures. Adding methanol and/or ethanol to the bio-oils reduced the viscosity and slowed down the increase in viscosity and water content during the storage. Blending of methanol or ethanol with the bio-oils may be a simple and cost-effective approach to making the pyrolytic bio-oils into a stable gas turbine or home heating fuels.

  6. Physical and chemical properties of bio-oils from microwave pyrolysis of corn stover.

    PubMed

    Yu, Fei; Deng, Shaobo; Chen, Paul; Liu, Yuhuan; Wan, Yiqin; Olson, Andrew; Kittelson, David; Ruan, Roger

    2007-04-01

    This study was aimed to understand the physical and chemical properties of pyrolytic bio-oils produced from microwave pyrolysis of corn stover regarding their potential use as gas turbine and home heating fuels. The ash content, solids content, pH, heating value, minerals, elemental ratio, moisture content, and viscosity of the bio-oils were determined. The water content was approx 15.2 wt%, solids content 0.22 wt%, alkali metal content 12 parts per million, dynamic viscosity 185 mPa.s at 40 degrees C, and gross high heating value 17.5 MJ/kg for a typical bio-oil produced. Our aging tests showed that the viscosity and water content increased and phase separation occurred during the storage at different temperatures. Adding methanol and/or ethanol to the bio-oils reduced the viscosity and slowed down the increase in viscosity and water content during the storage. Blending of methanol or ethanol with the bio-oils may be a simple and cost-effective approach to making the pyrolytic bio-oils into a stable gas turbine or home heating fuels.

  7. Spray pyrolysis deposition of Cu-ZnO and Zn-SnO{sub 2} solar cells

    SciTech Connect

    Khelfane, A.; Tarzalt, H.; Sebboua, B.; Zerrouki, H.; Kesri, N.

    2015-12-31

    Large-gap metal oxides, such as titanium, tin, and zinc oxides, have attracted great interest because of their remarkable potential in dye-sensitized solar cells (DSSC) and their low cost and simple preparation procedure. In this work, we investigated several Zn-SnO{sub 2} and Cu-ZnO thin films that were sprayed under different experimental conditions. We varied [Zn/[Sn] and [Cu/[Zn] ratios, calculated on atomic percent in the starting solution. We report some structural results of the films using X-ray diffraction. Optical reflection and transmission spectra investigated by an UV/VIS/NIR spectrophotometer permit the determination of optical constants. The direct band gap was deduced from the photon energy dependence of the absorption coefficient.

  8. Electrostatic spraying in the chemical control of Triozoida limbata (Enderlein) (Hemiptera: Triozidae) in guava trees (Psidium guajava L.).

    PubMed

    Tavares, Rafael M; Cunha, João Par; Alves, Thales C; Bueno, Mariana R; Silva, Sérgio M; Zandonadi, César Hs

    2017-06-01

    Owing to the difficulty in reaching targets during pesticide applications on guava trees, it is important to evaluate new technologies that may improve pest management. In electrostatic spraying, an electric force is added to the droplets to control their movements such that they are efficiently directed to the target. The present study evaluated the performance of electrostatic and non-electrostatic spraying in the control of the guava psyllid, the deposition of the spray mixture on the leaves and the losses to the soil. The deposition of the spray mixture was up to 2 times greater when using electrostatic spraying in comparison with non-electrostatic application. The losses of the spray mixture to the soil were up to 4 times smaller with the electrostatic spraying. Electrostatic spraying had better control of the psyllid. It was possible to reduce the volume rate of application with electrostatic spraying without adversely affecting the control of the guava psyllid. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  9. Slow pyrolysis of prot, alkali and dealkaline lignins for production of chemicals.

    PubMed

    Biswas, Bijoy; Singh, Rawel; Kumar, Jitendra; Khan, Adnan Ali; Krishna, Bhavya B; Bhaskar, Thallada

    2016-08-01

    Effect of different lignins were studied during slow pyrolysis. Maximum bio-oil yield of 31.2, 34.1, and 29.5wt.% was obtained at 350, 450 and 350°C for prot lignin, alkali lignin and dealkaline lignin respectively. Maximum yield of phenolic compounds 78%, 80% and 92% from prot lignin, alkali and dealkaline lignin at 350, 450 and 350°C. The differences in the pyrolysis products indicated the source of lignins such as soft and hard wood lignins. The biochar characterisation revealed that the various ether linkages were broken during pyrolysis and lignin was converted into monomeric substituted phenols. Bio-oil showed that the relative contents of each phenolic compound changes significantly with pyrolysis temperature and also the relative contents of each compound changes with different samples.

  10. Physi-chemical and sorption properties of biochars prepared from peanut shell using thermal pyrolysis and microwave irradiation.

    PubMed

    Chu, Gang; Zhao, Jing; Chen, Fangyuan; Dong, Xudong; Zhou, Dandan; Liang, Ni; Wu, Min; Pan, Bo; Steinberg, Christian E W

    2017-08-01

    Microwave irradiation (MW) is an effective technique in heating and pyrolysis. This study compared the properties of peanut shell-biochars produced using MW and muffle furnace (FN). At the same pyrolysis temperature, MW biochars preserved more biomass (as indicated by their higher yields and higher abundance of functional groups) and possessed larger surface areas due to the high abundance of micropores. MW biochars generally exhibited higher adsorption of carbamazepine (CBZ) and bisphenol A (BPA) than FN biochars. However, their surface area-normalized sorption was lower, suggesting that the inner pores may not be fully available to CBZ and BPA sorption. We observed significant free radical signals in both types of biochars. Although CBZ and BPA did not degrade in the biochar sorption systems, the potential role of stronger free radical signals in MW biochars for organic contaminant control may not be overlooked in studies with other chemicals. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Comparison of Physical-chemical and Mechanical Properties of Chlorapatite and Hydroxyapatite Plasma Sprayed Coatings

    PubMed Central

    Demnati, Imane; Grossin, David; Marsan, Olivier; Bertrand, Ghislaine; Collonges, Gérard; Combes, Christèle; Parco, Maria; Braceras, Inigo; Alexis, Joel; Balcaen, Yannick; Rey, Christian

    2015-01-01

    Chlorapatite can be considered a potential biomaterial for orthopaedic applications. Its use as plasma-sprayed coating could be of interest considering its thermal properties and particularly its ability to melt without decomposition unlike hydroxyapatite. Chlorapatite (ClA) was synthesized by a high-temperature ion exchange reaction starting from commercial stoichiometric hydroxyapatites (HA). The ClA powder showed similar characteristics as the original industrial HA powder, and was obtained in the monoclinic form. The HA and ClA powders were plasma-sprayed using a low-energy plasma spraying system with identical processing parameters. The coatings were characterized by physical-chemical methods, i.e. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy, including distribution mapping of the main phases detected such as amorphous calcium phosphate (ACP), oxyapatite (OA), and HA or ClA. The unexpected formation of oxyapatite in ClA coatings was assigned to a side reaction with contaminating oxygenated species (O2, H2O). ClA coatings exhibited characteristics different from HA, showing a lower content of oxyapatite and amorphous phase. Although their adhesion strength was found to be lower than that of HA coatings, their application could be an interesting alternative, offering, in particular, a larger range of spraying conditions without formation of massive impurities. PMID:25893015

  12. Deposition of LaMO 3 (M=Co, Cr, Al) films by spray pyrolysis in inductively coupled plasma

    NASA Astrophysics Data System (ADS)

    Ichinose, Hiromichi; Katsuki, Hiroaki; Nagano, Masamitsu

    1994-11-01

    LaMO 3 (M=Co, Cr, Al) films were prepared on substrates by introducing ultrasonically atomized metal nitrate solutions into an inductively coupled plasma under atmospheric pressure (spray-ICP technique). Dense perovskite-type oxide films of LaCoO 3 and LaCrO 3 were obtained at 600-900°C, while the LaAiO 3 films consisted of loosely packed aggregates. Deposition rates of the films were 6-35 nm/min at 600-900°C. The high temperature phases (cubic) of LaCoO 3 and LaAlO 3 crystallized due to effect of grain size. LaCrO 3 film crystallized in the room temperature phase (orthorhombic). LaCoO 3 was highly oriented to (100) on MgO(100), and LaCrO 3 to (011) and (101) on sapphire(001). Lowest electric resistivities of LaCoO 3 and LaCrO 3 film on MgO were 9.8X10 -3 and 2.7X10 -1 Ω m, respectively, at room temperature.

  13. Comparative studies of CdS, CdS:Al, CdS:Na and CdS:(Al-Na) thin films prepared by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Yılmaz, S.; Atasoy, Y.; Tomakin, M.; Bacaksız, E.

    2015-12-01

    In the present study, the spray pyrolysis technique was used to prepare pure CdS, 4 at.% Al-doped CdS, 4 at.% Na-doped CdS and (4 at.% Al, 4 at.% Na)-co-doped CdS thin films. It was found from X-ray diffraction data that all the specimens showed hexagonal wurtzite structure with the preferred orientation of (101). Scanning electron microscopy results indicated that 4 at.% Al-doping caused a grain growth in the morphology of CdS thin films whereas the 4 at.% Na-doping and (4 at.% Al, 4 at.% Na)-co-doping led to porous structure with small grains. The band gap value of CdS thin films increased to 2.42 eV after 4 at.% Al-doping. However, it reduced to 2.30 eV and 2.08 eV for 4 at.% Na-doping and (4 at.% Al, 4 at.% Na)-co-doping, respectively. The room temperature photoluminescence measurements illustrated that the peak intensity of CdS thin films enhanced with 4 at.% Al-doping while 4 at.% Na-doping and (4 at.% Al, 4 at.% Na)-co-doping caused a decline in the intensity. The maximum carrier concentration and minimum resistivity were obtained for 4 at.% Al-doped CdS thin films, which is associated with the grain growth. Furthermore, (4 at.% Al, 4 at.% Na)-co-doping gave rise to a slight reduction in the carrier concentration and a slight increment in the resistivity. As a result, it can be said that 4 at.% Al-doped CdS thin films exhibited the best electrical and optical properties, which is important for the opto-electronic applications.

  14. Investigations of AlGaN/GaN MOS-HEMT with Al2O3 deposition by ultrasonic spray pyrolysis method

    NASA Astrophysics Data System (ADS)

    Chou, Bo-Yi; Hsu, Wei-Chou; Liu, Han-Yin; Lee, Ching-Sung; Wu, Yu-Sheng; Sun, Wen-Ching; Wei, Sung-Yen; Yu, Sheng-Min; Chiang, Meng-Hsueh

    2015-01-01

    This work investigates Al2O3/AlGaN/GaN metal-oxide-semiconductor high electron mobility transistors (MOS-HEMTs) grown on SiC substrate by using the non-vacuum ultrasonic spray pyrolysis deposition (USPD) method. The Al2O3 was deposited as gate dielectric and surface passivation simultaneously to effectively suppress gate leakage current, enhance output current density, reduce RF drain current collapse, and improve temperature-dependent stabilities performance. The present MOS-HEMT design has shown improved device performances with respect to a Schottky-gate HEMT, including drain-source saturation current density at zero gate bias (IDSS: 337.6 mA mm-1 → 462.9 mA mm-1), gate-voltage swing (GVS: 1.55 V → 2.92 V), two-terminal gate-drain breakdown voltage (BVGD: -103.8 V → -183.5 V), unity-gain cut-off frequency (fT: 11.3 GHz → 17.7 GHz), maximum oscillation frequency (fmax: 14.2 GHz → 19.1 GHz), and power added effective (P.A.E.: 25.1% → 43.6%). The bias conditions for measuring fT and fmax of the studied MOS-HEMT (Schottky-gate HEMT) are VGS = -2.5 (-2) V and VDS = 7 V. The corresponding VGS and VDS biases are -2.5 (-2) V and 15 V for measuring the P.A.E. characteristic. Moreover, small capacitance-voltage (C-V) hysteresis is obtained in the Al2O3-MOS structure by using USPD. Temperature-dependent characteristics of the present designs at 300-480 K are also studied.

  15. Synthesis of Zn1- x Co x Al2O4 Spinel Nanoparticles by Liquid-Feed Flame Spray Pyrolysis: Ceramic Pigments Application

    NASA Astrophysics Data System (ADS)

    Betancur Granados, Natalia; Yi, Eongyu; Laine, Richard M.; Restrepo Baena, Oscar Jaime

    2016-01-01

    Zn1- x Co x Al2O4 ( x = 0.0, 0.2, 0.4, 0.6, 0.8, and 1.0) spinel nanoparticles were synthesized by a liquid-feed flame spray pyrolysis (LF-FSP) method by combusting metallorganic precursor solutions to produce nanopowders with precise composition control. The precursor solutions were aerosolized into a methane/oxygen flame where it was combusted in an oxygen-rich environment to result in nanopowders at a single step. The nanopowders were analyzed by x-ray diffraction, Fourier transform infrared spectroscopy, colorimetry, field emission scanning electron microscopy, transmission electron microscopy, and BET (Brunauer-Emmett-Teller) N2 adsorption. Results show formation of spherical nanopowders with specific surface areas of 42 m2/g to 50 m2/g, which correspond to average particle sizes of 26 nm to 31 nm. Single-phase materials were obtained with a high control of composition, which indicates that LF-FSP is an excellent method to produce mixed-metal oxides for applications in which powder homogeneity is crucial. The products were evaluated for ceramic pigment application, where the ratio of Zn to Co was gradually changed to observe the color change in the structure with the increase of cobalt concentration. The resulting pigments were calcined at 1200°C, which aimed to identify the color stability after a high-temperature process, whereby the colors were measured using the color space CIE L*a*b* under standardized light, D65. Finally, the powders were tested for ceramic decoration using transparent glazes and ceramic bodies. The application was carried out at 1250°C to evaluate the color performance after a decoration process.

  16. Characterization of a Heterostructure TiO2/SnO2:F/SUBSTRATE with Two Different Geometries, Prepared by Spray Pyrolysis to BE Used as Photocatalyst

    NASA Astrophysics Data System (ADS)

    Velázquez-Cruz, E. I.; Anaya-Castillejos, K. M.; Martínez-Martínez, R.; Soto-Guzmán, A. B.; Falcony, C.

    2013-07-01

    Two TiO2/SnO2:F/substrate hetero-structures (HS) with different geometry were deposited by spray pyrolysis. The thickness for the TiO2 and SnO2:F films was 3.8 μm and 2.3 μm, and the band gap energy 3.3 eV and 3.6 eV, respectively. Both films have a transmittance greater than 70% in most of the visible spectrum. The electrical resistivity of the SnO2:F film was ρ = (1.7)×10-4Ω ṡ cm. The surface morphology of the TiO2 film shows hemispheric agglomerates formed by nano-metric needle/platy shaped particles that give them a porous texture much like a "ball of wool," the length of the needles is from 100 nm and its thickness close to 20 nm. The geometry of HS has an important influence on its efficiency as photocatalyst under low-powered UV radiation. One of the geometry for this HS, in which the TiO2/SnO2:F interface is exposed, showed greater efficiency than the TiO2 and SnO2:F films separately, or than the common "sandwich" type HS geometry. Specifically, a decrease by 62% of the initial concentration of a watery solution of methylene blue (mb) of 20 ppm in approximately 5 h of UV radiation is observed for the exposed interface HS compared with less than 30% reduction observed for the common sandwich type HS.

  17. Soil organic degradation: bridging the gap between Rock-Eval pyrolysis and chemical characterization (CPMAS 13C NMR)

    NASA Astrophysics Data System (ADS)

    Albrecht, Remy; Sebag, David; Verrecchia, Eric

    2013-04-01

    Being a source of mineral nutrients, organic matter contributes to soil chemical fertility and acts on soil physical fertility through its role in soil structure. Soil organic matter (SOM) is a key component of soils. Despite the paramount importance of SOM, information on its chemistry and behaviour in soils is incomplete. Numerous methods are used to characterize and monitor OM dynamics in soils using different approaches (Kogel-Knabner, 2000). Two of the main approaches are evaluated and compared in this study. Rock-Eval pyrolysis (RE pyrolysis) provides a description of a SOM's general evolution using its thermal resistance. The second tool (13C CPMAS NMR) aims to give precise and accurate chemical information on OM characterization. The RE pyrolysis technique was designed for petroleum exploration (Lafargue et al., 1998) and because of its simplicity, it has been applied to a variety of other materials such as soils or Recent sediments (Disnar et al., 2000; Sebag, 2006). Recently, RE pyrolysis became a conventional tool to study OM dynamics in soils. In RE pyrolysis, a peak deconvolution is applied to the pyrolysis signal in order to get four main components related to major classes of organic constituents. These components differ in origin and resistance to pyrolysis: labile biological constituents (F1), resistant biological constituents (F2), immature non-biotic constituents (F3) and a mature refractory fraction (F4) (Sebag, 2006; Coppard, 2006). Main advantages of the technique are its repeatability, and rapidity to provide an overview of OM properties and stocks. However, do the four major classes used in the literature reflect a pertinent chemical counterpart? To answer this question, we used 13C Nuclear Magnetic Resonance Spectroscopy in the solid state (13C CPMAS NMR) to collect direct information on structural and conformational characteristics of OM. NMR resonances were assigned to chemical structures according to five dominant forms: alkyl C, O

  18. Elaboration of Ti{sub 0.5}Pb{sub 0.5}Sr{sub 2}CaCu{sub 2}O{sub x} superconducting phases by an ultrasonic spray-pyrolysis process

    SciTech Connect

    Abraham, R.; Guenard, F.; Lebbou, K.; Trosset, S.; Cohen-Adad, M.T.; Jorda, J.L.; Couach, M.

    1998-02-01

    An ultrasonic spray-pyrolysis process has been used to prepare a homogeneous T{sub 10.5}Pb{sub 0.5}Sr{sub 2}CaCu{sub 2}O{sub x} high-temperature superconductor. Depending on experimental conditions, the grain morphology changes from platelet to cauliflower-like, contrary to the three copper layers series. The (Tl/Pb)-Sr-1212 phase has remarkable stability and does not decompose before melting. The critical temperature onset, about 80 K, is similar to that for samples prepared by the usual sintering methods.

  19. The Influence of Process Conditions on the Chemical Composition of Pine Wood Catalytic Pyrolysis Oils

    DOE PAGES

    Pereira, J.; Agblevor, F. A.; Beis, S. H.

    2012-01-01

    Pine wood samples were used as model feedstock to study the properties of catalytic fast pyrolysis oils. The influence of two commercial zeolite catalysts (BASF and SudChem) and pretreatment of the pine wood with sodium hydroxide on pyrolysis products were investigated. The pyrolysis oils were first fractionated using column chromatography and characterized using GC-MS. Long chain aliphatic hydrocarbons, levoglucosan, aldehydes and ketones, guaiacols/syringols, and benzenediols were the major compounds identified in the pyrolysis oils. The catalytic pyrolysis increased the polycyclic hydrocarbons fraction. Significant decreases in phthalate derivatives using SudChem and long chain aliphatics using BASF catalyst were observed. Significant amountsmore » of aromatic heterocyclic hydrocarbons and benzene derivatives were formed, respectively, using BASF and SudChem catalysts. Guaiacyl/syringyl and benzenediols derivatives were partly suppressed by the zeolite catalysts, while the sodium hydroxide treatment enriched phenolic derivatives. Zeolite catalyst and sodium hydroxide were employed together; they showed different results for each catalyst.« less

  20. Comparison of the effect of wet and dry torrefaction on chemical structure and pyrolysis behavior of corncobs.

    PubMed

    Zheng, Anqing; Zhao, Zengli; Chang, Sheng; Huang, Zhen; Zhao, Kun; Wei, Guoqiang; He, Fang; Li, Haibin

    2015-01-01

    Wet and dry torrefaction of corncobs was conducted in high-pressure reactor and tube-type reactor, respectively. Effect of wet and dry torrefaction on chemical structure and pyrolysis behavior of corncobs was compared. The results showed that hemicellulose could be effectively removed from corncobs by torrefaction. However, dry torrefaction caused severe degradation of cellulose and the cross-linking and charring of corncobs. X-ray diffraction analysis revealed that crystallinity degree of corncobs was evidently enhanced during wet torrefaction, but reduced during dry torrefaction as raising treatment temperature. In thermogravimetric analysis, wet torrefied corncobs produced less carbonaceous residues than raw corncobs, while dry torrefied corncobs gave much more residues owing to increased content of acid insoluble lignin. Pyrolysis-gas chromatography/mass spectroscopy analysis indicated that wet torrefaction significantly promoted levoglucosan yield owing to the removal of alkali metals. Therefore, wet torrefaction can be considered as a more effective pretreatment method for fast pyrolysis of biomass. Copyright © 2014 Elsevier Ltd. All rights reserved.

  1. The KIVA-II computer program for transient multidimensional chemically reactive flows with sprays

    SciTech Connect

    Amsden, A.A.; Butler, T.D.; O'Rourke, P.J.

    1987-01-01

    Since its public release in 1985, the KIVA computer program has been utilized for the time dependent analysis of chemically reacting flows with sprays in two and three space dimensions. This paper describes some of the improvements to the original version that have been made since that time. The new code called KIVA-II is planned for public release in early 1988. KIVA-II improves the earlier version in the accuracy and efficiency of the computational procedure, the accuracy of the physics submodels, and in versatility and ease of use. Numerical improvements include the use of the ICE solution procedure in place of the acoustic subcycling method and the implementation of a quasi-second-order-accurate convection scheme. Major extensions to the physical submodels include the inclusion of an optional k-epsilon turbulence model, and several additions to the spray model. We illustrate some of the new capabilities by means of example solutions. 25 refs., 7 figs.

  2. Effect of pyrolysis temperature on chemical and physical properties of sewage sludge biochar.

    PubMed

    Khanmohammadi, Zahra; Afyuni, Majid; Mosaddeghi, Mohammad Reza

    2015-03-01

    The objective of this study was to evaluate the effects of pyrolysis temperatures (300, 400, 500, 600 and 700°C) on properties of biochar produced from an urban sewage sludge. Biochar yield significantly decreased from 72.5% at 300°C to 52.9% at 700°C, whereas an increase in temperature increased the gas yield. Biochar pH and electrical conductivity increased by 3.8 and 1.4 dS m⁻¹, proportionally to the increment of temperature. Biochar produced at low temperatures had higher total nitrogen and total organic carbon content but a lower C/N ratio, calcium carbonate equivalent, and total P, K and Na contents. Total and diethylene triamine penta acetic acid (DTPA)-extractable concentrations of Fe, Zn, Cu, Mn, Ni, Cr and Pb increased with increment of temperature. Lower DTPA-extractable concentrations of Fe, Zn, Cu, Mn, Ni and Pb were found in biochars compared to the sewage sludge. Pyrolysis decreased bulk density, whereas particle density and porosity increment was observed upon pyrolysis with increment of temperature. Sewage sludge saturated water content (θs ) was 130.4 g 100g⁻¹ and significantly greater than biochar, but biochar θs significantly increased with temperature (95.7 versus 105.4 g 100g⁻¹ at 300 and 700°C, respectively). Pyrolysis decreased the biochar's water repellency, assessed by molarity of ethanol droplet (MED), compared to the sewage sludge. The lowest MED of 0.2 and water repellency rating of 3 were found for the biochar produced at 700°C. Based on our results and considering the energy consumption, pyrolysis temperature in the range of 300-400°C may be suggested for sewage sludge pyrolysis.

  3. Spray-dried voriconazole-cyclodextrin complexes: solubility, dissolution rate and chemical stability.

    PubMed

    Miletic, Tijana; Kyriakos, Kachrimanis; Graovac, Adrijana; Ibric, Svetlana

    2013-10-15

    The present work investigates the effect of complexation with hydroxypropyl-beta-cyclodextrin (HPBCD) and 2-O-methyl-beta-cyclodextrin (2-O-MBCD), on voriconazole solubility, dissolution rate and chemical stability. Drug-cyclodextrin complexes were prepared as aqueous solutions, which were spray-dried, and their properties were compared to wet ground samples and physical mixtures. DSC analysis revealed absence of crystalline voriconazole from spray-dried complexes. FTIR spectroscopy indicated changes in the H-bonding network of the hydroxyl groups of cyclodextrin following drug inclusion. Dissolution rate of voriconazole was significantly higher from spray-dried complexes with either cyclodextrin in comparison with free drug, physical mixtures, or wet ground mixtures. However, two degradation impurities were found in aged samples, with slightly higher impurity level with HPBCD. Performed solubility studies suggested that 2-O-MBCD is more efficient solubilizer. Molecular docking simulations showed a difference in the 1:1 binding affinities and sites, with HPBCD surprisingly forming complexes of much lower energy, thus suggesting a multiple rather than a 1:1 complexation.

  4. Production Mechanism, Number Concentration, Size Distribution, Chemical Composition, and Optical Properties of Sea Spray Aerosols Workshop, Summer 2012

    SciTech Connect

    Meskhidze, Nicholas

    2013-10-21

    The objective of this workshop was to address the most urgent open science questions for improved quantification of sea spray aerosol-radiation-climate interactions. Sea spray emission and its influence on global climate remains one of the most uncertain components of the aerosol-radiation-climate problem, but has received less attention than other aerosol processes (e.g. production of terrestrial secondary organic aerosols). Thus, the special emphasis was placed on the production flux of sea spray aerosol particles, their number concentration and chemical composition and properties.

  5. Leaf spray: direct chemical analysis of plant material and living plants by mass spectrometry.

    PubMed

    Liu, Jiangjiang; Wang, He; Cooks, R Graham; Ouyang, Zheng

    2011-10-15

    The chemical constituents of intact plant material, including living plants, are examined by a simple spray method that provides real-time information on sugars, amino acids, fatty acids, lipids, and alkaloids. The experiment is applicable to various plant parts and is demonstrated for a wide variety of species. An electrical potential is applied to the plant and its natural sap, or an applied solvent generates an electrospray that carries endogenous chemicals into an adjacent benchtop or miniature mass spectrometer. The sharp tip needed to create a high electric field can be either natural (e.g., bean sprout) or a small nick can be cut in a leaf, fruit, bark, etc. Stress-induced changes in glucosinolates can be followed on the minute time scale in several plants, including potted vegetables. Differences in spatial distributions and the possibility of studying plant metabolism are demonstrated. © 2011 American Chemical Society

  6. Study of Fundamental Chemical Processes in Explosive Decomposition by Laser-Powered Homogeneous Pyrolysis.

    DTIC Science & Technology

    1981-11-12

    nitrotoluenes actually represent surface- catalyzed reactions . Preliminary qualitative results for pyrolysis of ortho-nitrotoluene in the absence of hot...quantitative validity. LPHP studies of azoisopropane decomposition chosen as a radical-forming test reaction , show the accepted literature parameters to...systematic errors or by rate control exerted by secondary reactions . (2) Support from these VLPP studies for the conclusion that some previous kinetic

  7. Relationships between Chemical Characteristics and Phytotoxicity of Biochar from Poultry Litter Pyrolysis.

    PubMed

    Rombolà, Alessandro G; Marisi, Giovanni; Torri, Cristian; Fabbri, Daniele; Buscaroli, Alessandro; Ghidotti, Michele; Hornung, Andreas

    2015-08-05

    Three biochars were prepared by intermediate pyrolysis from poultry litter at different temperatures (400, 500, and 600 °C with decreasing residence times) and compared with biochars from corn stalk prepared under the same pyrolysis conditions. The phytotoxicity of these biochars was estimated by means of seed germination tests on cress (Lepidium sativum L.) conducted in water suspensions (at 2, 5, and 40 g/L) and on biochars wetted according to their water-holding capacity. Whereas the seeds germinated after 72 h in water suspensions with corn stalk biochar were similar to the control (water only), significant inhibition was observed with poultry litter biochars. In comparison to corn stalk, poultry litter generated biochars with higher contents of ash, ammonium, nitrogen, and volatile fatty acids (VFAs) and a similar concentration of polycyclic aromatic hydrocarbons (PAHs). Results from analytical pyrolysis (Py-GC-MS) indicated that nitrogen-containing organic compounds (NCCs) and aliphatic components were distinctive constituents of the thermally labile fraction of poultry litter biochar. The inhibition of germination due to poultry litter biochar produced at 400 °C (PL400) was suppressed after solvent extraction or treatment with active sludge. A novel method based on solid-phase microextraction (SPME) enabled the identification of mobile organic compounds in PL400 capable of being released in air and water, including VFAs and NCCs. The higher phytotoxicity of poultry litter than corn biochars was tentatively attributed to hydrophilic biodegradable substances derived from lipids or proteins removable by water leaching or microbial treatments.

  8. Chemical pleurodesis using mistletoe extracts via spray catheter during medical thoracoscopy for management of malignant pleural effusion.

    PubMed

    Eom, Jung Seop; Kim, Tae Hwa; Lee, Geewon; Ahn, Hyo Yeong; Mok, Jeong Ha; Lee, Min Ki

    2017-05-01

    We present three cases of successful chemical pleurodesis with a liquid solution of mistletoe extract using a spray catheter during medical thoracoscopy. The medical thoracoscopy was performed in all presented cases to remove pleural effusion and conduct chemical pleurodesis to manage symptomatic malignant pleural effusion. A spray catheter was used to instil the mistletoe extract evenly into the pleural cavity, and there were no pleurodesis-related complications. Respiratory symptoms caused by pleural effusion improved after pleurodesis, and successful pleurodesis was maintained for more than 3 months after medical thoracoscopy in all three patients.

  9. Mechanism of Microwave-Assisted Pyrolysis of Glucose to Furfural Revealed by Isotopic Tracer and Quantum Chemical Calculations.

    PubMed

    Bao, Liwei; Shi, Lei; Luo, Hu; Kong, Lingzhao; Li, Shenggang; Wei, Wei; Sun, Yuhan

    2017-08-10

    Glucose labeled with (13) C or (18) O was used to investigate the mechanism of its conversion into furfural by microwaveassisted pyrolysis. The isotopic content and location in furfural were determined from GC-MS and (13) C NMR spectroscopic measurements and data analysis. The results suggest that the carbon skeleton in furfural is mainly derived from C1 to C5 of glucose, whereas the C of the aldehyde group and the O of the furan ring in furfural primarily originate from C1 and O5 of glucose, respectively. For the first time, the source of O in the furan ring of furfural was elucidated directly by experiment, providing results that are consistent with predictions from recent quantum chemical calculations. Moreover, further theoretical calculations indicate substantially lower energy barriers than previous predictions by considering the potential catalytic effect of formic acid, which is one of the pyrolysis products. The catalytic role of formic acid is further confirmed by experimental evidence. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Quantum chemical investigation of the primary thermal pyrolysis reactions of the sodium carboxylate group in a brown coal model.

    PubMed

    Li, Jian; Zhang, Baisheng; Zhang, Zhiqiang; Yan, Kefeng; Kang, Lixun

    2014-12-01

    The primary pyrolysis mechanisms of the sodium carboxylate group in sodium benzoate-used as a model compound of brown coal-were studied by performing quantum chemical computations using B3LYP and the CBS method. Various possible reaction pathways involving reactions such as unimolecular and bimolecular decarboxylation and decarbonylation, crosslinking, and radical attack in the brown coal matrix were explored. Without the participation of reactive radicals, unimolecular decarboxylation to release CO2 was calculated to be the most energetically favorable primary reaction pathway at the B3LYP/6-311+G (d, p) level of theory, and was also found to be more energetically favorable than decarboxylation of an carboxylic acid group. When CBS-QBS results were included, crosslinking between the sodium carboxylate group and the carboxylic acid and the decarboxylation of the sodium carboxylate group (catalyzed by the phenolic hydroxyl group) were found to be possible; this pathway competes with unimolecular decarboxylation of the sodium carboxylate group. Provided that H and CH3 radicals are present in the brown coal matrix and can access the sodium carboxylate group, accelerated pyrolysis of the sodium carboxylate group becomes feasible, leading to the release of an Na atom or an NaCO2 radical at the B3LYP/6-311+G (d, p) or CBS-QB3 level of theory, respectively.

  11. Pyrolysis of the tetra pak

    SciTech Connect

    Korkmaz, Ahmet; Yanik, Jale Brebu, Mihai; Vasile, Cornelia

    2009-11-15

    This study deals with pyrolysis of tetra pak which is widely used as an aseptic beverage packaging material. Pyrolysis experiments were carried out under inert atmosphere in a batch reactor at different temperatures and by different pyrolysis modes (one- and two-step). The yields of char, liquid and gas were quantified. Pyrolysis liquids produced were collected as three separate phases; aqueous phase, tar and polyethylene wax. Characterization of wax and the determination of the total amount of phenols in aqueous phase were performed. Chemical compositions of gas and char products relevant to fuel applications were determined. Pure aluminum can be also recovered by pyrolysis.

  12. Pyrolysis of the tetra pak.

    PubMed

    Korkmaz, Ahmet; Yanik, Jale; Brebu, Mihai; Vasile, Cornelia

    2009-11-01

    This study deals with pyrolysis of tetra pak which is widely used as an aseptic beverage packaging material. Pyrolysis experiments were carried out under inert atmosphere in a batch reactor at different temperatures and by different pyrolysis modes (one- and two-step). The yields of char, liquid and gas were quantified. Pyrolysis liquids produced were collected as three separate phases; aqueous phase, tar and polyethylene wax. Characterization of wax and the determination of the total amount of phenols in aqueous phase were performed. Chemical compositions of gas and char products relevant to fuel applications were determined. Pure aluminum can be also recovered by pyrolysis.

  13. Real time monitoring of accelerated chemical reactions by ultrasonication-assisted spray ionization mass spectrometry.

    PubMed

    Lin, Shu-Hsuan; Lo, Ta-Ju; Kuo, Fang-Yin; Chen, Yu-Chie

    2014-01-01

    Ultrasonication has been used to accelerate chemical reactions. It would be ideal if ultrasonication-assisted chemical reactions could be monitored by suitable detection tools such as mass spectrometry in real time. It would be helpful to clarify reaction intermediates/products and to have a better understanding of reaction mechanism. In this work, we developed a system for ultrasonication-assisted spray ionization mass spectrometry (UASI-MS) with an ~1.7 MHz ultrasonic transducer to monitor chemical reactions in real time. We demonstrated that simply depositing a sample solution on the MHz-based ultrasonic transducer, which was placed in front of the orifice of a mass spectrometer, the analyte signals can be readily detected by the mass spectrometer. Singly and multiply charged ions from small and large molecules, respectively, can be observed in the UASI mass spectra. Furthermore, the ultrasonic transducer used in the UASI setup accelerates the chemical reactions while being monitored via UASI-MS. The feasibility of using this approach for real-time acceleration/monitoring of chemical reactions was demonstrated. The reactions of Girard T reagent and hydroxylamine with steroids were used as the model reactions. Upon the deposition of reactant solutions on the ultrasonic transducer, the intermediate/product ions are readily generated and instantaneously monitored using MS within 1 s. Additionally, we also showed the possibility of using this reactive UASI-MS approach to assist the confirmation of trace steroids from complex urine samples by monitoring the generation of the product ions.

  14. Bringing the ocean into the laboratory to probe the chemical complexity of sea spray aerosol

    PubMed Central

    Prather, Kimberly A.; Bertram, Timothy H.; Grassian, Vicki H.; Deane, Grant B.; Stokes, M. Dale; DeMott, Paul J.; Aluwihare, Lihini I.; Palenik, Brian P.; Azam, Farooq; Seinfeld, John H.; Moffet, Ryan C.; Molina, Mario J.; Cappa, Christopher D.; Geiger, Franz M.; Roberts, Gregory C.; Russell, Lynn M.; Ault, Andrew P.; Baltrusaitis, Jonas; Collins, Douglas B.; Corrigan, Craig E.; Cuadra-Rodriguez, Luis A.; Ebben, Carlena J.; Forestieri, Sara D.; Guasco, Timothy L.; Hersey, Scott P.; Kim, Michelle J.; Lambert, William F.; Modini, Robin L.; Mui, Wilton; Pedler, Byron E.; Ruppel, Matthew J.; Ryder, Olivia S.; Schoepp, Nathan G.; Sullivan, Ryan C.; Zhao, Defeng

    2013-01-01

    The production, size, and chemical composition of sea spray aerosol (SSA) particles strongly depend on seawater chemistry, which is controlled by physical, chemical, and biological processes. Despite decades of studies in marine environments, a direct relationship has yet to be established between ocean biology and the physicochemical properties of SSA. The ability to establish such relationships is hindered by the fact that SSA measurements are typically dominated by overwhelming background aerosol concentrations even in remote marine environments. Herein, we describe a newly developed approach for reproducing the chemical complexity of SSA in a laboratory setting, comprising a unique ocean-atmosphere facility equipped with actual breaking waves. A mesocosm experiment was performed in natural seawater, using controlled phytoplankton and heterotrophic bacteria concentrations, which showed SSA size and chemical mixing state are acutely sensitive to the aerosol production mechanism, as well as to the type of biological species present. The largest reduction in the hygroscopicity of SSA occurred as heterotrophic bacteria concentrations increased, whereas phytoplankton and chlorophyll-a concentrations decreased, directly corresponding to a change in mixing state in the smallest (60–180 nm) size range. Using this newly developed approach to generate realistic SSA, systematic studies can now be performed to advance our fundamental understanding of the impact of ocean biology on SSA chemical mixing state, heterogeneous reactivity, and the resulting climate-relevant properties. PMID:23620519

  15. Chemical oxygen-iodine laser with a centrifugal spray generator of singlet oxygen

    NASA Astrophysics Data System (ADS)

    Špalek, Otomar; Jirásek, Vít; Čenský, Miroslav; Kodymová, Jarmila

    2010-09-01

    A chemical oxygen-iodine laser driven by the centrifugal spray generator of singlet oxygen was developed and experimentally studied. Modeling and experimental studies showed that the designed generator can produce singlet oxygen, O2(1Δg), with a high efficiency (chlorine utilization 0.68 - 0.87 and O2(1Δg) yield 0.35 - 0.7) even at very high generator pressures (25 - 70 kPa), which cannot be attained by other O2(1Δg) generators. This high-pressure operation should be beneficial for a pressure recovery system of the laser. Another specific feature of the generator is a very high BHP utilization (0.24-0.6). The developed separator can effectively remove even small droplets (> 1 μm) from gas at the generator exit. Preliminary experiments on the COIL driven the centrifugal spray generator provided the small signal gain up to 0.5 % cm-1.

  16. Effect of phytoplankton biomass in seawater on chemical properties of sea spray aerosols.

    PubMed

    Park, Jiyeon; Kim, Dohyung; Lee, Kwangyul; Han, Seunghee; Kim, Hyunji; Williams, Leah R; Joo, Hung Soo; Park, Kihong

    2016-09-15

    This study is to investigate the effect of biological seawater properties on sea spray aerosols (SSA). Concentrations of chlorophyll-a and bacteria were measured at coastal site in Korea in fall and summer seasons. Also, aerosol mass spectrometer (AMS) was used to determine chemical constituents (organics, sulfate, nitrate, ammonium, and chloride) of non-refractory submicrometer aerosols sprayed from seawaters using a bubble bursting system. The average concentration of chlorophyll-a in seawater in fall was 1.75±0.78μg/l, whereas it significantly increased to 5.11±2.16μg/l in summer. It was found that the fraction of organics in the submicrometer SSA was higher in summer (68%) than fall (49%), and that the organic fraction in the SSA increased as the concentration of chlorophyll-a increased in seawater, suggesting that the high phytoplankton biomass in seawater could lead to the enhancement of organic species in the SSA. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Chemical composition of Titan's aerosols analogues characterized with a systematic pyrolysis-gas chromatography-mass spectrometry characterization

    NASA Astrophysics Data System (ADS)

    Szopa, Cyril; Raulin, Francois; Coll, Patrice; Cabane, Michel; GCMS Team

    2014-05-01

    The in situ chemical characterization of Titan's atmosphere was achieved in 2005 with two instruments present onboard the Huygens atmospheric probe : the Aerosol Collector and Pyrolyzer (ACP) devoted to collect and pyrolyse Titan's aerosols ; the Gas Chromatograph-Mass Spectrometer (GCMS) experiment devoted to analyze gases collected in the atmosphere or coming from the aerosols pyrolysis. The GCMS was developed by Hasso Niemann in the filiation of the quadrupole mass spectrometers he built for several former space missions. The main objectives were to : determine the concentration profile of the most abundant chemical species; seek for minor atmospheric organic species not detected with remote observations ; give a first view of the organic aerosols structure; characterize the condensed volatiles present at the surface (e.g. lakes) in case of survival of the probe to the landing impact. Taking into account for the potential complexity of the gaseous samples to be analyzed, it was decided to couple to the MS analyzer a gas chromatograph capable to separate volatile species from light inorganic molecules and noble gases, to organic compounds including aromatics. This was the first GCMS analyzer that worked in an extraterrestrial environment since the Viking missions on Mars. Even if the GCMS coupling mode did not provide any result of interest, it has been demonstrated to be functional during the Huygens descent. But, the direct MS analysis of the atmosphere, and the pyrolysis-MS analysis of aerosols allowed to make great discoveries which are still of primary importance to describe the Titan's lower atmosphere composition. This contribution aims at presenting this instrument that worked in the Titan's atmosphere, and summarizing the most important discoveries it allowed.

  18. Chemical and ecotoxicological characterization of solid residues produced during the co-pyrolysis of plastics and pine biomass.

    PubMed

    Bernardo, Maria S; Lapa, N; Barbosa, R; Gonçalves, M; Mendes, B; Pinto, F; Gulyurtlu, I

    2009-07-15

    A mixture of 70% (w/w) pine biomass and 30% (w/w) plastics (mixture of polypropylene, polyethylene, and polystyrene) was subjected to pyrolysis at 400 degrees C, for 15 min, with an initial pressure of 40 MPa. Part of the solid residue produced was subjected to extraction with dichloromethane (DCM). The extracted residue (residue A) and raw residue (residue B) were analyzed by weight loss combustion and submitted to the leaching test ISO/TS 21268-2 using two different leachants: DCM (0.2%, v/v) and calcium chloride (0.001 mol/L). The concentrations of the heavy metals Cd, Cr, Ni, Zn, Pb and Cu were determined in the eluates and in the two residues. The eluates were further characterized by determining their pH and the concentrations of benzene, toluene, ethylbenzene and xylenes (BTEX). The presence of other organic contaminants in the eluates was qualitatively evaluated by gas chromatography, coupled with mass spectrometry. An ecotoxicological characterization was also performed by using the bio-indicator Vibrio fischeri. The chemical and ecotoxicological results were analyzed according to the French proposal of Criteria on the Evaluation Methods of Waste Ecotoxicity (CEMWE). Residue A was not considered to be ecotoxic by the ecotoxicological criterion (EC(50) (30 min) >or=10%), but it was considered to be ecotoxic by the chemical criterion (Ni>or=0.5mg/L). Residue B was considered to be ecotoxic by the ecotoxicological criterion: EC(50) (30 min)pyrolysis residue with DCM was an efficient method for removing lighter organic contaminants.

  19. Fabrication method for photovoltaic materials by chemical atomisation spray. Final report

    SciTech Connect

    Savelli, M.; LaHaye, J.; Vadel, J.

    1982-09-01

    Acetonitrile has been shown to be a suitable carrier solvent for the preparation of thin layers of cuprous sulphide by chemical atomisation. A reactive spraying apparatus for monodispersed mist has been developed. It is claimed to be indispensible for establishing a firm relation between the characteristics of the mist and those of the films obtained. The formation of thin layers of cadmium sulphide and stannic oxide on various supports has been studied and the quality of the layers, their adhesion to the support, and the influence of the nature and temperature of the support on the reactions have been investigated. Three laboratories have participated in the evaluation of the physical characteristics of the thin layers.

  20. Direct Analysis of Aerosolized Chemical Warfare Simulants Captured on a Modified Glass-Based Substrate by "Paper-Spray" Ionization.

    PubMed

    Dhummakupt, Elizabeth S; Mach, Phillip M; Carmany, Daniel; Demond, Paul S; Moran, Theodore S; Connell, Theresa; Wylie, Harold S; Manicke, Nicholas E; Nilles, J Michael; Glaros, Trevor

    2017-09-25

    Paper spray ionization mass spectrometry offers a rapid alternative platform requiring no sample preparation. Aerosolized chemical warfare agent (CWA) simulants trimethyl phosphate, dimethyl methylphosphonate, and diisopropyl methylphosphonate were captured by passing air through a glass fiber filter disk within a disposable paper spray cartridge. CWA simulants were aerosolized at varying concentrations using an in-house built aerosol chamber. A custom 3D-printed holder was designed and built to facilitate the aerosol capture onto the paper spray cartridges. The air flow through each of the collection devices was maintained equally to ensure the same volume of air sampled across methods. Each approach yielded linear calibration curves with R(2) values between 0.98-0.99 for each compound and similar limits of detection in terms of disbursed aerosol concentration. While the glass fiber filter disk has a higher capture efficiency (≈40%), the paper spray method produces analogous results even with a lower capture efficiency (≈1%). Improvements were made to include glass fiber filters as the substrate within the paper spray cartridge consumable. Glass fiber filters were then treated with ammonium sulfate to decrease chemical interaction with the simulants. This allowed for improved direct aerosol capture efficiency (>40%). Ultimately, the limits of detection were reduced to levels comparable to current worker population limits of 1 × 10(-6) mg/m(3).

  1. Learning Numeracy on the Job: A Case Study of Chemical Handling and Spraying. An Adult Literacy National Project Report

    ERIC Educational Resources Information Center

    FitzSimons, Gail; Mlcek, Susan; Hull, Oksana; Wright, Claire

    2005-01-01

    Ensuring that people have the appropriate level of numeracy skills is particularly important in jobs which involve a risk to public safety and the environment. This research investigates the job-related numeracy requirements in the chemical spraying and handling operations of the horticulture, local government, outdoor recreation and warehousing…

  2. Chemical Phase and Valence Studies of Plasma Sprayed Coatings: EDXRD and X-ray Absorption Spectroscopy (XAS) Results

    DTIC Science & Technology

    2010-06-01

    Versatile XAS micro-(NSLS)/nano(NSLS-II)- probe: local mapping of structure chemistry Rare Earth (RE) 4f -localized atomic, core states** Ce Problem and Ce-L3...powder • Ce3+ n-PS coating Ce4+O2 Ce 3+ !!!!!! PS Plasma Spray Chemical reduction of Ce Average Ce-O distance estimate Rare Earth continuum...local ligand coordination - structure EDXRD: plasma sprayed alumina-titania coatings (on Ti-6-4) • nATCZ → nano composite alumina-titania coating

  3. Controlled catalytic and thermal sequential pyrolysis and hydrolysis of phenolic resin containing waste streams to sequentially recover monomers and chemicals

    DOEpatents

    Chum, H.L.; Evans, R.J.

    1992-08-04

    A process is described for using fast pyrolysis in a carrier gas to convert a waste phenolic resin containing feedstreams in a manner such that pyrolysis of said resins and a given high value monomeric constituent occurs prior to pyrolyses of the resins in other monomeric components therein comprising: selecting a first temperature program range to cause pyrolysis of said resin and a given high value monomeric constituent prior to a temperature range that causes pyrolysis of other monomeric components; selecting, if desired, a catalyst and a support and treating said feedstreams with said catalyst to effect acid or basic catalyzed reaction pathways to maximize yield or enhance separation of said high value monomeric constituent in said first temperature program range to utilize reactive gases such as oxygen and steam in the pyrolysis process to drive the production of specific products; differentially heating said feedstreams at a heat rate within the first temperature program range to provide differential pyrolysis for selective recovery of optimum quantity of said high value monomeric constituent prior to pyrolysis of other monomeric components therein; separating said high value monomeric constituent; selecting a second higher temperature program range to cause pyrolysis of a different high value monomeric constituent of said phenolic resins waste and differentially heating said feedstreams at said higher temperature program range to cause pyrolysis of said different high value monomeric constituent; and separating said different high value monomeric constituent. 11 figs.

  4. Controlled catalytic and thermal sequential pyrolysis and hydrolysis of phenolic resin containing waste streams to sequentially recover monomers and chemicals

    DOEpatents

    Chum, Helena L.; Evans, Robert J.

    1992-01-01

    A process of using fast pyrolysis in a carrier gas to convert a waste phenolic resin containing feedstreams in a manner such that pyrolysis of said resins and a given high value monomeric constituent occurs prior to pyrolyses of the resins in other monomeric components therein comprising: selecting a first temperature program range to cause pyrolysis of said resin and a given high value monomeric constituent prior to a temperature range that causes pyrolysis of other monomeric components; selecting, if desired, a catalyst and a support and treating said feedstreams with said catalyst to effect acid or basic catalyzed reaction pathways to maximize yield or enhance separation of said high value monomeric constituent in said first temperature program range to utilize reactive gases such as oxygen and steam in the pyrolysis process to drive the production of specific products; differentially heating said feedstreams at a heat rate within the first temperature program range to provide differential pyrolysis for selective recovery of optimum quantity of said high value monomeric constituent prior to pyrolysis of other monomeric components therein; separating said high value monomeric constituent; selecting a second higher temperature program range to cause pyrolysis of a different high value monomeric constituent of said phenolic resins waste and differentially heating said feedstreams at said higher temperature program range to cause pyrolysis of said different high value monomeric constituent; and separating said different high value monomeric constituent.

  5. Characterization and pyrolysis of Chlorella vulgaris and Arthrospira platensis: potential of bio-oil and chemical production by Py-GC/MS analysis.

    PubMed

    Almeida, Hanna N; Calixto, Guilherme Q; Chagas, Bruna M E; Melo, Dulce M A; Resende, Fabio M; Melo, Marcus A F; Braga, Renata Martins

    2017-06-01

    Biofuels have been seen as potential sources to meet future energy demand as a renewable and sustainable energy source. Despite the fact that the production technology of first-generation biofuels is consolidated, these biofuels are produced from foods crops such as grains, sugar cane, and vegetable oils competing with food for crop use and agricultural land. In recent years, it was found that microalgae have the potential to provide a viable alternative to fossil fuels as source of biofuels without compromising food supplies or arable land. On this scenario, this paper aims to demonstrate the energetic potential to produce bio-oil and chemicals from microalgae Chlorella vulgaris and Arthrospira platensis. The potential of these biomasses was evaluated in terms of physical-chemical characterization, thermogravimetric analysis, and analytical pyrolysis interfaced with gas chromatograph (Py-GC/MS). The results show that C. vulgaris and A. platensis are biomasses with a high heating value (24.60 and 22.43 MJ/kg) and low ash content, showing a high percentage of volatile matter (72.49 and 79.42%). These characteristics confirm their energetic potential for conversion process through pyrolysis, whereby some important aromatic compounds such as toluene, styrene, and phenol were identified as pyrolysis products, which could turn these microalgae a potential for biofuels and bioproduct production through the pyrolysis.

  6. Influence of zinc chloride addition on the chemical structure of bio-oil obtained during co-pyrolysis of wood/synthetic polymer blends.

    PubMed

    Rutkowski, Piotr

    2009-12-01

    The chemical structure of liquid products of the pinewood sawdust (W) co-pyrolysis with polystyrene (PS) and polypropylene (PP) with and without the zinc chloride as an additive was investigated. The pyrolysis process was carried out at 450 degrees C with the heating rate of 5 degrees C/min. The yield of liquid products of pyrolysis was in the range of 37-91 wt% and their form was liquid or semi-solid depending on the composition of the wood/polymer blend. The zinc chloride addition to wood/polymer blends has influenced the range of samples decomposition as well as the chemical structure of resulted bio-oils. All bio-oils from wood/polypropylene blends were two-phase (liquid and solid). Contrarily, all bio-oils obtained from biopolymer/polypropylene blends with zinc chloride added were yellow liquids. All analyses proved that the structure and the quality of bio-oil strongly depend on both the composition of the blend and the presence of ZnCl(2) as an additive. The FT-IR analyses of oils showed that oxygen-containing groups and hydrocarbons content highly depend on the composition of biomass/synthetic polymer mixture. The fractionation of bio-oils by column chromatography with four different solvents was followed by GC-MS analysis. Results confirmed the significant removal and/or transformation of oxygen-containing organic compounds due to the zinc chloride presence during pyrolysis process.

  7. Quantum-dot-sensitized solar cells fabricated by the combined process of the direct attachment of colloidal CdSe quantum dots having a ZnS glue layer and spray pyrolysis deposition.

    PubMed

    Im, Sang Hyuk; Lee, Yong Hui; Seok, Sang Il; Kim, Sung Woo; Kim, Sang-Wook

    2010-12-07

    We were able to attach CdSe quantum dots (QDs) having a ZnS inorganic glue layer directly to a mesoporous TiO(2) (mp-TiO(2)) surface by spray coating and thermal annealing. Quantum-dot-sensitized solar cells based on CdSe QDs having ZnS as the inorganic glue layer could easily transport generated charge carriers because of the intimate bonding between CdSe and mp-TiO(2). The application of spray pyrolysis deposition (SPD) to obtain additional CdSe layers improved the performance characteristics to V(oc) = 0.45 V, J(sc) = 10.7 mA/cm(2), fill factor = 35.8%, and power conversion efficiency = 1.7%. Furthermore, ZnS post-treatment improved the device performance to V(oc) = 0.57 V, J(sc) = 11.2 mA/cm(2), fill factor = 35.4%, and power conversion efficiency = 2.2%.

  8. New candidate for biofuel feedstock beyond terrestrial biomass for thermo-chemical process (pyrolysis/gasification) enhanced by carbon dioxide (CO2).

    PubMed

    Kwon, Eilhann E; Jeon, Young Jae; Yi, Haakrho

    2012-11-01

    The enhanced thermo-chemical process (i.e., pyrolysis/gasification) of various macroalgae using carbon dioxide (CO(2)) as a reaction medium was mainly investigated. The enhanced thermo-chemical process was achieved by expediting the thermal cracking of volatile chemical species derived from the thermal degradation of the macroalgae. This process enables the modification of the end products from the thermo-chemical process and significant reduction of the amount of condensable hydrocarbons (i.e., tar, ∼50%), thereby directly increasing the efficiency of the gasification process.

  9. Influence of pyrolysis temperature on lead immobilization by chemically modified coconut fiber-derived biochars in aqueous environments.

    PubMed

    Wu, Weidong; Li, Jianhong; Niazi, Nabeel Khan; Müller, Karin; Chu, Yingchao; Zhang, Lingling; Yuan, Guodong; Lu, Kouping; Song, Zhaoliang; Wang, Hailong

    2016-11-01

    Biochar has received widespread attention as an eco-friendly and efficient material for immobilization of toxic heavy metals in aqueous environments. In the present study, three types of coconut fiber-derived biochars were obtained by pyrolyzing at three temperatures, i.e., 300, 500, and 700 °C. In addition, nine types of biochars were prepared by chemical modification with ammonia, hydrogen peroxide, and nitric acid, respectively, which were used to investigate changes in physico-chemical properties by inter alia, Fourier transformation infrared spectrophotometry (FTIR), scanning electron microscope (SEM), and BET specific surface area analysis. Batch sorption experiments were carried out to determine the sorption capacity of the biochars for lead (Pb) in aqueous solutions. Results showed that the cation exchange capacity of biochar pyrolyzed at 300 °C and modified with nitric acid increased threefold compared to the control. Loosely corrugated carbon surface and uneven carbon surface of the biochar pyrolyzed at 300 °C were produced during ammonia and nitric acid modifications. Removal rate of Pb by the coconut biochar pyrolyzed at 300 °C and modified with ammonia was increased from 71.8 to 99.6 % compared to the untreated biochar in aqueous solutions containing 100 mg L(-1) Pb. However, chemical modification did not enhance adsorption of Pb of the biochars pyrolyzed at higher temperatures (e.g., 500 or 700 °C), indicating that resistance of biochars to chemical treatment increased with pyrolysis temperature.

  10. Assessing the efficacy of spray-delivered 'eco-friendly' chemicals for the control and eradication of marine fouling pests.

    PubMed

    Piola, Richard F; Dunmore, Robyn A; Forrest, Barrie M

    2010-01-01

    Despite its frequent use in terrestrial and freshwater systems, there is a lack of published experimental research examining the effectiveness of spray-delivered chemicals for the management of non-indigenous and/or unwanted pests in marine habitats. This study tested the efficacy of spraying acetic acid, hydrated lime and sodium hypochlorite for the control of marine fouling assemblages. The chemicals are considered relatively 'eco-friendly' due to their low toxicity and reduced environmental persistence compared to synthetic biocides, and they were effective in controlling a wide range of organisms. Pilot trials highlighted acetic acid as the most effective chemical at removing fouling cover, therefore it was selected for more comprehensive full-scale trials. A single spray of 5% acetic acid with an exposure time of 1 min effectively removed up to 55% of the invertebrate species present and 65% of the cover on fouled experimental plates, while one application of 10% acetic acid over 30 min removed up to 78% of species present and 95% of cover. Single-spray treatments of 5% acetic acid reduced cover of the tunicate pest species Didemnum vexillum by up to 100% depending on the exposure duration, while repeat-spraying ensured that even short exposure times (1 min) achieved approximately 99% mortality. Both 5 and 10% acetic acid solutions appeared equally effective at removing the majority of algal species. This technique could be used for controlling the introduction of unwanted species or preventing the spread of pests, and is applicable to use on a variety of natural and artificial substrata, or for the treatment of structures that can be removed from the water.

  11. On methane pyrolysis special applications

    NASA Astrophysics Data System (ADS)

    Toncu, D. C.; Toncu, G.; Soleimani, S.

    2015-11-01

    Methane pyrolysis represents one of the most important processes in industrial use, with applications rising from the chemical and petrochemical industry, combustion, materials and protective coatings. Despite the intense research, experimental data lack kinetic aspects, and the thermodynamics involved often leads to inaccurate results when applied to various systems. Carrying out a comparative analysis of several available data on methane pyrolysis, the paper aims to study the phenomenon of methane pyrolysis under different environments (combustion and plasma), concluding on the most possible reaction pathways involved in many of its applications. Computer simulation using different database underlines the conclusion, helping to the understanding of methane pyrolysis importance in future technologies.

  12. Dissolved phosphorus speciation of flash carbonization, slow pyrolysis, and fast pyrolysis biochars

    USDA-ARS?s Scientific Manuscript database

    Pyrolysis of waste biomass is a promising technology to produce sterile and renewable organic phosphorus fertilizers. Systematic studies are necessary to understand how different pyrolysis platforms influence the chemical speciation of dissolved (bioavailable) phosphorus. This study employed solut...

  13. Production of p-xylene from biomass by catalytic fast pyrolysis using ZSM-5 catalysts with reduced pore openings.

    PubMed

    Cheng, Yu-Ting; Wang, Zhuopeng; Gilbert, Christopher J; Fan, Wei; Huber, George W

    2012-10-29

    Pores for thought: Chemical liquid deposition of silica onto ZSM-5 catalysts led to smaller pore openings that resulted in >90% selectivity for p-xylene over the other xylenes in the catalytic fast pyrolysis of furan and 2-methylfuran (see scheme). The p-xylene selectivity increased from 51% with gallium spray-dried ZSM-5 to 72% with a pore-mouth-modified catalyst in the pyrolysis of pine wood. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Atmospheric Pressure Spray Chemical Vapor Deposited CuInS2 Thin Films for Photovoltaic Applications

    NASA Technical Reports Server (NTRS)

    Harris, J. D.; Raffaelle, R. P.; Banger, K. K.; Smith, M. A.; Scheiman, D. A.; Hepp, A. F.

    2002-01-01

    Solar cells have been prepared using atmospheric pressure spray chemical vapor deposited CuInS2 absorbers. The CuInS2 films were deposited at 390 C using the single source precursor (PPh3)2CuIn(SEt)4 in an argon atmosphere. The absorber ranges in thickness from 0.75 - 1.0 micrometers, and exhibits a crystallographic gradient, with the leading edge having a (220) preferred orientation and the trailing edge having a (112) orientation. Schottky diodes prepared by thermal evaporation of aluminum contacts on to the CuInS2 yielded diodes for films that were annealed at 600 C. Solar cells were prepared using annealed films and had the (top down) composition of Al/ZnO/CdS/CuInS2/Mo/Glass. The Jsc, Voc, FF and (eta) were 6.46 mA per square centimeter, 307 mV, 24% and 0.35%, respectively for the best small area cells under simulated AM0 illumination.

  15. Coupled process of plastics pyrolysis and chemical vapor deposition for controllable synthesis of vertically aligned carbon nanotube arrays

    NASA Astrophysics Data System (ADS)

    Yang, Zhou; Zhang, Qiang; Luo, Guohua; Huang, Jia-Qi; Zhao, Meng-Qiang; Wei, Fei

    2010-08-01

    Efficient conversion of waste plastics into advanced materials is of conspicuous environmental, social and economic benefits. A coupled process of plastic pyrolysis and chemical vapor deposition for vertically aligned carbon nanotube (CNT) array growth was proposed. Various kinds of plastics, such as polypropylene, polyethylene, and polyvinyl chloride, were used as carbon sources for the controllable growth of CNT arrays. The relationship between the length of CNT arrays and the growth time was investigated. It was found that the length of aligned CNTs increased with prolonged growth time. CNT arrays with a length of 500 μm were obtained for a 40-min growth and the average growth rate was estimated to be 12 μm/min. The diameter of CNTs in the arrays can be modulated by controlling the growth temperature and the feeding rate of ferrocene. In addition, substrates with larger specific surface area such as ceramic spheres, quartz fibers, and quartz particles, were adopted to support the growth of CNT arrays. Those results provide strong evidence for the feasibility of conversion from waste plastics into CNT arrays via this reported sustainable materials processing.

  16. Synthesis Characterization and Decomposition Studies of tris[N-N-dibenzyidithocarbaso)Indium (III) Chemical Spray Deposition of Polycrystalline CuInS2 on Copper Films

    NASA Technical Reports Server (NTRS)

    Hehemann, David G.; Lau, J. Eva; Harris, Jerry D.; Hoops, Michael D.; Duffy, Norman V.

    2005-01-01

    This paper presents the results of the synthesis characterization and decomposition studies of tris[N-N-dibenzyidithocarbaso)Indium (III) with chemical spray deposition of polycrystalline CuInS2 on Copper Films.

  17. Synthesis Characterization and Decomposition Studies of tris[N-N-dibenzyidithocarbaso)Indium (III) Chemical Spray Deposition of Polycrystalline CuInS2 on Copper Films

    NASA Technical Reports Server (NTRS)

    Hehemann, David G.; Lau, J. Eva; Harris, Jerry D.; Hoops, Michael D.; Duffy, Norman V.

    2005-01-01

    This paper presents the results of the synthesis characterization and decomposition studies of tris[N-N-dibenzyidithocarbaso)Indium (III) with chemical spray deposition of polycrystalline CuInS2 on Copper Films.

  18. Characterization of the Chemical Composition of TITAN'S Aerosols Analogues with a Systematic Pyrolysis-GCMS Analysis Approach

    NASA Astrophysics Data System (ADS)

    Szopa, C.; Morisson, M.; Carrasco, N.; Buch, A.; Gautier, T.

    2014-12-01

    Pyrolysis coupled to gas chromatography-mass spectrometry is used for long to characterize the chemical composition and structure of analogues of Titan's aerosols (tholins). However, a review of the characterizations of tholins done for 30 years with this technique show that the nature of the tholins were quite different in the different studies, and the analytical conditions used for Pyr-GCMS analysis were generally very limited. The differences observed in the results obtained in these different studies are therefore difficult to attribute either to the process used to produce the tholins, or to the analytical conditions used. These are the reasons we performed a systematic study on tholins produced uniquely with the PAMPRE laboratory experiment based on a RF cold plasma, to determine the composition and structure of these analogues of Titan's aerosols, and to estimate the difference of properties induced by a variation of the content of CH4 in the initial gaseous mixture. To take the whole benefit of the pyr-GCMS technique, we performed analyses of tholins by studying the influence of all the analytical parameters. Among the main parameters, we studied : the influence of the temperature of pyrolysis on the nature of the gaseous compounds released by the solid tholins; the program of temperature used to heat the GC column in order to find a tradeoff for the analysis of both the lightest and heaviest compounds released by the sample; the separation of the same pyrolysates with two different columns. Moreover, the identification of numerous isomers was confirmed using analytical standards. WIth this study, we managed to strictly characterize a wide range of pyrolyzates for the three tholins sample studied. Most of these species are nitrogen bearing organics of various natures. More than the detection of pyrolyzates which have never been reported in previous studies, we showed that even if numerous pyrolysates were common between the three types of tholins studied

  19. The effect of clay catalyst on the chemical composition of bio-oil obtained by co-pyrolysis of cellulose and polyethylene

    SciTech Connect

    Solak, Agnieszka; Rutkowski, Piotr

    2014-02-15

    Highlights: • Non-catalytic and catalytic fast pyrolysis of cellulose/polyethylene blend was carried out in a laboratory scale reactor. • Optimization of process temperature was done. • Optimization of clay catalyst type and amount for co-pyrolysis of cellulose and polyethylene was done. • The product yields and the chemical composition of bio-oil was investigated. - Abstract: Cellulose/polyethylene (CPE) mixture 3:1, w/w with and without three clay catalysts (K10 – montmorillonite K10, KSF – montmorillonite KSF, B – Bentonite) addition were subjected to pyrolysis at temperatures 400, 450 and 500 °C with heating rate of 100 °C/s to produce bio-oil with high yield. The pyrolytic oil yield was in the range of 41.3–79.5 wt% depending on the temperature, the type and the amount of catalyst. The non-catalytic fast pyrolysis at 500 °C gives the highest yield of bio-oil (79.5 wt%). The higher temperature of catalytic pyrolysis of cellulose/polyethylene mixture the higher yield of bio-oil is. Contrarily, increasing amount of montmorillonite results in significant, almost linear decrease in bio-oil yield followed by a significant increase of gas yield. The addition of clay catalysts to CPE mixture has a various influence on the distribution of bio-oil components. The addition of montmorillonite K10 to cellulose/polyethylene mixture promotes the deepest conversion of polyethylene and cellulose. Additionally, more saturated than unsaturated hydrocarbons are present in resultant bio-oils. The proportion of liquid hydrocarbons is the highest when a montmorillonite K10 is acting as a catalyst.

  20. Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods

    DOE PAGES

    Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.; ...

    2016-07-05

    Here, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. In this paper, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 °C), 31P NMR for determination ofmore » hydroxyl groups, and a quantitative gas chromatography–mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to -determine metrics for bio-oil quality. Lastly, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.« less

  1. Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods

    SciTech Connect

    Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.; Padmaperuma, Asanga B.; Connatser, Raynella M.; Stankovikj, Filip; Meier, Dietrich; Paasikallio, Ville

    2016-07-05

    Here, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. In this paper, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 °C), 31P NMR for determination of hydroxyl groups, and a quantitative gas chromatography–mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to -determine metrics for bio-oil quality. Lastly, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.

  2. Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods

    SciTech Connect

    Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.; Padmaperuma, Asanga B.; Connatser, Raynella M.; Stankovikj, Filip; Meier, Dietrich; Paasikallio, Ville

    2016-07-05

    Here, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. In this paper, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 °C), 31P NMR for determination of hydroxyl groups, and a quantitative gas chromatography–mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to -determine metrics for bio-oil quality. Lastly, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.

  3. Pyrolysis-Molecular Beam Mass Spectrometry to Characterize Soil Organic Matter Composition in Chemically Isolated Fractions from Differing Land Uses

    SciTech Connect

    Plante, A. F.; Magrini-Bair, K.; Vigil, M.; Paul, E. A.

    2009-01-01

    Today's questions concerning the role of soil organic matter (SOM) in soil fertility, ecosystem functioning and global change can only be addressed through knowledge of the controls on SOM stabilization and their interactions. Pyrolysis molecular beam mass spectrometry (py-MBMS) provides a powerful and rapid means of assessing the biochemical composition of SOM. However, characterization of SOM composition alone is insufficient to predict its dynamic behavior. Chemical fractionation is frequently used to isolate more homogeneous SOM components, but the composition of fractions is frequently unknown. We characterized biochemical SOM composition in two previously studied soils from the USA, under contrasting land uses: cultivated agriculture and native vegetation. Bulk soils, as well as chemically isolated SOM fractions (humic acid, humin and non-acid hydrolysable), were analyzed using py-MBMS. Principal components analysis (PCA) showed distinct differences in the SOM composition of isolated fractions. Py-MBMS spectra and PCA loadings were dominated by low molecular weight fragments associated with peptides and other N-containing compounds. The py-MBMS spectra were similar for native whole-soil samples under different vegetation, while cultivation increased heterogeneity. An approach based on previously published data on marker signals also suggests the importance of peptides in distinguishing samples. While the approach described here represents significant progress in the characterization of changing SOM composition, a truly quantitative analysis will only be achieved using multiple internal standards and by correcting for inorganic interference during py-MBMS analysis. Overall, we have provided proof of principle that py-MBMS can be a powerful tool to understand the controls on SOM dynamics, and further method development is underway.

  4. Low cost sprayed CdTe solar cell research

    NASA Astrophysics Data System (ADS)

    Squillante, M.; Turcotte, R.; Lis, S.; Serreze, H. B.; Entine, G.

    1980-06-01

    Experiments were carried out to optimize the conditions of the chemical reaction and the physical parameters of the spray process in order to produce high quality CdTe thin films. Films containing 95% or more of CdTe were produced by the reaction of (MH4) 2TeO4 with cadmium salts in the presence of a reducing agent. The physical quality of the films improved so that recent ones have been smoother and more uniform. Furthermore, photoconductive effects were observed in many of the films. This progress is partly due to the removal of oxygen by an efficient purge of the spray box and partly due to an increased understanding and control of the spray pyrolysis process.

  5. A comprehensive experimental and detailed chemical kinetic modelling study of 2,5-dimethylfuran pyrolysis and oxidation

    PubMed Central

    Somers, Kieran P.; Simmie, John M.; Gillespie, Fiona; Conroy, Christine; Black, Gráinne; Metcalfe, Wayne K.; Battin-Leclerc, Frédérique; Dirrenberger, Patricia; Herbinet, Olivier; Glaude, Pierre-Alexandre; Dagaut, Philippe; Togbé, Casimir; Yasunaga, Kenji; Fernandes, Ravi X.; Lee, Changyoul; Tripathi, Rupali; Curran, Henry J.

    2013-01-01

    The pyrolytic and oxidative behaviour of the biofuel 2,5-dimethylfuran (25DMF) has been studied in a range of experimental facilities in order to investigate the relatively unexplored combustion chemistry of the title species and to provide combustor relevant experimental data. The pyrolysis of 25DMF has been re-investigated in a shock tube using the single-pulse method for mixtures of 3% 25DMF in argon, at temperatures from 1200–1350 K, pressures from 2–2.5 atm and residence times of approximately 2 ms. Ignition delay times for mixtures of 0.75% 25DMF in argon have been measured at atmospheric pressure, temperatures of 1350–1800 K at equivalence ratios (ϕ) of 0.5, 1.0 and 2.0 along with auto-ignition measurements for stoichiometric fuel in air mixtures of 25DMF at 20 and 80 bar, from 820–1210 K. This is supplemented with an oxidative speciation study of 25DMF in a jet-stirred reactor (JSR) from 770–1220 K, at 10.0 atm, residence times of 0.7 s and at ϕ = 0.5, 1.0 and 2.0. Laminar burning velocities for 25DMF-air mixtures have been measured using the heat-flux method at unburnt gas temperatures of 298 and 358 K, at atmospheric pressure from ϕ = 0.6–1.6. These laminar burning velocity measurements highlight inconsistencies in the current literature data and provide a validation target for kinetic mechanisms. A detailed chemical kinetic mechanism containing 2768 reactions and 545 species has been simultaneously developed to describe the combustion of 25DMF under the experimental conditions described above. Numerical modelling results based on the mechanism can accurately reproduce the majority of experimental data. At high temperatures, a hydrogen atom transfer reaction is found to be the dominant unimolecular decomposition pathway of 25DMF. The reactions of hydrogen atom with the fuel are also found to be important in predicting pyrolysis and ignition delay time experiments. Numerous proposals are made on the mechanism and kinetics of the previously

  6. Gas Chromatography/Atmospheric Pressure Chemical Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry of Pyrolysis Oil from German Brown Coal

    PubMed Central

    Zuber, Jan; Kroll, Marius M.; Rathsack, Philipp; Otto, Matthias

    2016-01-01

    Pyrolysis oil from the slow pyrolysis of German brown coal from Schöningen, obtained at a temperature of 500°C, was separated and analyzed using hyphenation of gas chromatography with an atmospheric pressure chemical ionization source operated in negative ion mode and Fourier transform ion cyclotron resonance mass spectrometry (GC-APCI-FT-ICR-MS). Development of this ultrahigh-resolving analysis method is described, that is, optimization of specific GC and APCI parameters and performed data processing. The advantages of GC-APCI-FT-ICR-MS hyphenation, for example, soft ionization, ultrahigh-resolving detection, and most important isomer separation, were demonstrated for the sample liquid. For instance, it was possible to separate and identify nine different propylphenol, ethylmethylphenol, and trimethylphenol isomers. Furthermore, homologous series of different acids, for example, alkyl and alkylene carboxylic acids, were verified, as well as homologous series of alkyl phenols, alkyl dihydroxy benzenes, and alkoxy alkyl phenols. PMID:27066076

  7. Gas Chromatography/Atmospheric Pressure Chemical Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry of Pyrolysis Oil from German Brown Coal.

    PubMed

    Zuber, Jan; Kroll, Marius M; Rathsack, Philipp; Otto, Matthias

    2016-01-01

    Pyrolysis oil from the slow pyrolysis of German brown coal from Schöningen, obtained at a temperature of 500°C, was separated and analyzed using hyphenation of gas chromatography with an atmospheric pressure chemical ionization source operated in negative ion mode and Fourier transform ion cyclotron resonance mass spectrometry (GC-APCI-FT-ICR-MS). Development of this ultrahigh-resolving analysis method is described, that is, optimization of specific GC and APCI parameters and performed data processing. The advantages of GC-APCI-FT-ICR-MS hyphenation, for example, soft ionization, ultrahigh-resolving detection, and most important isomer separation, were demonstrated for the sample liquid. For instance, it was possible to separate and identify nine different propylphenol, ethylmethylphenol, and trimethylphenol isomers. Furthermore, homologous series of different acids, for example, alkyl and alkylene carboxylic acids, were verified, as well as homologous series of alkyl phenols, alkyl dihydroxy benzenes, and alkoxy alkyl phenols.

  8. Relative toxicity of pyrolysis gases from materials - Effects of chemical composition and test conditions

    NASA Technical Reports Server (NTRS)

    Hilado, C. J.; Cumming, H. J.

    1978-01-01

    Relative toxicity test data on 270 materials are presented, based on test procedures developed at the University of San Francisco. The effects of chemical composition, using data on 13 types of synthetic polymers and eight types of fabrics, are discussed. Selected materials were evaluated using nine test conditions with the USF method, and using methods developed at the FAA Civil Aeromedical Institute, Douglas Aircraft Company and San Jose State University.

  9. Influence of deposition parameters on chemical properties of calcium phosphate coatings prepared by using electrostatic spray deposition.

    PubMed

    Leeuwenburgh, S; Wolke, J; Schoonman, J; Jansen, J A

    2005-08-01

    The electrostatic spray deposition (ESD) technique offers the possibility of depositing calcium phosphate (CaP) coatings onto various substrate materials with defined chemical and morphological properties. The relationship between physical, apparatus-related deposition parameters, and the chemical characteristics of ESD coatings was investigated by means of X-ray diffraction, Fourier transform infrared spectroscopy, and energy dispersive spectroscopy to be able to deposit CaP coatings with tailored chemical properties. The results showed that the chemical characteristics of CaP coatings, deposited with use of the ESD technique, were strongly dependent on the deposition temperature, the nozzle-to-substrate distance, the liquid flow rate, and the geometry of the spraying nozzle. By investigating the influence of the deposition temperature, information could be obtained on the formation mechanism of CaP coatings-and specifically the biologically interesting carbonate apatite phase-using the ESD technique. CaP coatings were not formed merely because of solvent evaporation; a chemical reaction was needed to synthesize the coatings. This reaction involved thermal decomposition of the organic solvent butyl carbitol into carbonate ions via formation of intermediate oxalate ions. The amount of carbonate incorporation, and consequently, the Ca/P ratios of the deposited coatings, was shown 1) to decrease with increasing nozzle-to-substrate distance, 2) to decrease with increasing liquid flow rate, and 3) to decrease by making use of a novel two-component nozzle geometry. (c) 2005 Wiley Periodicals, Inc.

  10. Thickness dependent optical properties of PEMA and (PEMA){sub 0.85}/(ZnO){sub 0.15} nanocomposite films deposited by spray pyrolysis technique on ITO substrate

    SciTech Connect

    Thakur, Anjna Thakur, Priya; Yadav, Kamlesh

    2016-05-06

    In this paper, poly (ethyl methacrylate) (PEMA) and (PEMA){sub 0.85}/(ZnO){sub 0.15} nanocomposite films for 2, 3, 4 and 5 minutes have been deposited by spray pyrolysis technique on indium tin oxide (ITO) coated substrate. The effect of thickness of the film on the morphological and optical properties of PEMA and (PEMA){sub 0.85}/(ZnO){sub 0.15} nanocomposite films are studied. The morphological and optical properties of pure PEMA and (PEMA){sub 0.85}/(ZnO){sub 0.15} nanocomposite films are compared. The field emission scanning electron microscopy (FESEM) shows that as the thickness of film increases, uniformity of films increases. It is found from UV-Visible spectra that the energy band gap decreases with increasing the deposition time and refractive index increases with increasing the thickness of the film. The band gap of the nanocomposites is found less than the pure polymer film and opposite trend is observed for refractive index. The optical absorption of PEMA/ZnO nanocomposite films is higher than pure PEMA film. The thickness of the nanocomposite film plays a significant role in the tunability of the optical properties.

  11. Spray pyrolysis of MgO templates on Hastelloy C276 and 310-austenitic stainless steel substrates for Y Ba2Cu3O7 (YBCO) deposition by pulsed laser deposition

    NASA Astrophysics Data System (ADS)

    Khateeb, Shadi Al; Button, T. W.; Abell, J. S.

    2010-09-01

    MgO thin films were deposited on Hastelloy C276 (HC) and 310 austenitic stainless steel by the spray pyrolysis technique, using magnesium nitrate and magnesium acetate as precursors. Thermogravimetrical analysis of the decomposition of the precursors was used to provide a guideline temperature for the thin film deposition. It was suggested that an amorphous MgO thin film was deposited on both 310-stainless steel and Hastelloy C-276 when using low concentration of the magnesium nitrate precursor. Higher concentrations were needed to obtain (200) oriented MgO films on C276. However, 310-stainless steel was found to not be a suitable substrate for MgO thin film deposition due to surface instability. A (200) oriented MgO thin film was grown on Hastelloy C276 using a magnesium acetate precursor at a much lower concentration compared to the nitrate precursor. The characterization of the thin films was done using scanning electron microscopy, x-ray photoelectron spectroscopy, atomic force microscopy, x-ray diffraction 2θ-scans, rocking curves (ω-scans), and pole figure measurements. MgO was found to have a very weak in-plane texture.

  12. Extremely fine structured cathode for solid oxide fuel cells using Sr-doped LaMnO3 and Y2O3-stabilized ZrO2 nano-composite powder synthesized by spray pyrolysis

    NASA Astrophysics Data System (ADS)

    Shimada, Hiroyuki; Yamaguchi, Toshiaki; Sumi, Hirofumi; Nomura, Katsuhiro; Yamaguchi, Yuki; Fujishiro, Yoshinobu

    2017-02-01

    A solid oxide fuel cell (SOFC) for high power density operation was developed with a microstructure-controlled cathode using a nano-composite powder of Sr-doped LaMnO3 (LSM) and Y2O3-stabilized ZrO2 (YSZ) synthesized by spray pyrolysis. The individual LSM-YSZ nano-composite particles, formed by crystalline and amorphous nano-size LSM and YSZ particles, showed spherical morphology with uniform particle size. The use of this powder for cathode material led to an extremely fine microstructure, in which all the LSM and YSZ grains (approximately 100-200 nm) were highly dispersed and formed their own network structures. This microstructure was due to the two phase electrode structure control using the powder, namely, nano-order level in each particle and micro-order level between particles. An anode-supported SOFC with the LSM-YSZ cathode using humidified H2 as fuel and ambient air as oxidant exhibited high power densities, such as 1.29 W cm-2 under a voltage of 0.75 V and a maximum power density of 2.65 W cm-2 at 800 °C. Also, the SOFC could be stably operated for 250 h with no degradation, even at a high temperature of 800 °C.

  13. Nanoscale carbon materials from hydrocarbons pyrolysis: Structure, chemical behavior, utilisation for non-aqueous supercapacitors

    SciTech Connect

    Savilov, Serguei V.; Strokova, Natalia E.; Ivanov, Anton S.; Arkhipova, Ekaterina A.; Desyatov, Andrey V.; Hui, Xia; Aldoshin, Serguei M.; Lunin, Valery V.

    2015-09-15

    Highlights: • N-doped and regular carbon nanomaterials were obtained by pyrolitic technique. • Dynamic vapor sorption of different solvents reveals smaller S{sub BET} values. • Steric hindrance and specific chemical interactions are the reasons for this. • Nitrogen doping leads to raise of capacitance and coulombic efficiency with non-aqueous N-containing electrolyte. - Abstract: This work systematically studies adsorption properties of carbon nanomaterials that are synthesized through hydrocarbons that is a powerful technique to fabricate different kinds of carbon materials, e.g., nanotubes, nanoshells, onions, including nitrogen substituted. The adsorption properties of the as-synthesized carbons are achieved by low temperature nitrogen adsorption and organic vapors sorption. Heptane, acetonitrile, water, ethanol, benzene and 1-methylimidazole, which are of great importance for development of supercapacitors, are used as substrates. It is discovered that while nitrogen adsorption reveals a high specific surface area, this parameter for most of organic compounds is rather small depending not only on the size of its molecule but also on chemical interactions for a pair adsorbent–adsorbate. The experimental values of heat of adsorption for carbon and N-substituted structures, when Coulomb cross-coupling of nitrogen atoms in adsorbent and adsorbate takes place, confirms this supposition.

  14. Mechanism of waste biomass pyrolysis: Effect of physical and chemical pre-treatments.

    PubMed

    Das, Oisik; Sarmah, Ajit K

    2015-12-15

    To impart usability in waste based biomass through thermo-chemical reactions, several physical and chemical pre-treatments were conducted to gain an insight on their mode of action, effect on the chemistry and the change in thermal degradation profiles. Two different waste biomasses (Douglas fir, a softwood and hybrid poplar, a hardwood) were subjected to four different pre-treatments, namely, hot water pre-treatment, torrefaction, acid (sulphuric acid) and salt (ammonium phosphate) doping. Post pre-treatments, the changes in the biomass structure, chemistry, and thermal makeup were studied through electron microscopy, atomic absorption/ultra violet spectroscopy, ion exchange chromatography, and thermogravimetry. The pre-treatments significantly reduced the amounts of inorganic ash, extractives, metals, and hemicellulose from both the biomass samples. Furthermore, hot water and torrefaction pre-treatment caused mechanical disruption in biomass fibres leading to smaller particle sizes. Torrefaction of Douglas fir wood yielded more solid product than hybrid poplar. Finally, the salt pre-treatment increased the activation energies of the biomass samples (especially Douglas fir) to a great extent. Thus, salt pre-treatment was found to bestow thermal stability in the biomass. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. ENGINEERING BULLETIN: PYROLYSIS TREATMENT

    EPA Science Inventory

    Pyrolysis is formally defined as chemical decomposition induced in organic materials by heat in the absence of oxygen. In practice, it is not possible to achieve a completely oxygen-free atmosphere; actual pyrolytic systems are operated with less than stoichiometric quantities of...

  16. ENGINEERING BULLETIN: PYROLYSIS TREATMENT

    EPA Science Inventory

    Pyrolysis is formally defined as chemical decomposition induced in organic materials by heat in the absence of oxygen. In practice, it is not possible to achieve a completely oxygen-free atmosphere; actual pyrolytic systems are operated with less than stoichiometric quantities of...

  17. Chemical Stability and Biological Properties of Plasma-Sprayed CaO-SiO2-ZrO2 Coatings

    NASA Astrophysics Data System (ADS)

    Liang, Ying; Xie, Youtao; Ji, Heng; Huang, Liping; Zheng, Xuebin

    2010-12-01

    In this work, calcia-stabilized zirconia powders were coated by silica derived from tetraethoxysilane (TEOS) hydrolysis. After calcining at 1400 °C, decalcification of calcia-stabilized zirconia by silica occurred and powders composed of Ca2SiO4, ZrO2, and CaZrO3 were prepared. We produced three kinds of powders with different Ca2SiO4 contents [20 wt.% (denoted as CZS2), 40 wt.% (denoted as CZS4), and 60 wt.% (denoted as CZS6)]. The obtained powders were sprayed onto Ti-6Al-4V substrates using atmospheric plasma spraying. The microstructure of the powders and coatings were analyzed. The dissolution rates of the coatings were assessed by monitoring the ions release and mass losses after immersion in Tris-HCl buffer solution. Results showed that the chemical stability of the coatings were significantly improved compared with pure calcium silicate coatings, and increased with the increase of Zr contents. The CZS4 coating showed not only good apatite-formation ability in simulated body fluid, but also well attachment and proliferation capability for the canine bone marrow stem cells. Results presented here indicate that plasma-sprayed CZS4 coating has medium dissolution rate and good biological properties, suggesting its potential use as bone implants.

  18. Effect of solvent volume on the physical properties of aluminium doped nanocrystalline zinc oxide thin films deposited using a simplified spray pyrolysis technique

    NASA Astrophysics Data System (ADS)

    Jabena Begum, N.; Mohan, R.; Ravichandran, K.

    2013-01-01

    Aluminium doped zinc oxide (AZO) thin films were deposited by employing a low cost and simplified spray technique using a perfume atomizer from starting solutions having different volumes (10, 20, … , 50 mL) of solvent. The effect of solvent volume on the structural, electrical, optical, photoluminescence (PL) and surface morphological properties was studied. The electrical resistivity of the AZO films is remarkably influenced by the variation in the solvent volume. The X-ray diffraction profiles clearly showed that all the films have preferential orientation along the (0 0 2) plane irrespective of the solvent volume. The crystallite size was found to be in the nano range of 35-46 nm. The optical transmittance in the visible region is desirably high (>85%). The AFM images show columnar morphology with varying grain size. The PL studies revealed that the AZO film deposited from 50 mL of solvent volume has good quality with lesser defect density.

  19. Pyrolysis-Molecular Beam Mass Spectrometry to Characterize Soil Organic Matter Composition in Chemically Isolated Fractions from Differing Land Uses

    USDA-ARS?s Scientific Manuscript database

    Questions concerning the role of soil organic matter (SOM) in soil fertility, ecosystem functioning and global change requires knowledge of the controls on SOM stabilization and their interactions. Pyrolysis molecular beam mass spectrometry (py-MBMS) provides a powerful and rapid means of characteri...

  20. Effect of boric acid on the properties of Li{sub 2}MnO{sub 3}·LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} composite cathode powders prepared by large-scale spray pyrolysis with droplet classifier

    SciTech Connect

    Hong, Young Jun; Choi, Seung Ho; Sim, Chul Min; Lee, Jung-Kul; Kang, Yun Chan

    2012-12-15

    Graphical abstract: Display Omitted Highlights: ► Spherical shape Li{sub 2}MnO{sub 3}·LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} composite cathode powders are prepared by large-scale spray pyrolysis with droplet classifier. ► Boric acid improves the morphological and electrochemical properties of the composite cathode powders. ► The discharge capacity of the composite cathode powders decreases from 217 to 196 mAh g{sup −1} by the 30th cycle. -- Abstract: Spherically shaped 0.3Li{sub 2}MnO{sub 3}·0.7LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} composite cathode powders with filled morphology and narrow size distribution are prepared by large-scale spray pyrolysis. A droplet classification reduces the standard deviation of the size distribution of the composite cathode powders. Addition of boric acid improves the morphological properties of the product powders by forming a lithium borate glass material with low melting temperature. The optimum amount of boric acid dissolved in the spray solution is 0.8 wt% of the composite powders. The powders prepared from the spray solution with 0.8 wt% boric acid have a mixed layered crystal structure comprising Li{sub 2}MnO{sub 3} and LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} phases, thus forming a composite compound. The initial charge and discharge capacities of the composite cathode powders prepared from the 0.8 wt% boric acid spray solution are 297 and 217 mAh g{sup −1}, respectively. The discharge capacity of the powders decreases from 217 to 196 mAh g{sup −1} by the 30th cycle, in which the capacity retention is 90%.

  1. Detection of chemical warfare agent simulants and hydrolysis products in biological samples by paper spray mass spectrometry.

    PubMed

    McKenna, Josiah; Dhummakupt, Elizabeth S; Connell, Theresa; Demond, Paul S; Miller, Dennis B; Michael Nilles, J; Manicke, Nicholas E; Glaros, Trevor

    2017-05-02

    Paper spray ionization coupled to a high resolution tandem mass spectrometer (a quadrupole orbitrap) was used to identify and quantitate chemical warfare agent (CWA) simulants and their hydrolysis products in blood and urine. Three CWA simulants, dimethyl methylphosphonate (DMMP), trimethyl phosphate (TMP), and diisopropyl methylphosphonate (DIMP), and their isotopically labeled standards were analyzed in human whole blood and urine. Calibration curves were generated and tested with continuing calibration verification standards. Limits of detection for these three compounds were in the low ng mL(-1) range for the direct analysis of both blood and urine samples. Five CWA hydrolysis products, ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic acid (IMPA), isobutyl methylphosphonic acid (iBuMPA), cyclohexyl methylphosphonic acid (CHMPA), and pinacolyl methylphosphonic acid (PinMPA), were also analyzed. Calibration curves were generated in both positive and negative ion modes. Limits of detection in the negative ion mode ranged from 0.36 ng mL(-1) to 1.25 ng mL(-1) in both blood and urine for the hydrolysis products. These levels were well below those found in victims of the Tokyo subway attack of 2 to 135 ng mL(-1). Improved stability and robustness of the paper spray technique in the negative ion mode was achieved by the addition of chlorinated solvents. These applications demonstrate that paper spray mass spectrometry (PS-MS) can be used for rapid, sample preparation-free detection of chemical warfare agents and their hydrolysis products at physiologically relevant concentrations in biological samples.

  2. Improved Orifice Plate for Spray Gun

    NASA Technical Reports Server (NTRS)

    Cunningham, W.

    1986-01-01

    Erratic spray pattern of commercial spray gun changed to repeatable one by simple redesign of two parts. In modified spray gun orifice plate and polytetrafluoroethylene bushing redesigned to assure centering and alignment with nozzle. Such improvement useful in many industrial applications requiring repeatable spray patterns. Might include spraying of foam insulation, paint, other protective coatings, detergents, abrasives, adhesives, process chemicals, or fuels. Unmodified spray gun produces erratic spray because lateral misalignment between orifice plate and nozzle.

  3. Improved Orifice Plate for Spray Gun

    NASA Technical Reports Server (NTRS)

    Cunningham, W.

    1986-01-01

    Erratic spray pattern of commercial spray gun changed to repeatable one by simple redesign of two parts. In modified spray gun orifice plate and polytetrafluoroethylene bushing redesigned to assure centering and alignment with nozzle. Such improvement useful in many industrial applications requiring repeatable spray patterns. Might include spraying of foam insulation, paint, other protective coatings, detergents, abrasives, adhesives, process chemicals, or fuels. Unmodified spray gun produces erratic spray because lateral misalignment between orifice plate and nozzle.

  4. Comparative studies on AlGaN/GaN/Si MOS-HFETs with Al2O3/TiO2 stacked dielectrics by using an ultrasonic spray pyrolysis deposition technique

    NASA Astrophysics Data System (ADS)

    Lee, Ching-Sung; Hsu, Wei-Chou; Chiang, Bo-Jung; Liu, Han-Yin; Lee, Hsin-Yuan

    2017-05-01

    Al0.26Ga0.74N/GaN metal-oxide-semiconductor heterostructure field-effect transistors (MOS-HFETs) grown on a Si substrate with Al2O3/TiO2 stacked gate dielectrics formed by using non-vacuum ultrasonic spray pyrolysis deposition (USPD) technique are investigated. High permittivity (k) values of Al2O3 and TiO2 were characterized to be 9 and 46.1, respectively, with an equal layer thickness of 10 nm. The present MOS-HFET (Schottky-gate HFET) design has demonstrated enhanced device characteristics at 300 K, including maximum drain-source current density (I DS,max) of 725 (530) mA/mm, I DS at V GS = 0 V (I DSS0) of 471 (383) mA/mm, gate-voltage swing (GVS) of 2.5 (1.6) V, two-terminal gate-drain breakdown voltage (BV GD) of -182 (-121) V, turn-on voltage (V on) of 4.9 (3.2) V, three-terminal off-state drain-source breakdown voltage (BV DS) of 174 (103) V, on/off current ratio (I on/I off) of 5.6 × 107 (3.7 × 103), unity-gain cut-off frequency (f T ) of 10.3 (6.8) GHz, maximum oscillation frequency (f max) of 14.8 (8.6) GHz, and power-added efficiency (P.A.E.) of 38.5% (31.7%) at 2.4 GHz. High temperature device characteristics up to 450 K are also discussed.

  5. Production Mechanisms, Number Concentration, Size Distribution. Chemical Composition, and Optical Properties of Sea Spray Aerosols

    NASA Technical Reports Server (NTRS)

    Meskhidze, Nicholas; Petters, Markus; Tsigaridis, Kostas; Bates. Tim; O'Dowd, Colin; Reid, Jeff; Lewis, Ernie R.; Gantt, Brett; Anguelova, Magdalena D.; Bhave, Prakash V.; Bird, James; Callaghan, Adrian H.; Ceburnis, Darius; Chang, Rachel; Clark, Antony; deLeeuw, Gerrit; Deane, Grant; DeMott, Paul J.; Elliot, Scott; Facchini, Maria Cristina; Fairall, Chris W.; Hawkins, Lelia; Hu, Yongxiang; Smirnov, Alexander

    2013-01-01

    Over forty scientists from six countries convened in Raleigh, NC on June 4-6 2012 to review the status and prospects of sea spray aerosol research. Participants were researchers from the oceanography and atmospheric science communities, including academia, private industry, and government agencies. The recommendations from the working groups are summarized in a science prioritization matrix that is meant to prioritize the research agenda and identify areas of investigation by the magnitude of their impact on proposed science questions. Str

  6. Gas phase temperature measurements in the liquid and particle regime of a flame spray pyrolysis process using O2-based pure rotational coherent anti-Stokes Raman scattering.

    PubMed

    Engel, Sascha R; Koegler, Andreas F; Gao, Yi; Kilian, Daniel; Voigt, Michael; Seeger, Thomas; Peukert, Wolfgang; Leipertz, Alfred

    2012-09-01

    For the production of oxide nanoparticles at a commercial scale, flame spray processes are frequently used where mostly oxygen is fed to the flame if high combustion temperatures and thus small primary particle sizes are desired. To improve the understanding of these complex processes in situ, noninvasive optical measurement techniques were applied to characterize the extremely turbulent and unsteady combustion field at those positions where the particles are formed from precursor containing organic solvent droplets. This particle-forming regime was identified by laser-induced breakdown detection. The gas phase temperatures in the surrounding of droplets and particles were measured with O(2)-based pure rotational coherent anti-Stokes Raman scattering (CARS). Pure rotational CARS measurements benefit from a polarization filtering technique that is essential in particle and droplet environments for acquiring CARS spectra suitable for temperature fitting. Due to different signal disturbing processes only the minority of the collected signals could be used for temperature evaluation. The selection of these suitable signals is one of the major problems to be solved for a reliable evaluation process. Applying these filtering and signal selection steps temperature measurements have successfully been conducted. Time-resolved, single-pulse measurements exhibit temperatures between near-room and combustion temperatures due to the strongly fluctuating and flickering behavior of the particle-generating flame. The mean flame temperatures determined from the single-pulse data are decreasing with increasing particle concentrations. They indicate the dissipation of large amounts of energy from the surrounding gas phase in the presence of particles.

  7. Acanthocephalan fish parasites (Rhadinorhynchidae Lühe, 1912) as potential biomarkers: Molecular-chemical screening by pyrolysis-field ionization mass spectrometry

    NASA Astrophysics Data System (ADS)

    Kleinertz, S.; Eckhardt, K.-U.; Theisen, S.; Palm, H. W.; Leinweber, P.

    2016-07-01

    The present study represents the first molecular-chemical screening by pyrolysis-field ionization mass spectrometry applied on fish parasites. A total of 71 fishes from Balinese fish markets, 36 Auxis rochei (Risso, 1810) and 35 A. thazard (Lacepède, 1800), were studied for their acanthocephalan parasites. This is the first record of Rhadinorhynchus zhukovi in Balinese waters, Indonesia, and we describe for the first time A. rochei and A. thazard as R. zhukovi hosts. Using this method, small scale variations within the chemical compounds of acanthocephalans could be detected. Using this methodology it will be possible to generate additional, pollutant specific information from aquatic habitats in future with the potential of a new bioindicator application for parasite/host origin and/or environmental pollution.

  8. Catalytic and non-catalytic pyrolysis of biomass in non-inert environments for production of deoxygenated bio-oil and chemicals

    USDA-ARS?s Scientific Manuscript database

    Fast pyrolysis processes are among the most effective methods for liquefaction of lignocellulosic biomass. Catalytic fast pyrolysis (CFP) over HZSM-5 or other zeolites and/or utilization of reactive atmospheres such as in the non-catalytic Tail Gas Reactive Pyrolysis (TRGP) process, a recent patent...

  9. Plasma-Sprayed Hydroxylapatite-Based Coatings: Chemical, Mechanical, Microstructural, and Biomedical Properties

    NASA Astrophysics Data System (ADS)

    Heimann, Robert B.

    2016-06-01

    This contribution discusses salient properties and functions of hydroxylapatite (HA)-based plasma-sprayed coatings, including the effect on biomedical efficacy of coating thickness, phase composition and distribution, amorphicity and crystallinity, porosity and surface roughness, cohesion and adhesion, micro- and nano-structured surface morphology, and residual coating stresses. In addition, it will provide details of the thermal alteration that HA particles undergo in the extremely hot plasma jet that leads to dehydroxylated phases such as oxyhydroxylapatite (OHA) and oxyapatite (OA) as well as thermal decomposition products such as tri-(TCP) and tetracalcium phosphates (TTCP), and quenched phases such as amorphous calcium phosphate (ACP). The contribution will further explain the role of ACP during the in vitro interaction of the as-deposited coatings with simulated body fluid resembling the composition of extracellular fluid (ECF) as well as the in vivo responses of coatings to the ECF and the host tissue, respectively. Finally, it will briefly describe performance profiles required to fulfill biological functions of osteoconductive bioceramic coatings designed to improve osseointegration of hip endoprostheses and dental root implants. In large parts, the content of this contribution is a targeted review of work done by the author and his students and coworkers over the last two decades. In addition, it is considered a stepping stone toward a standard operation procedure aimed at depositing plasma-sprayed bioceramic implant coatings with optimum properties.

  10. Peat pyrolysis and the analytical semi-empirical model

    SciTech Connect

    Feng, J.; Green, A.E.S.

    2007-07-01

    Pyrolysis of peat could convert this material into useful fuels and valuable hydrocarbons. A study of peat pyrolysis can also serve as a useful bridge between studies of coal pyrolysis and biomass pyrolysis. Using an analytical model of pyrolysis that has previously been applied to biomass and to coal, we present here the results of applications of this model to a representative peat. The analysis suggests means of organizing and processing rate and yield data that should be useful in applications of pyrolysis for the production of fuels and chemicals.

  11. Spray Chemical Vapor Deposition of CulnS2 Thin Films for Application in Solar Cell Devices

    NASA Technical Reports Server (NTRS)

    Hollingsworth, Jennifer A.; Buhro, William E.; Hepp, Aloysius F.; Jenkins. Philip P.; Stan, Mark A.

    1998-01-01

    Chalcopyrite CuInS2 is a direct band gap semiconductor (1.5 eV) that has potential applications in photovoltaic thin film and photoelectrochemical devices. We have successfully employed spray chemical vapor deposition using the previously known, single-source, metalorganic precursor, (Ph3P)2CuIn(SEt)4, to deposit CuInS2 thin films. Stoichiometric, polycrystalline films were deposited onto fused silica over a range of temperatures (300-400 C). Morphology was observed to vary with temperature: spheroidal features were obtained at lower temperatures and angular features at 400 C. At even higher temperatures (500 C), a Cu-deficient phase, CuIn5S8, was obtained as a single phase. The CuInS2 films were determined to have a direct band gap of ca. 1.4 eV.

  12. Critical evaluation of Jet-A spray combustion using propane chemical kinetics in gas turbine combustion simulated by KIVA-2

    NASA Technical Reports Server (NTRS)

    Nguyen, H. L.; Ying, S.-J.

    1990-01-01

    Jet-A spray combustion has been evaluated in gas turbine combustion with the use of propane chemical kinetics as the first approximation for the chemical reactions. Here, the numerical solutions are obtained by using the KIVA-2 computer code. The KIVA-2 code is the most developed of the available multidimensional combustion computer programs for application of the in-cylinder combustion dynamics of internal combustion engines. The released version of KIVA-2 assumes that 12 chemical species are present; the code uses an Arrhenius kinetic-controlled combustion model governed by a four-step global chemical reaction and six equilibrium reactions. Researchers efforts involve the addition of Jet-A thermophysical properties and the implementation of detailed reaction mechanisms for propane oxidation. Three different detailed reaction mechanism models are considered. The first model consists of 131 reactions and 45 species. This is considered as the full mechanism which is developed through the study of chemical kinetics of propane combustion in an enclosed chamber. The full mechanism is evaluated by comparing calculated ignition delay times with available shock tube data. However, these detailed reactions occupy too much computer memory and CPU time for the computation. Therefore, it only serves as a benchmark case by which to evaluate other simplified models. Two possible simplified models were tested in the existing computer code KIVA-2 for the same conditions as used with the full mechanism. One model is obtained through a sensitivity analysis using LSENS, the general kinetics and sensitivity analysis program code of D. A. Bittker and K. Radhakrishnan. This model consists of 45 chemical reactions and 27 species. The other model is based on the work published by C. K. Westbrook and F. L. Dryer.

  13. Molecular mechanisms in the pyrolysis of unsaturated chlorinated hydrocarbons: formation of benzene rings. 1. Quantum chemical studies.

    PubMed

    McIntosh, Grant J; Russell, Douglas K

    2013-05-23

    Analogues of important aromatic growth mechanisms in hydrocarbon pyrolysis and combustion systems are extended to chlorinated systems. We consider the addition of C2Cl2 to both C4Cl3 and C4Cl5 radicals at the M06-2X/6-311+G(3df,3p)//B3LYP/6-31G(d) level of theory, and we demonstrate that these reaction systems have much in common with those of nonchlorinated species. In particular, we find that these radicals appear to lead preferentially to fulvenes, and not to the observed aromatic products, as is found in nonchlorinated systems. We have therefore also considered nonradical C4/C2 channels by way of Diels-Alder cyclization of C4Cl4/C2Cl2 and C4H2Cl2/C2HCl pairs to describe aromatic formation. While the latter pair readily leads to the formation of partially chlorinated benzenes, the fully chlorinated congeners are sterically prohibited from ring closing directly; this leads to a series of novel rearrangement processes which predict the formation of hexachloro-1,5-diene-3-yne, in addition to hexachlorobenzene, in good agreement with experiment. This suggests, for the first time, that facile nonradical routes to aromatic formation are operative in partially and fully chlorinated pyrolysis and combustion systems.

  14. The Chemical Composition and Mixing State of Sea Spray Aerosol and Organic Aerosol in the Winter-Spring Arctic

    NASA Astrophysics Data System (ADS)

    Kirpes, R.; Bondy, A. L.; Bonanno, D.; Moffet, R.; Wang, B.; Laskin, A.; Ault, A. P.; Pratt, K.

    2016-12-01

    The Arctic region is undergoing rapid transformations and loss of sea ice due to climate change. With increased sea ice fracturing resulting in greater open ocean surface, winter emissions of sea spray aerosol (SSA) are expected to be increasing. Additionally, during the winter-spring transition, Arctic haze contributes to the Arctic aerosol budget. The magnitude of aerosol climate effects depends on the aerosol composition and mixing state (distribution of chemical species within and between particles). However, few studies of aerosol chemistry have been conducted in the winter Arctic, despite it being a time when aerosol impacts on clouds are expected to be significant. To study aerosol composition and mixing state in the winter Arctic, atmospheric particles were collected near Barrow, Alaska in January and February 2014 for off-line individual particle chemical analysis. SSA was the most prevalent particle type observed. Sulfate and nitrate were observed to be internally mixed with SSA and organic aerosol. Greater than 98% of observed SSA particles contained organic content, with 15-35% organic volume fraction on average for individual particles. The SSA organic compounds consisted of carbohydrates, lipids, and fatty acids found in the seawater surface microlayer. SSA was determined to be emitted from open leads, while transported sulfate and nitrate contributed to aging of SSA and organic aerosol. Determining the aerosol chemical composition and mixing state in the winter Arctic will further the understanding of how individual aerosol particles impact climate through radiative effects and cloud formation.

  15. Influence of precursor solution parameters on chemical properties of calcium phosphate coatings prepared using Electrostatic Spray Deposition (ESD).

    PubMed

    Leeuwenburgh, S C G; Wolke, J G C; Schoonman, J; Jansen, J A

    2004-02-01

    A novel coating technique, referred to as Electrostatic Spray Deposition (ESD), was used to deposit calcium phosphate (CaP) coatings with a variety of chemical properties. The relationship between the composition of the precursor solutions and the crystal and molecular structure of the deposited coatings was investigated by means of X-ray diffraction (XRD), Fourier-Transform Infrared Spectroscopy (FTIR) and Energy Dispersive Spectroscopy (EDS). It was shown that the relative Ca/P ratio in the precursor solution, the absolute precursor concentration, the acidity of the precursor solution and the type of Ca-precursor strongly influenced the chemical nature of the deposited CaP coatings. Various crystal phases and phase mixtures were obtained, such as carbonate apatite, beta-TCP, Mg-substituted whitlockite, monetite, beta/gamma-pyrophosphate, and calcite. It was shown that carbonate plays an essential role in the chemical mechanism of coating formation. Carbonate is formed due to a decomposition reaction of organic solvents. Depending on deposition conditions, carbonate anions (a) react with acidic phosphate groups, (b) are incorporated into apatitic calcium phosphate phases, and (c) react with excessive Ca(2+) cations in case of phosphate-deficient precursor solutions.

  16. Aqueous stream characterization from biomass fast pyrolysis and catalytic fast pyrolysis

    SciTech Connect

    Black, Brenna A.; Michener, William E.; Ramirez, Kelsey J.; Biddy, Mary J.; Knott, Brandon C.; Jarvis, Mark W.; Olstad, Jessica; Mante, Ofei D.; Dayton, David C.; Beckham, Gregg T.

    2016-09-05

    Here, biomass pyrolysis offers a promising means to rapidly depolymerize lignocellulosic biomass for subsequent catalytic upgrading to renewable fuels. Substantial efforts are currently ongoing to optimize pyrolysis processes including various fast pyrolysis and catalytic fast pyrolysis schemes. In all cases, complex aqueous streams are generated containing solubilized organic compounds that are not converted to target fuels or chemicals and are often slated for wastewater treatment, in turn creating an economic burden on the biorefinery. Valorization of the species in these aqueous streams, however, offers significant potential for substantially improving the economics and sustainability of thermochemical biorefineries. To that end, here we provide a thorough characterization of the aqueous streams from four pilot-scale pyrolysis processes: namely, from fast pyrolysis, fast pyrolysis with downstream fractionation, in situ catalytic fast pyrolysis, and ex situ catalytic fast pyrolysis. These configurations and processes represent characteristic pyrolysis processes undergoing intense development currently. Using a comprehensive suite of aqueous-compatible analytical techniques, we quantitatively characterize between 12 g kg-1 of organic carbon of a highly aqueous catalytic fast pyrolysis stream and up to 315 g kg-1 of organic carbon present in the fast pyrolysis aqueous streams. In all cases, the analysis ranges between 75 and 100% of mass closure. The composition and stream properties closely match the nature of pyrolysis processes, with high contents of carbohydrate-derived compounds in the fast pyrolysis aqueous phase, high acid content in nearly all streams, and mostly recalcitrant phenolics in the heavily deoxygenated ex situ catalytic fast pyrolysis stream. Overall, this work provides a detailed compositional analysis of aqueous streams from leading thermochemical processes -- analyses that are critical for subsequent

  17. Aqueous stream characterization from biomass fast pyrolysis and catalytic fast pyrolysis

    DOE PAGES

    Black, Brenna A.; Michener, William E.; Ramirez, Kelsey J.; ...

    2016-09-05

    Here, biomass pyrolysis offers a promising means to rapidly depolymerize lignocellulosic biomass for subsequent catalytic upgrading to renewable fuels. Substantial efforts are currently ongoing to optimize pyrolysis processes including various fast pyrolysis and catalytic fast pyrolysis schemes. In all cases, complex aqueous streams are generated containing solubilized organic compounds that are not converted to target fuels or chemicals and are often slated for wastewater treatment, in turn creating an economic burden on the biorefinery. Valorization of the species in these aqueous streams, however, offers significant potential for substantially improving the economics and sustainability of thermochemical biorefineries. To that end, heremore » we provide a thorough characterization of the aqueous streams from four pilot-scale pyrolysis processes: namely, from fast pyrolysis, fast pyrolysis with downstream fractionation, in situ catalytic fast pyrolysis, and ex situ catalytic fast pyrolysis. These configurations and processes represent characteristic pyrolysis processes undergoing intense development currently. Using a comprehensive suite of aqueous-compatible analytical techniques, we quantitatively characterize between 12 g kg-1 of organic carbon of a highly aqueous catalytic fast pyrolysis stream and up to 315 g kg-1 of organic carbon present in the fast pyrolysis aqueous streams. In all cases, the analysis ranges between 75 and 100% of mass closure. The composition and stream properties closely match the nature of pyrolysis processes, with high contents of carbohydrate-derived compounds in the fast pyrolysis aqueous phase, high acid content in nearly all streams, and mostly recalcitrant phenolics in the heavily deoxygenated ex situ catalytic fast pyrolysis stream. Overall, this work provides a detailed compositional analysis of aqueous streams from leading thermochemical processes -- analyses that are critical for subsequent development of selective

  18. Aqueous stream characterization from biomass fast pyrolysis and catalytic fast pyrolysis

    SciTech Connect

    Black, Brenna A.; Michener, William E.; Ramirez, Kelsey J.; Biddy, Mary J.; Knott, Brandon C.; Jarvis, Mark W.; Olstad, Jessica; Mante, Ofei D.; Dayton, David C.; Beckham, Gregg T.

    2016-09-05

    Here, biomass pyrolysis offers a promising means to rapidly depolymerize lignocellulosic biomass for subsequent catalytic upgrading to renewable fuels. Substantial efforts are currently ongoing to optimize pyrolysis processes including various fast pyrolysis and catalytic fast pyrolysis schemes. In all cases, complex aqueous streams are generated containing solubilized organic compounds that are not converted to target fuels or chemicals and are often slated for wastewater treatment, in turn creating an economic burden on the biorefinery. Valorization of the species in these aqueous streams, however, offers significant potential for substantially improving the economics and sustainability of thermochemical biorefineries. To that end, here we provide a thorough characterization of the aqueous streams from four pilot-scale pyrolysis processes: namely, from fast pyrolysis, fast pyrolysis with downstream fractionation, in situ catalytic fast pyrolysis, and ex situ catalytic fast pyrolysis. These configurations and processes represent characteristic pyrolysis processes undergoing intense development currently. Using a comprehensive suite of aqueous-compatible analytical techniques, we quantitatively characterize between 12 g kg-1 of organic carbon of a highly aqueous catalytic fast pyrolysis stream and up to 315 g kg-1 of organic carbon present in the fast pyrolysis aqueous streams. In all cases, the analysis ranges between 75 and 100% of mass closure. The composition and stream properties closely match the nature of pyrolysis processes, with high contents of carbohydrate-derived compounds in the fast pyrolysis aqueous phase, high acid content in nearly all streams, and mostly recalcitrant phenolics in the heavily deoxygenated ex situ catalytic fast pyrolysis stream. Overall, this work provides a detailed compositional analysis of aqueous streams from leading thermochemical processes -- analyses that are critical for subsequent

  19. Chemical composition and biological value of spray dried porcine blood by-products and bone protein hydrolysate for young chickens.

    PubMed

    Jamroz, D; Wiliczkiewicz, A; Orda, J; Skorupińska, J; Słupczyńska, M; Kuryszko, J

    2011-10-01

    The chemical composition of spray dried porcine blood by-products is characterised by wide variation in crude protein contents. In spray dried porcine blood plasma (SDBP) it varied between 670-780 g/kg, in spray dried blood cells (SDBC) between 830-930 g/kg, and in bone protein hydrolysate (BPH) in a range of 740-780 g/kg. Compared with fish meal, these feeds are poor in Met and Lys. Moreover, in BPH deep deficits of Met, Cys, Thr and other amino acids were found. The experiment comprised 7 dietary treatments: SDBP, SDBC, and BPH, each at an inclusion rate of 20 or 40 g/kg diet, plus a control. The addition of 20 or 40 g/kg of the analysed meals into feeds for very young chickens (1-28 d post hatch) significantly decreased the body weight (BW) of birds. Only the treatments with 40 g/kg of SDBP and SDBC showed no significant difference in BW as compared with the control. There were no significant differences between treatments and type of meal for feed intake, haematocrit and haemoglobin concentrations in blood. Addition of bone protein and blood cell meals to feed decreased the IgG concentration in blood and caused shortening of the femur and tibia bones. However, changes in the mineral composition of bones were not significantly affected by the type of meal used. The blood by-products, which are rich in microelements, improved retention of Ca and Cu only. In comparison to control chickens, significantly better accretion of these minerals was found in treatments containing 20 g/kg of SDBP or 40 g/kg of SDBC. Great variability in apparent ileal amino acid digestibility in chickens was determined. In this respect, some significant differences related to the type of meal fed were confirmed for Asp, Pro, Val, Tyr and His. In general, the apparent ileal digestibility of amino acids was about 2-3 percentage units better in chickens fed on diets containing the animal by products than in control birds.

  20. Microprobe sampling--photo ionization-time-of-flight mass spectrometry for in situ chemical analysis of pyrolysis and combustion gases: examination of the thermo-chemical processes within a burning cigarette.

    PubMed

    Hertz, Romy; Streibel, Thorsten; Liu, Chuan; McAdam, Kevin; Zimmermann, Ralf

    2012-02-10

    A microprobe sampling device (μ-probe) has been developed for in situ on-line photo ionization mass spectrometric analysis of volatile chemical species formed within objects consisting of organic matter during thermal processing. With this approach the chemical signature occurring during heating, pyrolysis, combustion, roasting and charring of organic material within burning objects such as burning fuel particles (e.g., biomass or coal pieces), lit cigarettes or thermally processed food products (e.g., roasting of coffee beans) can be investigated. Due to its dynamic changes between combustion and pyrolysis phases the cigarette smoking process is particularly interesting and has been chosen as first application. For this investigation the tip of the μ-probe is inserted directly into the tobacco rod and volatile organic compounds from inside the burning cigarette are extracted and real-time analyzed as the glowing front (or coal) approaches and passes the μ-probe sampling position. The combination of micro-sampling with photo ionization time-of-flight mass spectrometry (PI-TOFMS) allows on-line intrapuff-resolved analysis of species formation inside a burning cigarette. Monitoring volatile smoke compounds during cigarette puffing and smoldering cycles in this way provides unparalleled insights into formation mechanisms and their time-dependent change. Using this technique the changes from pyrolysis conditions to combustion conditions inside the coal of a cigarette could be observed directly. A comparative analysis of species formation within a burning Kentucky 2R4F reference cigarette with μ-probe analysis reveals different patterns and behaviors for nicotine, and a range of semi-volatile aromatic and aliphatic species.

  1. Effects of spray-drying conditions on the chemical, physical, and sensory properties of cheese powder.

    PubMed

    Koca, Nurcan; Erbay, Zafer; Kaymak-Ertekin, Figen

    2015-05-01

    Dairy powders are produced to increase the shelf life of fresh dairy products and for use as flavoring agents. In this study, 24 cheese powders produced under 7 different conditions were used to investigate the effects of spray-drying parameters (e.g., inlet air temperature, atomization pressure, and outlet air temperature) on the quality of white cheese powder. Composition, color, physical properties, reconstitution, and sensory characteristics of white cheese powders were determined. The results revealed that the white cheese powders produced in this study had low moisture content ratios and water activity values. High outlet air temperatures caused browning and enhanced Maillard reactions. Additionally, high outlet air temperatures increased wettability and dispersibility and decreased the solubility of white cheese powders. Free fat content was positively correlated with inlet air temperature and negatively correlated with outlet air temperature and atomization pressure. Sensory analyses revealed that white cheese powder samples had acceptable sensory characteristics with the exception of the sample produced at an outlet air temperature of 100°C, which had high scores for scorched flavor and color and low scores for cheese flavor.

  2. Direct aerosol chemical composition measurements to evaluate the physicochemical differences between controlled sea spray aerosol generation schemes

    NASA Astrophysics Data System (ADS)

    Collins, D. B.; Zhao, D. F.; Ruppel, M. J.; Laskina, O.; Grandquist, J. R.; Modini, R. L.; Stokes, M. D.; Russell, L. M.; Bertram, T. H.; Grassian, V. H.; Deane, G. B.; Prather, K. A.

    2014-11-01

    Controlled laboratory studies of the physical and chemical properties of sea spray aerosol (SSA) must be under-pinned by a physically and chemically accurate representation of the bubble-mediated production of nascent SSA particles. Bubble bursting is sensitive to the physico-chemical properties of seawater. For a sample of seawater, any important differences in the SSA production mechanism are projected into the composition of the aerosol particles produced. Using direct chemical measurements of SSA at the single-particle level, this study presents an intercomparison of three laboratory-based, bubble-mediated SSA production schemes: gas forced through submerged sintered glass filters ("frits"), a pulsed plunging-waterfall apparatus, and breaking waves in a wave channel filled with natural seawater. The size-resolved chemical composition of SSA particles produced by breaking waves is more similar to particles produced by the plunging waterfall than those produced by sintered glass filters. Aerosol generated by disintegrating foam produced by sintered glass filters contained a larger fraction of organic-enriched particles and a different size-resolved elemental composition, especially in the 0.8-2 μm dry diameter range. Interestingly, chemical differences between the methods only emerged when the particles were chemically analyzed at the single-particle level as a function of size; averaging the elemental composition of all particles across all sizes masked the differences between the SSA samples. When dried, SSA generated by the sintered glass filters had the highest fraction of particles with spherical morphology compared to the more cubic structure expected for pure NaCl particles produced when the particle contains relatively little organic carbon. In addition to an intercomparison of three SSA production methods, the role of the episodic or "pulsed" nature of the waterfall method on SSA composition was under-taken. In organic-enriched seawater, the continuous

  3. Spray Pyrolysis as a Synthetic Tool.

    DTIC Science & Technology

    1984-11-01

    tetracyclic system (84) (40%) m.p. > 350*C (Lit. 40> 3300C). I+ S’ 0 S 45. References 1. Azidoformates were prepared by the method of L.A. Caprino , B.A... Caprino , C.A. Giz, R.N. Murray, A.A. Santilli, and P.H. Terry, Organic Synthesis, 1973, Coil. Vol , p.168. 2. R.K. Smalley, ’Azepines’ in

  4. Efficacy of chemical sprays to eliminate inoculated Salmonella from defeathered broiler breast skin

    USDA-ARS?s Scientific Manuscript database

    Contamination of poultry with Salmonella is a food safety concern. Because Salmonella-free broilers cannot always be produced on the farm, antimicrobials are used in the processing plant. The objective of this study was to look at the efficacy of several chemicals to eliminate 104 cells of a marker...

  5. Extent of pyrolysis impacts on fast pyrolysis biochar properties.

    PubMed

    Brewer, Catherine E; Hu, Yan-Yan; Schmidt-Rohr, Klaus; Loynachan, Thomas E; Laird, David A; Brown, Robert C

    2012-01-01

    A potential concern about the use of fast pyrolysis rather than slow pyrolysis biochars as soil amendments is that they may contain high levels of bioavailable C due to short particle residence times in the reactors, which could reduce the stability of biochar C and cause nutrient immobilization in soils. To investigate this concern, three corn ( L.) stover fast pyrolysis biochars prepared using different reactor conditions were chemically and physically characterized to determine their extent of pyrolysis. These biochars were also incubated in soil to assess their impact on soil CO emissions, nutrient availability, microorganism population growth, and water retention capacity. Elemental analysis and quantitative solid-state C nuclear magnetic resonance spectroscopy showed variation in O functional groups (associated primarily with carbohydrates) and aromatic C, which could be used to define extent of pyrolysis. A 24-wk incubation performed using a sandy soil amended with 0.5 wt% of corn stover biochar showed a small but significant decrease in soil CO emissions and a decrease in the bacteria:fungi ratios with extent of pyrolysis. Relative to the control soil, biochar-amended soils had small increases in CO emissions and extractable nutrients, but similar microorganism populations, extractable NO levels, and water retention capacities. Corn stover amendments, by contrast, significantly increased soil CO emissions and microbial populations, and reduced extractable NO. These results indicate that C in fast pyrolysis biochar is stable in soil environments and will not appreciably contribute to nutrient immobilization. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  6. Direct aerosol chemical composition measurements to evaluate the physicochemical differences between controlled sea spray aerosol generation schemes

    NASA Astrophysics Data System (ADS)

    Collins, D. B.; Zhao, D. F.; Ruppel, M. J.; Laskina, O.; Grandquist, J. R.; Modini, R. L.; Stokes, M. D.; Russell, L. M.; Bertram, T. H.; Grassian, V. H.; Deane, G. B.; Prather, K. A.

    2014-07-01

    Controlled laboratory studies of the physical and chemical properties of sea spray aerosol (SSA) must be underpinned by a physically and chemically accurate representation of the bubble mediated production of nascent SSA particles. Since bubble bursting is sensitive to the physicochemical properties of seawater, any important differences in the SSA production mechanism are projected into SSA composition. Using direct chemical measurements of SSA at the single-particle level, this study presents an inter-comparison of three laboratory-based, bubble-mediated SSA production schemes: gas forced through submerged sintered glass filters ("frits"), a pulsed plunging waterfall apparatus, and breaking waves in a wave channel filled with natural seawater. The size-resolved chemical composition of SSA particles produced by breaking waves is more similar to particles produced by the plunging waterfall than sintered glass filters. Aerosol generated by disintegrating foam produced by sintered glass filters contained a larger fraction of organic enriched particles and a different size-resolved elemental composition, especially in the 0.8-2 μm size range. These particles, when dried, had more spherical morphologies compared to the more cubic structure expected for pure NaCl particles, which can be attributed to the presence of additional organic carbon. In addition to an inter-comparison of three SSA production methods, the role of the episodic or "pulsed" nature of the waterfall method utilized in this study on SSA composition was undertaken. In organic-enriched seawater, the continuous operation of the plunging waterfall mechanism resulted in the accumulation of surface foam and an over-expression of organic matter in SSA particles compared to pulsed plunging waterfall. Throughout this set of experiments, comparative differences in the SSA number size distribution were coincident with differences in aerosol composition, indicating that the production mechanism of SSA exerts

  7. Linear-Source Ultrasonic Spray Chemical Vapor Deposition Method for Fabrication of ZnMgO Films and Ultraviolet Photodetectors

    NASA Astrophysics Data System (ADS)

    Kamada, Yudai; Kawaharamura, Toshiyuki; Nishinaka, Hiroyuki; Fujita, Shizuo

    2006-08-01

    A linear-source ultrasonic spray chemical vapor deposition method has been developed and applied to fabricate ZnMgO ternary alloy thin films on glass substrates. A water solution of zinc acetate and magnesium acetate was ultrasonically atomized to form aerosol particles of water containing the sources, and then they were supplied onto the heated substrate by a nitrogen carrier gas through a nozzle with a linear aperture to form ZnMgO films. The source concentration ratios in the water solution successfully controlled the solid composition and hence raised the band gap of ZnMgO up to 3.75 eV, keeping the optical transmission higher than 90% for the visible-light region. An UV photodetector fabricated using the ZnMgO film showed the photoresponsivity to be as high as a few A/W, suggesting that this simple and cost-effective technique is promising for fabricating ZnMgO films for various applications.

  8. Formation of Indium-Doped Zinc Oxide Thin Films Using Ultrasonic Spray Pyrolysis: The Importance of the Water Content in the Aerosol Solution and the Substrate Temperature for Enhancing Electrical Transport.

    PubMed

    Biswal, Rajesh; Castañeda, Luis; Moctezuma, Rosario; Vega-Pérez, Jaime; Olvera, María De La Luz; Maldonado, Arturo

    2012-03-12

    Indium doped zinc oxide [ZnO:In] thin films have been deposited at 430°C on soda-lime glass substrates by the chemical spray technique, starting from zinc acetate and indium acetate. Pulverization of the solution was done by ultrasonic excitation. The variations in the electrical, structural, optical, and morphological characteristics of ZnO:In thin films, as a function of both the water content in the starting solution and the substrate temperature, were studied. The electrical resistivity of ZnO:In thin films is not significantly affected with the increase in the water content, up to 200 mL/L; further increase in water content causes an increase in the resistivity of the films. All films show a polycrystalline character, fitting well with the hexagonal ZnO wurtzite-type structure. No preferential growth in samples deposited with the lowest water content was observed, whereas an increase in water content gave rise to a (002) growth. The surface morphology of the films shows a consistency with structure results, as non-geometrical shaped round grains were observed in the case of films deposited with the lowest water content, whereas hexagonal slices, with a wide size distribution were observed in the other cases. In addition, films deposited with the highest water content show a narrow size distribution.

  9. Formation of Indium-Doped Zinc Oxide Thin Films Using Ultrasonic Spray Pyrolysis: The Importance of the Water Content in the Aerosol Solution and the Substrate Temperature for Enhancing Electrical Transport

    PubMed Central

    Biswal, Rajesh; Castañeda, Luis; Moctezuma, Rosario; Vega-Pérez, Jaime; De La Luz Olvera, María; Maldonado, Arturo

    2012-01-01

    Indium doped zinc oxide [ZnO:In] thin films have been deposited at 430°C on soda-lime glass substrates by the chemical spray technique, starting from zinc acetate and indium acetate. Pulverization of the solution was done by ultrasonic excitation. The variations in the electrical, structural, optical, and morphological characteristics of ZnO:In thin films, as a function of both the water content in the starting solution and the substrate temperature, were studied. The electrical resistivity of ZnO:In thin films is not significantly affected with the increase in the water content, up to 200 mL/L; further increase in water content causes an increase in the resistivity of the films. All films show a polycrystalline character, fitting well with the hexagonal ZnO wurtzite-type structure. No preferential growth in samples deposited with the lowest water content was observed, whereas an increase in water content gave rise to a (002) growth. The surface morphology of the films shows a consistency with structure results, as non-geometrical shaped round grains were observed in the case of films deposited with the lowest water content, whereas hexagonal slices, with a wide size distribution were observed in the other cases. In addition, films deposited with the highest water content show a narrow size distribution. PMID:28817056

  10. Chemical stability and osteogenic activity of plasma-sprayed boron-modified calcium silicate-based coatings.

    PubMed

    Lu, Xiang; Li, Kai; Xie, Youtao; Huang, Liping; Zheng, Xuebin

    2016-11-01

    In recent years, CaSiO3 bio-ceramic coatings have attracted great attention because of their good bioactivity. However, their high degradation rates in physiological environment restrict their practical applications. In this work, boron-modified CaSiO3 ceramic (Ca11Si4B2O22, B-CS) coating was developed on Ti substrates by plasma-spraying technique attempting to obtain enhanced chemical stability and osteogenic activity. The B-CS coating possessed significantly increased chemical stability due to the introduction of boron and consequently the modified crystal structure, while maintaining good bioactivity. Scanning electron microscope and immunofluorescence studies showed that better cellular adhesion and extinctive filopodia-like processes were observed on the B-CS coating. Compared with the pure CaSiO3 (CS) coating, the B-CS coating promoted MC3T3-E1 cells attachment and proliferation. In addition, enhanced collagen I (COL-I) secretion, alkaline phosphatase activity, and extracellular matrix mineralization levels were detected from the B-CS coating. According to RT-PCR results, notable up-regulation expressions of mineralized tissue-related genes, such as runt-related transcription factor 2 (Runx2), bone sialoprotein and osteocalcin, and bone morphogenetic protein 7 (BMP-7) were observed on the B-CS coating compared with the CS coating. The above results suggested that Ca11Si4B2O22 coatings possess excellent osteogenic activity and might be a promising candidate for orthopedic applications.

  11. Spray-Pyrolyzed Three-Dimensional CuInS2 Solar Cells on Nanocrystalline-Titania Electrodes with Chemical-Bath-Deposited Inx(OH)ySz Buffer Layers

    NASA Astrophysics Data System (ADS)

    Nguyen, Duy-Cuong; Mikami, Yuki; Tsujimoto, Kazuki; Ryo, Toshihiro; Ito, Seigo

    2012-10-01

    Three-dimensional (3D) compound solar cells with the structure of have been fabricated by spray pyrolysis deposition of CuInS2 and chemical-bath deposition of Inx(OH)ySz for the light absorber and buffer layer, respectively. The effect of deposition and annealing conditions of Inx(OH)ySz on the photovoltaic properties of 3D CuInS2 solar cells was investigated. Inx(OH)ySz annealed in air ambient showed a better cell performance than those annealed in nitrogen ambient and without annealing. The improvement of the performance of cells with Inx(OH)ySz buffer layers annealed in air ambient is due to the increase in oxide concentration in the buffer layers [confirmed by X-ray photoelectron spectroscopy (XPS) measurement]. Among cells with Inx(OH)ySz buffer layers deposited for 1, 1.5, 1.75, and 2 h, that with Inx(OH)ySz deposited for 1.75 h showed the best cell performance. The best cell performance was observed for Inx(OH)ySz deposited for 1.75 h with annealing at 300 °C for 30 min in air ambient, and cell parameters were 22 mA cm-2 short-circuit photocurrent density, 0.41 V open-circuit voltage, 0.35 fill factor, and 3.2% conversion efficiency.

  12. Pyrolysis kinetics of lignocellulosic materials

    SciTech Connect

    Balci, S.; Dogu, T.; Yuecel, H. . Dept. of Chemical Engineering)

    1993-11-01

    Pyrolysis kinetics of almond and hazelnut shells and beech wood were carried out using a thermogravimetric technique. Experiments were repeated for different final pyrolysis temperatures ranging from 300 to 850 C. Approximately 90% of the pyrolysis reactions were completed up to 450 C. The initial values of the activation energy of pyrolysis reaction were found to be around 22 kcal/mol for shells of almond and hazelnut. On the other hand, initial activation energy of beech wood pyrolysis was found as 29.4 kcal/mol. Results indicated that a first-order decomposition in terms of volatile content of the reactant showed good agreement with the data only at the initial stages of the reaction. The reaction rate constant was found to decrease with reaction extent due to the changes in the chemical and physical structure of the solid. Among several models proposed, a model which predicted an increase of activation energy with reaction extent gave the best agreement with the experimental data.

  13. Modifications Of A Commercial Spray Gun

    NASA Technical Reports Server (NTRS)

    Allen, Peter B.

    1993-01-01

    Commercial spray gun modified to increase spray rate and make sprayed coats more nearly uniform. Consists of gun head and pneumatic actuator. Actuator opens valves for two chemical components, called "A" and "B," that react to produce foam. Components flow through orifices, into mixing chamber in head. Mixture then flows through control orifice to spray tip. New spray tip tapered to reduce area available for accumulation of foam and makes tip easier to clean.

  14. Modifications Of A Commercial Spray Gun

    NASA Technical Reports Server (NTRS)

    Allen, Peter B.

    1993-01-01

    Commercial spray gun modified to increase spray rate and make sprayed coats more nearly uniform. Consists of gun head and pneumatic actuator. Actuator opens valves for two chemical components, called "A" and "B," that react to produce foam. Components flow through orifices, into mixing chamber in head. Mixture then flows through control orifice to spray tip. New spray tip tapered to reduce area available for accumulation of foam and makes tip easier to clean.

  15. Pyrolysis Oil Biorefinery.

    PubMed

    Meier, Dietrich

    2017-03-14

    In biorefineries several conversion processes for biomasses may be applied to obtain maximum value from the feed materials. One viable option is the liquefaction of lignocellulosic feedstocks or residues by fast pyrolysis. The conversion technology requires rapid heating of the biomass particles along with rapid cooling of the hot vapors and aerosols. The main product, bio-oil, is obtained in yields of up to 75 wt% on a dry feed basis, together with by-product char and gas which are used within the process to provide the process heat requirements; there are no waste streams other than flue gas and ash. Bio-oils from fast pyrolysis have a great potential to be used as renewable fuel and/or a source for chemical feedstocks. Existing technical reactor designs are presented together with actual examples. Bio-oil characterization and various options for bio-oil upgrading are discussed based on the potential end-use. Existing and potential utilization alternatives for bio-oils are presented with respect to their use for heat and power generation as well as chemical and material use.

  16. Direct determination of arsenic in soil samples by fast pyrolysis-chemical vapor generation using sodium formate as a reductant followed by nondispersive atomic fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Duan, Xuchuan; Zhang, Jingya; Bu, Fanlong

    2015-09-01

    This new study shows for the first time that sodium formate can react with trace arsenic to form volatile species via fast pyrolysis - chemical vapor generation. We found that the presence of thiourea greatly enhanced the generation efficiency and eliminated the interference of copper. We studied the reaction temperature, the volume of sodium formate, the reaction acidity, and the carried argon rate using nondispersive atomic fluorescence spectrometry. Under optimal conditions of T = 500 °C, the volumes of 30% sodium formate and 10% thiourea were 0.2 ml and 0.05 ml, respectively. The carrier argon rate was 300 ml min- 1 and the detection limit and precision of arsenic were 0.39 ng and 3.25%, respectively. The amount of arsenic in soil can be directly determined by adding trace amount of hydrochloric acid as a decomposition reagent without any sample pretreatment. The method was successfully applied to determine trace amount of arsenic in two soil-certified reference materials (GBW07453 and GBW07450), and the results were found to be in agreement with certified reference values.

  17. Regulation for Optimal Liquid Products during Biomass Pyrolysis: A Review

    NASA Astrophysics Data System (ADS)

    Wang, F.; Hu, L. J.; Zheng, Y. W.; Huang, Y. B.; Yang, X. Q.; Liu, C.; Kang, J.; Zheng, Z. F.

    2016-08-01

    The liquid product obtained from biomass pyrolysis is very valuable that it could be used for extraction of chemicals as well as for liquid fuel. The desire goal is to obtain the most bio-oil with desired higher heating value (HHV), high physicochemical stability. The yields and chemical composition of products from biomass pyrolysis are closely related to the feedstock, pyrolysis parameters and catalysts. Current researches mainly concentrated on the co-pyrolysis of different biomass and introduce of novel catalysts as well as the combined effect of catalysts and pyrolysis parameters. This review starts with the chemical composition of biomass and the fundamental parameters and focuses on the influence of catalysts on bio-oil. What is more, the pyrolysis facilities at commercial scales were also involved. The classic researches and the current literature about the yield and composition of products (mainly liquid products) are summarized.

  18. Corrosivity Of Pyrolysis Oils

    SciTech Connect

    Keiser, James R; Bestor, Michael A; Lewis Sr, Samuel Arthur; Storey, John Morse

    2011-01-01

    Pyrolysis oils from several sources have been analyzed and used in corrosion studies which have consisted of exposing corrosion coupons and stress corrosion cracking U-bend samples. The chemical analyses have identified the carboxylic acid compounds as well as the other organic components which are primarily aromatic hydrocarbons. The corrosion studies have shown that raw pyrolysis oil is very corrosive to carbon steel and other alloys with relatively low chromium content. Stress corrosion cracking samples of carbon steel and several low alloy steels developed through-wall cracks after a few hundred hours of exposure at 50 C. Thermochemical processing of biomass can produce solid, liquid and/or gaseous products depending on the temperature and exposure time used for processing. The liquid product, known as pyrolysis oil or bio-oil, as produced contains a significant amount of oxygen, primarily as components of water, carboxylic acids, phenols, ketones and aldehydes. As a result of these constituents, these oils are generally quite acidic with a Total Acid Number (TAN) that can be around 100. Because of this acidity, bio-oil is reported to be corrosive to many common structural materials. Despite this corrosive nature, these oils have the potential to replace some imported petroleum. If the more acidic components can be removed from this bio-oil, it is expected that the oil could be blended with crude oil and then processed in existing petroleum refineries. The refinery products could be transported using customary routes - pipelines, barges, tanker trucks and rail cars - without a need for modification of existing hardware or construction of new infrastructure components - a feature not shared by ethanol.

  19. Thermal and catalytic slow pyrolysis of Calophyllum inophyllum fruit shell.

    PubMed

    Alagu, R M; Sundaram, E Ganapathy; Natarajan, E

    2015-10-01

    Pyrolysis of Calophyllum inophyllum shell was performed in a fixed bed pyrolyser to produce pyrolytic oil. Both thermal (without catalysts) and catalytic pyrolysis process were conducted to investigate the effect of catalysts on pyrolysis yield and pyrolysis oil characteristics. The yield of pyrolytic oil through thermal pyrolysis was maximum (41% wt) at 425 °C for particle size of 1.18 mm and heating rate of 40 °C/min. In catalytic pyrolysis the pyrolytic oil yield was maximum (45% wt) with both zeolite and kaolin catalysts followed by Al2O3 catalyst (44% wt). The functional groups and chemical components present in the pyrolytic oil are identified by Fourier Transform Infrared Spectroscopy (FT-IR) and Gas Chromatography-Mass Spectrometry (GC-MS) techniques. This study found that C. inophyllum shell is a potential new green energy source and that the catalytic pyrolysis process using zeolite catalyst improves the calorific value and acidity of the pyrolytic oil.

  20. Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods: Bio-oil Analytical Standardization

    SciTech Connect

    Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.; Padmaperuma, Asanga B.; Connatser, Raynella M.; Stankovikj, Filip; Meier, Dietrich; Paasikallio, Ville

    2016-07-05

    In this perspective, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. Here, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 degrees C), 31P NMR for determination of hydroxyl groups, and a quantitative gas chromatography-mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to determine metrics for bio-oil quality. Finally, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.

  1. A review of the chemical and physical mechanisms of the storage stability of fast pyrolysis bio-oils

    SciTech Connect

    Diebold, J.P.

    1999-01-27

    Understanding the fundamental chemical and physical aging mechanisms is necessary to learn how to produce a bio-oil that is more stable during shipping and storage. This review provides a basis for this understanding and identifies possible future research paths to produce bio-oils with better storage stability.

  2. Pyrolysis of polymeric materials. I - Effect of chemical structure, temperature, heating rate, and air flow on char yield and toxicity

    NASA Technical Reports Server (NTRS)

    Hilado, C. J.; Casey, C. J.

    1979-01-01

    Various polymeric materials, including synthetic polymers and cellulosic materials, were evaluated at different temperatures, heating rates and air flow rates for thermophysical and toxicological responses. It is shown that char yields appeared to be a function of air access as much as of the chemical structure of the material. It is stated that the sensitivity of the apparent thermal stability of some materials to air access is so marked that thermogravimetric studies in oxygen-free atmospheres may be a consistently misleading approach to comparing synthetic polymers intended to increase fire safety. Toxicity also appeared to be a function of temperature and air access as much as of the chemical structure of the material. Toxicity of the gases evolved seemed to increase with increasing char yield for some polymers.

  3. Pyrolysis of polymeric materials. I - Effect of chemical structure, temperature, heating rate, and air flow on char yield and toxicity

    NASA Technical Reports Server (NTRS)

    Hilado, C. J.; Casey, C. J.

    1979-01-01

    Various polymeric materials, including synthetic polymers and cellulosic materials, were evaluated at different temperatures, heating rates and air flow rates for thermophysical and toxicological responses. It is shown that char yields appeared to be a function of air access as much as of the chemical structure of the material. It is stated that the sensitivity of the apparent thermal stability of some materials to air access is so marked that thermogravimetric studies in oxygen-free atmospheres may be a consistently misleading approach to comparing synthetic polymers intended to increase fire safety. Toxicity also appeared to be a function of temperature and air access as much as of the chemical structure of the material. Toxicity of the gases evolved seemed to increase with increasing char yield for some polymers.

  4. Using different chemical methods for deposition of copper selenide thin films and comparison of their characterization.

    PubMed

    Güzeldir, Betül; Sağlam, Mustafa

    2015-11-05

    Different chemical methods such as Successive Ionic Layer Adsorption and Reaction (SILAR), spin coating and spray pyrolysis methods were used to deposite of copper selenide thin films on the glass substrates. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-ray analysis (EDX) spectroscopy and UV-vis spectrophotometry. The XRD and SEM studies showed that all the films exhibit polycrystalline nature and crystallinity of copper selenide thin films prepared with spray pyrolysis greater than spin coating and SILAR methods. From SEM and AFM images, it was observed copper selenide films were uniform on the glass substrates without any visible cracks or pores. The EDX spectra showed that the expected elements exist in the thin films. Optical absorption studies showed that the band gaps of copper selenide thin films were in the range 2.84-2.93 eV depending on different chemical methods. The refractive index (n), optical static and high frequency dielectric constants (ε0, ε∞) values were calculated by using the energy bandgap values for each deposition method. The obtained results from different chemical methods revealed that the spray pyrolysis technique is the best chemical deposition method to fabricate copper selenide thin films. This absolute advantage was lead to play key roles on performance and efficiency electrochromic and photovoltaic devices. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Analysis of the pyrolysis products of dimethyldichlorosilane in the chemical vapor deposition of silicon carbide in argon

    NASA Technical Reports Server (NTRS)

    Cagliostro, Domenick E.; Riccitiello, Salvatore R.; Carswell, Marty G.

    1990-01-01

    A study of the products and reactions occurring during the chemical vapor deposition of silicon carbide from dimethyldichlorosilane in argon is presented. Reaction conditions were as follows: 700 to 1100 C, a contact time of about 1 min, and a pressure of 1 atm. At these conditions, the gases that formed were mainly methane, hydrogen, silicon tetrachloride, trichlorosilane, and methyltrichlorosilane. The silicon carbide solid that formed showed the presence of hydrogen and chloride as impurities, which might degrade the silicon carbide properties. These impurities were eliminated slowly, even at 1100 C, forming hydrogen, trichlorosilane, and silicon tetrachloride.

  6. Analysis of the pyrolysis products of dimethyldichlorosilane in the chemical vapor deposition of silicon carbide in argon

    NASA Technical Reports Server (NTRS)

    Cagliostro, Domenick E.; Riccitiello, Salvatore R.; Carswell, Marty G.

    1990-01-01

    A study of the products and reactions occurring during the chemical vapor deposition of silicon carbide from dimethyldichlorosilane in argon is presented. Reaction conditions were as follows: 700 to 1100 C, a contact time of about 1 min, and a pressure of 1 atm. At these conditions, the gases that formed were mainly methane, hydrogen, silicon tetrachloride, trichlorosilane, and methyltrichlorosilane. The silicon carbide solid that formed showed the presence of hydrogen and chloride as impurities, which might degrade the silicon carbide properties. These impurities were eliminated slowly, even at 1100 C, forming hydrogen, trichlorosilane, and silicon tetrachloride.

  7. Chemical rate model for the surface pyrolysis of tetrakis(dimethylamido)titanium to form titanium nitride films

    NASA Astrophysics Data System (ADS)

    Toprac, Anthony J.; Iacoponi, John A.; Littau, Karl A.

    1998-09-01

    A chemical kinetic rate model for the deposition of titanium nitride films from the surface reaction of tetrakis(dimethyl-amido)titanium (TDMAT) was developed. Without ammonia addition, TDMAT forms a titanium nitride film by pyrolyzing on the hot substrate surface. Experimental data from the applied materials 5000 deposition tool was modeled using a CSTR formulation. With the parameters of the surface reaction model regressed to fit portions of the experimental results, reasonably accurate model predictions over the entire domain of experimental data were obtained.

  8. Mild pyrolysis of selectively oxidized coals

    SciTech Connect

    Hippo, E.J.

    1991-01-01

    The primary objective of this study is to investigate the removal organic sulfur from selectively oxidized Illinois coals using mild thermal/chemical processes. Work completed this quarter includes the investigation of the mild pyrolysis of unoxidized coals plus a selection of selectively oxidized coals. In addition the effect of particle size and extent of oxidation on pyrolysis was investigated. Some preliminary data concerning pyrolysis under vacuum and ambient pressure was also obtained. Work completed this quarter supports the following conclusions: (1) Desulfurization of unoxidized coals increases with increasing pyrolysis temperature and correlates with the loss of volatile matter. (2) Particle size did not influence the extent of desulfurization significantly. (3) Removing pyrite prior to pyrolysis helps to achieve a lower sulfur product beyond that expected from the removal of pyrite alone. (4) The extent of selective oxidation in teh pretreatment step did not effect the level of desulfurization obtained by pyrolysis alone. However this factor was important in the desulfurization obtained with supercritical methanol (SCM)/base. (5) Up to 84% of the sulfur has been removed from the IBC 101 coal by combining selective oxidation and SCM/base reactions. (6) Evidence for regressive reactions between volatilized sulfur compounds and partially desulfurized products was obtained by studying how changes in pyrolysis pressure effected the product sulfur content.

  9. Pyrolysis of waste tyres: A review

    SciTech Connect

    Williams, Paul T.

    2013-08-15

    Graphical abstract: - Highlights: • Pyrolysis of waste tyres produces oil, gas and char, and recovered steel. • Batch, screw kiln, rotary kiln, vacuum and fluidised-bed are main reactor types. • Product yields are influenced by reactor type, temperature and heating rate. • Pyrolysis oils are complex and can be used as chemical feedstock or fuel. • Research into higher value products from the tyre pyrolysis process is reviewed. - Abstract: Approximately 1.5 billion tyres are produced each year which will eventually enter the waste stream representing a major potential waste and environmental problem. However, there is growing interest in pyrolysis as a technology to treat tyres to produce valuable oil, char and gas products. The most common reactors used are fixed-bed (batch), screw kiln, rotary kiln, vacuum and fluidised-bed. The key influence on the product yield, and gas and oil composition, is the type of reactor used which in turn determines the temperature and heating rate. Tyre pyrolysis oil is chemically very complex containing aliphatic, aromatic, hetero-atom and polar fractions. The fuel characteristics of the tyre oil shows that it is similar to a gas oil or light fuel oil and has been successfully combusted in test furnaces and engines. The main gases produced from the pyrolysis of waste tyres are H{sub 2}, C{sub 1}–C{sub 4} hydrocarbons, CO{sub 2}, CO and H{sub 2}S. Upgrading tyre pyrolysis products to high value products has concentrated on char upgrading to higher quality carbon black and to activated carbon. The use of catalysts to upgrade the oil to a aromatic-rich chemical feedstock or the production of hydrogen from waste tyres has also been reported. Examples of commercial and semi-commercial scale tyre pyrolysis systems show that small scale batch reactors and continuous rotary kiln reactors have been developed to commercial scale.

  10. Chemical compatibility and properties of suspension plasma-sprayed SrTiO3-based anodes for intermediate-temperature solid oxide fuel cells

    NASA Astrophysics Data System (ADS)

    Zhang, Shan-Lin; Li, Cheng-Xin; Li, Chang-Jiu

    2014-10-01

    La-doped strontium titanate (LST) is a promising, redox-stable perovskite material for direct hydrocarbon oxidation anodes in intermediate-temperature solid oxide fuel cells (IT-SOFCs). In this study, nano-sized LST and Sm-doped ceria (SDC) powders are produced by the sol-gel and glycine-nitrate processes, respectively. The chemical compatibility between LST and electrolyte materials is studied. A LST-SDC composite anode is prepared by suspension plasma spraying (SPS). The effects of annealing conditions on the phase structure, microstructure, and chemical stability of the LST-SDC composite anode are investigated. The results indicate that the suspension plasma-sprayed LST-SDC anode has the same phase structure as the original powders. LST exhibits a good chemical compatibility with SDC and Mg/Sr-doped lanthanum gallate (LSGM). The anode has a porosity of ∼40% with a finely porous structure that provides high gas permeability and a long three-phase boundary for the anode reaction. Single cells assembled with the LST-SDC anode, La0.8Sr0.2Ga0.8Mg0.2O3 electrolyte, and La0.8Sr0.2CoO3-SDC cathode show a good performance at 650-800 °C. The annealing reduces the impedances due to the enhancement in the bonding between the particles in the anode and interface of anode and LSGM electrolyte, thus improving the output performance of the cell.

  11. Review of NMR characterization of pyrolysis oils

    DOE PAGES

    Hao, Naijia; Ben, Haoxi; Yoo, Chang Geun; ...

    2016-08-24

    Here, pyrolysis of renewable biomass has been developed as a method to produce green fuels and chemicals in response to energy security concerns as well as to alleviate environmental issues incurred with fossil fuel usage. However, pyrolysis oils still have limited commercial application, mainly because unprocessed oils cannot be readily blended with current petroleum-based transportation fuels. To better understand these challenges, researchers have applied diverse characterization techniques in the development of bio-oil studies. In particular, nuclear magnetic resonance (NMR) is a key spectroscopic characterization method through analysis of bio-oil components. This review highlights the NMR strategies for pyrolysis oil characterizationmore » and critically discusses the applications of 1H, 13C, 31P, 19F, and two-dimensional (2-D NMR) analyses such as heteronuclear single quantum correlation (HSQC) in representative pyrolysis oil studies.« less

  12. Review of NMR characterization of pyrolysis oils

    SciTech Connect

    Hao, Naijia; Ben, Haoxi; Yoo, Chang Geun; Adhikari, Sushil; Ragauskas, Arthur J.

    2016-08-24

    Here, pyrolysis of renewable biomass has been developed as a method to produce green fuels and chemicals in response to energy security concerns as well as to alleviate environmental issues incurred with fossil fuel usage. However, pyrolysis oils still have limited commercial application, mainly because unprocessed oils cannot be readily blended with current petroleum-based transportation fuels. To better understand these challenges, researchers have applied diverse characterization techniques in the development of bio-oil studies. In particular, nuclear magnetic resonance (NMR) is a key spectroscopic characterization method through analysis of bio-oil components. This review highlights the NMR strategies for pyrolysis oil characterization and critically discusses the applications of 1H, 13C, 31P, 19F, and two-dimensional (2-D NMR) analyses such as heteronuclear single quantum correlation (HSQC) in representative pyrolysis oil studies.

  13. Review of NMR characterization of pyrolysis oils

    SciTech Connect

    Hao, Naijia; Ben, Haoxi; Yoo, Chang Geun; Adhikari, Sushil; Ragauskas, Arthur J.

    2016-08-24

    Here, pyrolysis of renewable biomass has been developed as a method to produce green fuels and chemicals in response to energy security concerns as well as to alleviate environmental issues incurred with fossil fuel usage. However, pyrolysis oils still have limited commercial application, mainly because unprocessed oils cannot be readily blended with current petroleum-based transportation fuels. To better understand these challenges, researchers have applied diverse characterization techniques in the development of bio-oil studies. In particular, nuclear magnetic resonance (NMR) is a key spectroscopic characterization method through analysis of bio-oil components. This review highlights the NMR strategies for pyrolysis oil characterization and critically discusses the applications of 1H, 13C, 31P, 19F, and two-dimensional (2-D NMR) analyses such as heteronuclear single quantum correlation (HSQC) in representative pyrolysis oil studies.

  14. Tuning of properties of sprayed CuZnS films

    NASA Astrophysics Data System (ADS)

    Sreejith, M. S.; Deepu, D. R.; Kartha, C. Sudha; Vijayakumar, K. P.

    2014-04-01

    CuZnS is an alloy having mixed structure of CuxS and ZnS. Here we studied the structural, optical, compositional and electrical properties of CuZnS films prepared using chemical spray pyrolysis (CSP). Just by varying ratio of Cu to Zn was observed that material can be changed from P type to N type and electrical conductivity can be increased by 4 orders. Increase in concentration of Cu leads to decrease bandgap to 1.8 eV from 3.4 eV. CuZnS films having high concentration of copper can be used as good absorber and weakly doped films as buffer / window layers in solar cells.

  15. Paper spray mass spectrometry applied in the monitoring of a chemical system in dynamic chemical equilibrium: the redox process of methylene blue.

    PubMed

    de Paula, Camila Cristina Almeida; Valadares, Alberto; Jurisch, Marina; Piccin, Evandro; Augusti, Rodinei

    2016-05-15

    The monitoring of chemical systems in dynamic equilibrium is not an easy task. This is due to the high rate at which the system returns to equilibrium after being perturbed, which hampers the possibility of following the aftereffects of the disturbance. In this context, it is necessary to use a fast analytical technique that requires no (or minimal) sample preparation, and which is capable of monitoring the species constituting the system in equilibrium. Paper spray ionization mass spectrometry (PS-MS), a recently introduced ambient ionization technique, has such characteristics and hence was chosen for monitoring a model system: the redox process of methylene blue. The model system evaluated herein was composed of three cationic species of methylene blue (MB), which coexist in a dynamic redox system: (1) [MB](+) of m/z 284 (cationic MB); (2) [MB + H + e](+•) of m/z 285 (the protonated form of a transient species resulting from the reduction of [MB](+) ); (3) [MB + 2H + 2e](+) or [leuco-MB + H](+) of m/z 286 (the protonated leuco form of MB). Aliquots of a MB solution were collected before and after the addition of a reducing agent (metallic zinc) and directly analyzed by PS-MS for identification of the predominant cationic species at different conditions. The mass spectra revealed that before the addition of the reducing agent the ion of m/z 284 (cationic MB) is the unique species. Upon the addition of the reducing agent and acid, however, the solution continuously undergo discoloration while reduced species derived directly from cationic MB (m/z 285 and 286) are detected in the mass spectra with increasing intensities. Fragmentation patterns obtained for each ionic species, i.e. [MB](+) , [MB + H + e](+•) and [leuco-MB + H](+) , shown to be consistent with the proposed structures. The PS-MS technique proved to be suitable for an in situ and 'near' real-time analysis of the dynamic equilibrium involving the redox of MB in aqueous medium. The data clearly

  16. Solid-state stability of spray-dried insulin powder for inhalation: chemical kinetics and structural relaxation modeling of Exubera above and below the glass transition temperature.

    PubMed

    Sadrzadeh, Negar; Miller, Danforth P; Lechuga-Ballesteros, David; Harper, Nancy J; Stevenson, Cynthia L; Bennett, David B

    2010-09-01

    The effect of temperature on the chemical stability of an amorphous spray-dried insulin powder formulation (Exubera) was evaluated in the solid state at constant moisture content. The chemical stability of the powder was assessed using reversed-phase high-performance liquid chromatography (RP-HPLC) and high-performance-size exclusion chromatography (HP-SEC). The major degradants in spray-dried insulin produced during heat stressing were identified as A21-desamidoinsulin (A21) and high molecular weight protein (HMWP). As expected, the rates of formation of A21 and HMWP were observed to increase with temperature. A stretched-time kinetic model (degradation rate is proportional to the square root of time) was applied to the degradant profiles above and below the glass transition temperature (T(g)) and apparent reaction rate constants were determined. Below T(g), isothermal enthalpy of relaxation measurements were used to assess the effect of temperature on molecular mobility. The formation of A21 and HMWP was found to follow an Arrhenius temperature dependence above and below the T(g). Comparison of reaction rate constants to those estimated from structural relaxation experiments suggests that the reaction pathways to form A21 and HMWP below the T(g) may be coupled with the molecular motions involved in structural relaxation.

  17. Surface characteristic of chemically converted graphene coated low carbon steel by electro spray coating method for polymer electrolyte membrane fuel cell bipolar plate.

    PubMed

    Kim, Jungsoo; Kim, Yang Do; Nam, Dae Geun

    2013-05-01

    Graphene was coated on low carbon steel (SS400) by electro spray coating method to improve its properties of corrosion resistance and contact resistance. Exfoliated graphite was made of the graphite by chemical treatment (Chemically Converted Graphene, CCG). CCG is distributed using dispersing agent, and low carbon steel was coated with diffuse graphene solution by electro spray coating method. The structure of the CCG was analyzed using XRD and the coating layer of surface was analyzed using SEM. Analysis showed that multi-layered graphite structure was destroyed and it was transformed in to fine layers graphene structure. And the result of SEM analysis on the surface and the cross section, graphene layer was uniformly formed with 3-5 microm thickness on the surface of substrate. Corrosion resistance test was applied in the corrosive solution which is similar to the polymer electrolyte membrane fuel cell (PEMFC) stack inside. And interfacial contact resistance (ICR) test was measured to simulate the internal operating conditions of PEMFC stack. As a result of measuring corrosion resistance and contact resistance, it could be confirmed that low carbon steel coated with CCG was revealed to be more effective in terms of its applicability as PEMFC bipolar plate.

  18. Plasma-sprayed coatings

    SciTech Connect

    Herman, H.

    1988-09-01

    Plasma spraying is one way to apply protective coatings. The hot, high-speed flame of a plasma gun can melt a powder of almost any ceramic or metal and spray it to form a coating for protection against corrosion, wear or high temperature. The technique carries much less risk of degrading the coating and substrate than many other high-temperature processes do, because the gas in the plasma flame is chemically inert and the target can be kept fairly cool. And yet a plasma gun can be only a little more cumbersome than a paint sprayer. Investigators are applying this technique to new materials. The General Electric Company is using vacuum plasma spraying to make freestanding components: intricate aircraft engine parts formed by plasma-spraying a superalloy on a removable substrate. Other workers spray ceramic particles or fibers and metal powder simulatious wrong, stiff composite materials: the ceramic particles dispersed in a matrix of metal. The author and colleagues at the U.S. Naval Research Laboratory have fabricated a thick film of high-temperature superconductor by plasma-spraying the compound in the form of a powder. 7 figs.

  19. Spray atomization of bio-oil/ethanol blends with externally mixed nozzles

    USDA-ARS?s Scientific Manuscript database

    Experiments were conducted to investigate the properties of sprays of pyrolysis oil from biomass (bio-oil) using an air assisted atomization nozzle operated without combustion to explore the potential of pyrolysis oil combustion in industrial and home furnaces. Bio-oil was blended with ethanol to im...

  20. Fundamental Pyrolysis Studies

    SciTech Connect

    Milne, T. A.; Evans, R. J.; Soltys, M. N.

    1983-03-01

    Progress on the direct mass spectrometric sampling of pyrolysis products from wood and its constituents is described for the period from June 1982 to February 1983. A brief summary and references to detailed reports, of the qualitative demonstration of our approach to the study of the separated processes of primary and secondary pyrolysis is presented. Improvements and additions to the pyrolysis and data acquisition systems are discussed and typical results shown. Chief of these are a heated-grid pyrolysis system for controlled primary pyrolysis and a sheathed flame arrangement for secondary cracking studies. Qualitative results of the secondary cracking of cellulose, lignin, and wood are shown as are comparisons with the literature for the pyrolysis spectra of cellulose, lignin, and levoglucosan. 'Fingerprints' for a number of materials are shown, with spectra taken under carefully controlled conditions so that sensitivity calibrations for different compounds, now being determined, can be applied.

  1. Structural analysis of pyrolytic lignins isolated from switchgrass fast pyrolysis oil

    USDA-ARS?s Scientific Manuscript database

    Structural characterization of lignin extracted from the bio-oil produced by fast pyrolysis of switchgrass (Panicum virgatum) is reported. This new information is important to understanding the utility of lignin as a chemical feedstock in a pyrolysis based biorefinery. Pyrolysis induces a variety of...

  2. Charcoal from the pyrolysis of rapeseed plant straw-stalk

    SciTech Connect

    Karaosmanoglu, F.; Tetik, E.

    1999-07-01

    Charcoal is an important product of pyrolysis of biomass sources. Charcoal can be used for domestic, agricultural, metallurgical, and chemical purposes. In this study different characteristics of charcoal, one of the rape seed plant straw-stalk pyrolysis product, was researched and presented as candidates.

  3. Preparation, properties, and bonding utilization of pyrolysis bio-oil

    USDA-ARS?s Scientific Manuscript database

    The rapid increase in energy consumption, limited fossil fuel resource, and environmental concerns have stimulated the research need for biomass-derived fuels and chemicals. Pyrolysis is a thermal degradation process of biomass in the absence of oxygen. The liquid product from pyrolysis is known as ...

  4. Adding value to ethanol production byproducts through microwave assisted pyrolysis

    USDA-ARS?s Scientific Manuscript database

    The aim of this project is to increase the value of distillers grain by utilizing it as a feedstock for microwave assisted pyrolysis (MAP). Pyrolysis is the chemical/thermal conversion of biomass without the presence of oxygen into newly formed products: gases, liquids and solids. This conversion pr...

  5. Influence of Pyrolysis Temperature on Physico-Chemical Properties of Corn Stover (Zea mays L.) Biochar and Feasibility for Carbon Capture and Energy Balance

    PubMed Central

    Rafiq, Muhammad Khalid; Bachmann, Robert Thomas; Rafiq, Muhammad Tariq; Shang, Zhanhuan; Joseph, Stephen; Long, Ruijun

    2016-01-01

    This study examined the influence of pyrolysis temperature on biochar characteristics and evaluated its suitability for carbon capture and energy production. Biochar was produced from corn stover using slow pyrolysis at 300, 400 and 500°C and 2 hrs holding time. The experimental biochars were characterized by elemental analysis, BET, FTIR, TGA/DTA, NMR (C-13). Higher heating value (HHV) of feedstock and biochars was measured using bomb calorimeter. Results show that carbon content of corn stover biochar increased from 45.5% to 64.5%, with increasing pyrolysis temperatures. A decrease in H:C and O:C ratios as well as volatile matter, coupled with increase in the concentration of aromatic carbon in the biochar as determined by FTIR and NMR (C-13) demonstrates a higher biochar carbon stability at 500°C. It was estimated that corn stover pyrolysed at 500°C could provide of 10.12 MJ/kg thermal energy. Pyrolysis is therefore a potential technology with its carbon-negative, energy positive and soil amendment benefits thus creating win- win scenario. PMID:27327870

  6. Influence of Pyrolysis Temperature on Physico-Chemical Properties of Corn Stover (Zea mays L.) Biochar and Feasibility for Carbon Capture and Energy Balance.

    PubMed

    Rafiq, Muhammad Khalid; Bachmann, Robert Thomas; Rafiq, Muhammad Tariq; Shang, Zhanhuan; Joseph, Stephen; Long, Ruijun

    2016-01-01

    This study examined the influence of pyrolysis temperature on biochar characteristics and evaluated its suitability for carbon capture and energy production. Biochar was produced from corn stover using slow pyrolysis at 300, 400 and 500°C and 2 hrs holding time. The experimental biochars were characterized by elemental analysis, BET, FTIR, TGA/DTA, NMR (C-13). Higher heating value (HHV) of feedstock and biochars was measured using bomb calorimeter. Results show that carbon content of corn stover biochar increased from 45.5% to 64.5%, with increasing pyrolysis temperatures. A decrease in H:C and O:C ratios as well as volatile matter, coupled with increase in the concentration of aromatic carbon in the biochar as determined by FTIR and NMR (C-13) demonstrates a higher biochar carbon stability at 500°C. It was estimated that corn stover pyrolysed at 500°C could provide of 10.12 MJ/kg thermal energy. Pyrolysis is therefore a potential technology with its carbon-negative, energy positive and soil amendment benefits thus creating win- win scenario.

  7. Supercritical Fuel Pyrolysis

    DTIC Science & Technology

    2010-05-30

    experiments are conducted in the isothermal , isobaric reactor designed expressly for such purposes by Davis [22] and used by Stewart [11,12] in the AFOSR... isothermal , isobaric reactor specially designed for such purposes, we have conducted supercritical pyrolysis experiments with three model fuels: 1...prevalent understanding of how these different component groups behave under pyrolysis conditions. Clearly we need to know more about the pyrolysis

  8. Catalytic partial oxidation of pyrolysis oils

    NASA Astrophysics Data System (ADS)

    Rennard, David Carl

    2009-12-01

    This thesis explores the catalytic partial oxidation (CPO) of pyrolysis oils to syngas and chemicals. First, an exploration of model compounds and their chemistries under CPO conditions is considered. Then CPO experiments of raw pyrolysis oils are detailed. Finally, plans for future development in this field are discussed. In Chapter 2, organic acids such as propionic acid and lactic acid are oxidized to syngas over Pt catalysts. Equilibrium production of syngas can be achieved over Rh-Ce catalysts; alternatively mechanistic evidence is derived using Pt catalysts in a fuel rich mixture. These experiments show that organic acids, present in pyrolysis oils up to 25%, can undergo CPO to syngas or for the production of chemicals. As the fossil fuels industry also provides organic chemicals such as monomers for plastics, the possibility of deriving such species from pyrolysis oils allows for a greater application of the CPO of biomass. However, chemical production is highly dependent on the originating molecular species. As bio oil comprises up to 400 chemicals, it is essential to understand how difficult it would be to develop a pure product stream. Chapter 3 continues the experimentation from Chapter 2, exploring the CPO of another organic functionality: the ester group. These experiments demonstrate that equilibrium syngas production is possible for esters as well as acids in autothermal operation with contact times as low as tau = 10 ms over Rh-based catalysts. Conversion for these experiments and those with organic acids is >98%, demonstrating the high reactivity of oxygenated compounds on noble metal catalysts. Under CPO conditions, esters decompose in a predictable manner: over Pt and with high fuel to oxygen, non-equilibrium products show a similarity to those from related acids. A mechanism is proposed in which ethyl esters thermally decompose to ethylene and an acid, which decarbonylates homogeneously, driven by heat produced at the catalyst surface. Chapter 4

  9. DRIFTSIM, A Computer Program for Estimating Spray Drift Distances

    USDA-ARS?s Scientific Manuscript database

    One of the severe problems with spraying pesticides is the spray drift. Drift is a problem if chemicals are sprayed too close to residential areas, livestock facilities, bodies of water, or sensitive crops. Complaints regarding spray drift are routinely brought to state departments of agriculture,...

  10. Pyrolysis system evaluation study

    NASA Technical Reports Server (NTRS)

    1974-01-01

    An evaluation of two different pyrolysis concepts which recover energy from solid waste was conducted in order to determine the merits of each concept for integration into a Integrated Utility System (IUS). The two concepts evaluated were a Lead Bath Furnace Pyrolysis System and a Slagging Vertical Shaft, Partial Air Oxidation Pyrolysis System. Both concepts will produce a fuel gas from the IUS waste and sewage sludge which can be used to offset primary fuel consumption in addition to the sanitary disposal of the waste. The study evaluated the thermal integration of each concept as well as the economic impact on the IUS resulting from integrating each pyrolysis concepts. For reference, the pyrolysis concepts were also compared to incineration which was considered the baseline IUS solid waste disposal system.

  11. Physico-chemical properties and gasification reactivity of co-pyrolysis char from different rank of coal blended with lignocellulosic biomass: Effects of the cellulose.

    PubMed

    Wu, Zhiqiang; Wang, Shuzhong; Luo, Zhengyuan; Chen, Lin; Meng, Haiyu; Zhao, Jun

    2017-07-01

    In this paper, the influence of cellulose on the physicochemical properties and the gasification reactivity of co-pyrolysis char was investigated. A specific surface area analyzer and an X-ray diffraction system were used to characterize the pore structure and the micro-crystalline structure of char. Fractal theory and deconvolution method were applied to quantitatively investigate the influence of cellulose on the structure of co-pyrolysis char. The results indicate that the improvements in the pore structure due to the presence of cellulose are more pronounced in the case of anthracite char with respect to bituminous char. Cellulose promotes the ordering of micro-scale structure and the uniformity of both anthracite and bituminous char, while the negative synergetic effect was observed during gasification of co-pyrolysis char. The exponential relationships between fractal dimension and specific surface area were determined, along with the relations between the gasification reactivity index and the microcrystalline structure parameter. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Pyrolysis and catalytic pyrolysis as a recycling method of waste CDs originating from polycarbonate and HIPS

    SciTech Connect

    Antonakou, E.V.; Kalogiannis, K.G.; Stephanidis, S.D.; Triantafyllidis, K.S.; Lappas, A.A.; Achilias, D.S.

    2014-12-15

    Highlights: • Thermal and catalytic pyrolysis is a powerful method for recycling of WEEEs. • Liquid products obtained from the pyrolysis of PC or HIPS found in waste CDs are very different. • Mainly phenols are obtained from pyrolysis PC based wastes while aromatics from HIPS. • Use of MgO catalyst increases the amount of phenols from CD recycling compared to ZSM-5. • Use of MgO or ZSM-5 catalysts reduces the amount of styrene recovered from HIPS. - Abstract: Pyrolysis appears to be a promising recycling process since it could convert the disposed polymers to hydrocarbon based fuels or various useful chemicals. In the current study, two model polymers found in WEEEs, namely polycarbonate (PC) and high impact polystyrene (HIPS) and their counterparts found in waste commercial Compact Discs (CDs) were pyrolysed in a bench scale reactor. Both, thermal pyrolysis and pyrolysis in the presence of two catalytic materials (basic MgO and acidic ZSM-5 zeolite) was performed for all four types of polymers. Results have shown significant recovery of the monomers and valuable chemicals (phenols in the case of PC and aromatic hydrocarbons in the case of HIPS), while catalysts seem to decrease the selectivity towards the monomers and enhance the selectivity towards other desirable compounds.

  13. Synthesis, Characterization and Decomposition Studies of Tris(N,N-dibenzyldithiocarbamato) Indium(III): Chemical Spray Deposition of Polycrystalline CuInS2 on Copper Films

    NASA Technical Reports Server (NTRS)

    Hehemann, David G.; Lau, J. Eva; Harris, Jerry D.; Hoops, Michael D.; Duffy, Norman V.; Fanwick, Philip E.; Khan, Osman; Jin, Michael H.-C.; Hepp, Aloysius F.

    2005-01-01

    Tris(bis(phenylmethyl)carbamodithioato-S,S ), commonly referred to as tris(N,Ndibenzyldithiocarbamato) indium(III), In(S2CNBz2)3, was synthesized and characterized by single crystal X-ray crystallography. The compound crystallizes in the triclinic space group P1 bar with two molecules per unit cell. The material was further characterized using a novel analytical system employing the combined powers of thermogravimetric analysis, gas chromatography/mass spectrometry and Fourier-Transform infrared spectroscopy to investigate its potential use as a precursor for the chemical vapor deposition (CVD) of thin film materials for photovoltaic applications. Upon heating, the material thermally decomposes to release CS2 and benzyl moieties in to the gas phase, resulting in bulk In2S3. Preliminary spray CVD experiments indicate that In(S2CNBz2)3 decomposed on a Cu substrate reacts to produce stoichiometric CuInS2 films.

  14. Characteristics of vanadium-doped indium oxide thin films for organic light-emitting diodes fabricated by spray chemical vapor deposition

    NASA Astrophysics Data System (ADS)

    Seki, Yoshiyuki; Seki, Shigeyuki; Hoshi, Yoichi; Uchida, Takayuki; Sawada, Yutaka

    2015-04-01

    An indium oxide transparent electrode for organic light-emitting diodes was fabricated by the inexpensive spray chemical vapor deposition method. The high work function (5.1 eV) necessary for a transparent anode and a hole-injection layer was successfully achieved with a vanadium doping concentration of 1.5 at. % V without any significant increase in resistivity and surface roughness or loss of transparency. The effect of vanadium doping on indium oxide was systematically investigated. The resistivity, average transmittance in the visible range, and surface roughness (Ra) were 1.08 × 10-3 Ω·cm, 84%, and 4.0 nm, respectively, for the vanadium-doped indium oxide.

  15. Facile spray-coating process for the fabrication of tunable adhesive superhydrophobic surfaces with heterogeneous chemical compositions used for selective transportation of microdroplets with different volumes.

    PubMed

    Li, Jian; Jing, Zhijiao; Zha, Fei; Yang, Yaoxia; Wang, Qingtao; Lei, Ziqiang

    2014-06-11

    In this paper, tunable adhesive superhydrophobic ZnO surfaces have been fabricated successfully by spraying ZnO nanoparticle (NP) suspensions onto desired substrates. We regulate the spray-coating process by changing the mass percentage of hydrophobic ZnO NPs (which were achieved by modifying hydrophilic ZnO NPs with stearic acid) in the hydrophobic/hydrophilic ZnO NP mixtures to control heterogeneous chemical composition of the ZnO surfaces. Thus, the water adhesion on the same superhydrophobic ZnO surface could be effectively tuned by controlling the surface chemical composition without altering the surface morphology. Compared with the conventional tunable adhesive superhydrophobic surfaces, on which there were only three different water sliding angle values: lower than 10°, 90° (the water droplet is firmly pinned on the surface at any tilted angles), and the value between the two ones, the water adhesion on the superhydrophobic ZnO surfaces has been tuned effectively, on which the sliding angle is controlled from 2 ± 1° to 9 ± 1°, 21 ± 2°, 39 ± 3°, and 90°. Accordingly, the adhesive force can be adjusted from extremely low (∼2.5 μN) to very high (∼111.6 μN). On the basis of the different adhesive forces of the tunable adhesive superhydrophobic surfaces, the selective transportation of microdroplets with different volumes was achieved, which has never been reported before. In addition, we demonstrated a proof of selective transportation of microdroplets with different volumes for application in the droplet-based microreactors via our tunable adhesive superhydrophobic surfaces for the quantitative detection of AgNO3 and NaOH. The results reported herein realize the selective transportation of microdroplets with different volumes and we believe that this method would potentially be used in many important applications, such as selective water droplet transportation, biomolecular quantitative detection and droplet-based biodetection.

  16. Comparison of the hazards posed to amphibians by the glyphosate spray control program versus the chemical and physical activities of coca production in Colombia.

    PubMed

    Brain, Richard A; Solomon, Keith R

    2009-01-01

    This study evaluates the cumulative multifactorial physical and chemical impacts resulting from coca production on amphibian populations in comparison with the potential impacts produced by the herbicide glyphosate (Glyphos), which, mixed with the surfactant Cosmo-Flux, is used in the spray control program for illicit crops in Colombia. Using similar worst-case assumptions for exposure, several other pesticides used for coca production, including mancozeb, lambda cyhalothrin, endosulfan, diazinon, malathion, and chlorpyrifos, were up to 10- to 100-fold more toxic to frogs than the Glyphos-Cosmo-Flux mixture. Comparing hazard quotients based on application rates, several of these compounds demonstrated hazards 3-383 times that of formulated glyphosate. Secondary effects, particularly of insecticides, are also a concern, as these agents selectively target the primary food source of amphibians, which may indirectly impact growth and development. Although the potential chemical impacts by other pesticides are considerable, physical activities associated with coca production, particularly deforestation of primary forests for new coca plots, portend the greatest hazard to amphibian populations. The entire production cycle of cocaine has been linked to ecosystem degradation. The clearing of pristine forests for coca propagation in Colombia is well documented, and some of these regions coincide with those that contain exceptional amphibian biodiversity. This is particularly problematic as coca production encroaches more deeply into more remote areas of tropical rain forest. Transportation of disease, including the chitrid fungus, to these remote regions via human intrusion may also adversely affect amphibian populations. Therefore, the cumulative impacts of coca production, through habitat destruction, application of agrochemicals, and potential transmission of disease, are judged to pose greater risks to amphibian populations in coca-growing regions than the glyphosate

  17. Stabilization of Fast Pyrolysis Oil: Post Processing Final Report

    SciTech Connect

    Elliott, Douglas C.; Lee, Suh-Jane; Hart, Todd R.

    2012-03-01

    UOP LLC, a Honeywell Company, assembled a comprehensive team for a two-year project to demonstrate innovative methods for the stabilization of pyrolysis oil in accordance with DOE Funding Opportunity Announcement (FOA) DE-PS36-08GO98018, Biomass Fast Pyrolysis Oil (Bio-oil) Stabilization. In collaboration with NREL, PNNL, the USDA Agricultural Research Service (ARS), Pall Fuels and Chemicals, and Ensyn Corporation, UOP developed solutions to the key technical challenges outlined in the FOA. The UOP team proposed a multi-track technical approach for pyrolysis oil stabilization. Conceptually, methods for pyrolysis oil stabilization can be employed during one or both of two stages: (1) during the pyrolysis process (In Process); or (2) after condensation of the resulting vapor (Post-Process). Stabilization methods fall into two distinct classes: those that modify the chemical composition of the pyrolysis oil, making it less reactive; and those that remove destabilizing components from the pyrolysis oil. During the project, the team investigated methods from both classes that were suitable for application in each stage of the pyrolysis process. The post processing stabilization effort performed at PNNL is described in this report. The effort reported here was performed under a CRADA between PNNL and UOP, which was effective on March 13, 2009, for 2 years and was subsequently modified March 8, 2011, to extend the term to December 31, 2011.

  18. Hydrous pyrolysis of pole treating chemicals: (a) initital measurement of hydrous pyrolysis rates for napthalene and pentachlorophenol; (b) solubility of flourene at temperatures up to 150{degrees}C

    SciTech Connect

    Leif, R. N., LLNL

    1997-11-15

    The temperature dependencies of the hydrous pyrolysis/oxidation (HPO) aqueous phase oxidation reactions of naphthalene and pentachlorophenol have been determined for phosphate buffered systems using Dickson-type reaction vessels. The HPO experimental temperatures ranged from 114{degrees}C to 148{degrees}C for naphthalene and 114{degrees}C to 137{degrees}C for pentachlorophenol. The loss of the organic species was used to determine activation energies of 95.8 kJ/mole for naphthalene oxidation and 84.8 kJ/mole for pentachlorophenol oxidation. Aqueous concentrations of target compounds and reaction intermediates were determined by gas chromatography and compound identification was verified by gas chromatography - mass spectrometry. During the experiments the pollutants were completely mineralized, as indicated by a stoichiometric production of inorganic carbon in the case of naphthalene and inorganic carbon and chloride in the case of pentachlorophenol. HPO of pentachlorophenol produced 2,3,5,6- tetrachlorophenol as an intermediate, whereas no intermediates amenable by GC were observed during the HPO of naphthalene. Measurements of the aqueous solubility of florin in an unbuffered solution have been made covering the temperature range from 20{degrees}C to 150{degrees}C. There is very good agreement between this data set and data previously published covering the lower temperature range (20{degrees}C to 75{degrees}C). Extension of the solubility measurements to higher temperatures covers the in situ temperatures achievable during field application of HPO and demonstrated a nearly exponential rise in aqueous solubility as a function of temperature, with a 10 fold increase in aqueous florin solubility going from 75{degrees}C to 125{degrees}C and a 20 fold increase in going from 75{degrees}C to 150{degrees}C.

  19. Pyrolysis of lipids using various catalysts

    USDA-ARS?s Scientific Manuscript database

    A specific pursuit of the thermochemical (combustion, gasification, pyrolysis, and liquefaction) conversion of biomass to energy research effort is the potential of converting lipids to alkanes, petroleum-like fuels and chemicals. Arguments can be made for, and against, the use of agricultural lipi...

  20. Mineral nutrient recovery from pyrolysis systems

    USDA-ARS?s Scientific Manuscript database

    Bioenergy crops such as high-energy sorghum (HES), bioenergy rice, corn stover, and switchgrass can be thermo-chemically converted by pyrolysis to produce bio-oil, synthesis gas from non-condensable gases, and biochar. The biochar fraction can be recycled back to the production field to improve soil...

  1. Pyrolysis with cyclone burner

    DOEpatents

    Green, Norman W.; Duraiswamy, Kandaswamy; Lumpkin, Robert E.

    1978-07-25

    In a continuous process for recovery of values contained in a solid carbonaceous material, the carbonaceous material is comminuted and then subjected to flash pyrolysis in the presence of a particulate heat source over an overflow weir to form a pyrolysis product stream containing a carbon containing solid residue and volatilized hydrocarbons. After the carbon containing solid residue is separated from the pyrolysis product stream, values are obtained by condensing volatilized hydrocarbons. The particulate source of heat is formed by oxidizing carbon in the solid residue and separating out the fines.

  2. Pyrolysis with staged recovery

    DOEpatents

    Green, Norman W.; Duraiswamy, Kandaswamy; Lumpkin, Robert E.; Winter, Bruce L.

    1979-03-20

    In a continuous process for recovery of values contained in a solid carbonaceous material, the carbonaceous material is comminuted and then subjected to flash pyrolysis in the presence of a particulate heat source fed over an overflow weir to form a pyrolysis product stream containing a carbon containing solid residue and volatilized hydrocarbons. After the carbon containing solid residue is separated from the pyrolysis product stream, values are obtained by condensing volatilized hydrocarbons. The particulate source of heat is formed by oxidizing carbon in the solid residue.

  3. Study of fundamental chemical processes in explosive decomposition by laser-powered homogeneous pyrolysis. Final report 1 jul 78-31 aug 81

    SciTech Connect

    McMillen, D.F.; Golden, D.M.

    1981-11-12

    Very Low-Pressure Pyrolysis studies of 2,4-dinitrotoluene decomposition resulted in decomposition rates consistent with log (ks) = 12.1 - 43.9/2.3 RT. These results support the conclusion that previously reported 'anomalously' low Arrhenius parameters for the homogeneous gas-phase decomposition of ortho-nitrotoluene actually represent surface-catalyzed reactions. Preliminary qualitative results for pyrolysis of ortho-nitrotouene in the absence of hot reactor walls, using the Laser-Powered Homogeneous Pyrolysis technique (LPHP), provide further support for this conclusion: only products resulting from Ph-NO2 bond scission were observed; no products indicating complex intramolecular oxidation-reduction or elimination processes could be detected. The LPHP technique was successfully modified to use a pulsed laser and a heated flow system, so that the technique becomes suitable for study of surface-sensitive, low vapor pressure substrates such as TNT. The validity and accuracy of the technique was demonstrated by applying it to the decomposition of substances whose Arrhenius parameters for decomposition were already well known. IR-fluorescence measurements show that the temperature-space-time behavior under the present LPHP conditions is in agreement with expectations and with requirements which must be met if the method is to have quantitative validity. LPHP studies of azoisopropane decomposition, chosen as a radical-forming test reaction, show the accepted literature parameters to be substantially in error and indicate that the correct values are in all probability much closer to those measured in this work: log (k/s) = 13.9 - 41.2/2.3 RT.

  4. Sprayed ZnO as effective window layer for CIS/CdS solar cell

    NASA Astrophysics Data System (ADS)

    Sreejith, M. S.; Deepu, D. R.; Kartha, C. Sudha; Vijayakumar, K. P.

    2014-01-01

    Thin film solar cells were fabricated using CuInS2 as absorber layer and CdS as buffer layer. CuInS2 and CdS layers are deposited using chemical spray pyrolysis and chemical bath deposition respectively. Proper movement and collection of generated carriers really affect the performance of the cell. Introduction of a very thin layer of silver doped ZnO (ZnO:Ag) window layer between the buffer layer and ITO improves performance of the cell, with open circuit voltage of 409mV, short circuit current density of 2.89 mA/cm2, fill factor of 44.3% and conversion efficiency of 0.52%.

  5. Behavior of chlorine during coal pyrolysis

    USGS Publications Warehouse

    Shao, D.; Hutchinson, E.J.; Cao, H.; Pan, W.-P.; Chou, C.-L.

    1994-01-01

    The behavior of chlorine in Illinois coals during pyrolysis was evaluated by combined thermo-gravimetry-Fourier transform infrared spectroscopy-ion chromatography (TG-FTIR-IC) techniques. It was found that more than 90% of chlorine in Illinois coals (IBC-103, 105, 106, and 109) was liberated as HCl gas during pyrolysis from 300 to 600??C, with the rate reaching a maximum at 440 ??C. Similarity of the HCl and NH3 release profiles during pyrolysis of IBC-109 supports the hypothesis that the chlorine in coal may be associated with nitrogen and the chlorine is probably bonded to the basic nitrogen sites on the inner walls of coal micropores. ?? 1994 American Chemical Society.

  6. Combustion Properties of Biomass Flash Pyrolysis Oils: Final Project Report

    SciTech Connect

    C. R. Shaddix; D. R. Hardesty

    1999-04-01

    Thermochemical pyrolysis of solid biomass feedstocks, with subsequent condensation of the pyrolysis vapors, has been investigated in the U.S. and internationally as a means of producing a liquid fuel for power production from biomass. This process produces a fuel with significantly different physical and chemical properties from traditional petroleum-based fuel oils. In addition to storage and handling difficulties with pyrolysis oils, concern exists over the ability to use this fuel effectively in different combustors. The report endeavors to place the results and conclusions from Sandia's research into the context of international efforts to utilize pyrolysis oils. As a special supplement to this report, Dr. Steven Gust, of Finland's Neste Oy, has provided a brief assessment of pyrolysis oil combustion research efforts and commercialization prospects in Europe.

  7. Indium Doped Zinc Oxide Thin Films Deposited by Ultrasonic Chemical Spray Technique, Starting from Zinc Acetylacetonate and Indium Chloride

    PubMed Central

    Biswal, Rajesh; Maldonado, Arturo; Vega-Pérez, Jaime; Acosta, Dwight Roberto; Olvera, María De La Luz

    2014-01-01

    The physical characteristics of ultrasonically sprayed indium-doped zinc oxide (ZnO:In) thin films, with electrical resistivity as low as 3.42 × 10−3 Ω·cm and high optical transmittance, in the visible range, of 50%–70% is presented. Zinc acetylacetonate and indium chloride were used as the organometallic zinc precursor and the doping source, respectively, achieving ZnO:In thin films with growth rate in the order of 100 nm/min. The effects of both indium concentration and the substrate temperature on the structural, morphological, optical, and electrical characteristics were measured. All the films were polycrystalline, fitting well with hexagonal wurtzite type ZnO. A switching in preferential growth, from (002) to (101) planes for indium doped samples were observed. The surface morphology of the films showed a change from hexagonal slices to triangle shaped grains as the indium concentration increases. Potential applications as transparent conductive electrodes based on the resulting low electrical resistance and high optical transparency of the studied samples are considered. PMID:28788118

  8. Indium Doped Zinc Oxide Thin Films Deposited by Ultrasonic Chemical Spray Technique, Starting from Zinc Acetylacetonate and Indium Chloride.

    PubMed

    Biswal, Rajesh; Maldonado, Arturo; Vega-Pérez, Jaime; Acosta, Dwight Roberto; De La Luz Olvera, María

    2014-07-04

    The physical characteristics of ultrasonically sprayed indium-doped zinc oxide (ZnO:In) thin films, with electrical resistivity as low as 3.42 × 10(-3) Ω·cm and high optical transmittance, in the visible range, of 50%-70% is presented. Zinc acetylacetonate and indium chloride were used as the organometallic zinc precursor and the doping source, respectively, achieving ZnO:In thin films with growth rate in the order of 100 nm/min. The effects of both indium concentration and the substrate temperature on the structural, morphological, optical, and electrical characteristics were measured. All the films were polycrystalline, fitting well with hexagonal wurtzite type ZnO. A switching in preferential growth, from (002) to (101) planes for indium doped samples were observed. The surface morphology of the films showed a change from hexagonal slices to triangle shaped grains as the indium concentration increases. Potential applications as transparent conductive electrodes based on the resulting low electrical resistance and high optical transparency of the studied samples are considered.

  9. Formate-assisted pyrolysis

    DOEpatents

    DeSisto, William Joseph; Wheeler, Marshall Clayton; van Heiningen, Adriaan R. P.

    2015-03-17

    The present invention provides, among other thing, methods for creating significantly deoxygenated bio-oils form biomass including the steps of providing a feedstock, associating the feedstock with an alkali formate to form a treated feedstock, dewatering the treated feedstock, heating the dewatered treated feedstock to form a vapor product, and condensing the vapor product to form a pyrolysis oil, wherein the pyrolysis oil contains less than 30% oxygen by weight.

  10. Gas chromatography/mass spectrometry and pyrolysis-gas chromatography/mass spectrometry for the chemical characterisation of modern and archaeological figs (Ficus carica).

    PubMed

    Ribechini, Erika; Pérez-Arantegui, Josefina; Colombini, Maria Perla

    2011-06-24

    Gas chromatography/mass spectrometry (GC/MS) after alkaline hydrolysis, solvent extraction and trimethylsilylation, and analytical pyrolysis using hexamethyldisilazane (HMDS) for in situ derivatisation followed by gas chromatographic/mass spectrometric analysis (Pyrolysis-silylation-GC/MS) were used to investigate the hydrolysable and soluble constituents, and the polymerised macromolecules of an archaeological fig (Ficus carica) recovered in Zaragoza (Spain), as well as of modern figs. The main aim was to study the compositional alterations undergone by the fig tissues in a particular archaeological environment: the fig was in a vessel and covered by a layer of a mixture of orpiment and gypsum. A comparison between the GC/MS results from modern and archaeological figs revealed that degradative reactions took place, leading to the disappearance/depletion of reactive (unsaturated fatty acids) and sensitive compounds (phytosterols and triterpenes). Py-silylation-GC/MS data provided evidence of a significant degradation of the saccharide and lipid components of the fig tissue, which left a residue enriched in polyphenols and polyesters. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Pyrolysis and catalytic pyrolysis as a recycling method of waste CDs originating from polycarbonate and HIPS.

    PubMed

    Antonakou, E V; Kalogiannis, K G; Stephanidis, S D; Triantafyllidis, K S; Lappas, A A; Achilias, D S

    2014-12-01

    Pyrolysis appears to be a promising recycling process since it could convert the disposed polymers to hydrocarbon based fuels or various useful chemicals. In the current study, two model polymers found in WEEEs, namely polycarbonate (PC) and high impact polystyrene (HIPS) and their counterparts found in waste commercial Compact Discs (CDs) were pyrolysed in a bench scale reactor. Both, thermal pyrolysis and pyrolysis in the presence of two catalytic materials (basic MgO and acidic ZSM-5 zeolite) was performed for all four types of polymers. Results have shown significant recovery of the monomers and valuable chemicals (phenols in the case of PC and aromatic hydrocarbons in the case of HIPS), while catalysts seem to decrease the selectivity towards the monomers and enhance the selectivity towards other desirable compounds.

  12. Relationship between hydrous and ordinary pyrolysis

    SciTech Connect

    Burnham, A.K.

    1993-06-01

    Pyrolysis results are reviewed briefly with the intent of drawing comparisons between open, high pressure, and hydrous pyrolysis. Empirically, the degree of pyrolysis severity to form volatile products in open pyrolysis is similar to that required to form an expelled oil phase in hydrous pyrolysis. The yields of hydrocarbons from open pyrolysis are close to those from hydrous pyrolysis, but hydrous pyrolysis tends to assist the separation of hydrocarbons from polar materials. Pressure has a small but measurable affect on the generation kinetics.

  13. BGRcast: A Disease Forecast Model to Support Decision-making for Chemical Sprays to Control Bacterial Grain Rot of Rice.

    PubMed

    Lee, Yong Hwan; Ko, Sug-Ju; Cha, Kwang-Hong; Park, Eun Woo

    2015-12-01

    A disease forecast model for bacterial grain rot (BGR) of rice, which is caused by Burkholderia glumae, was developed in this study. The model, which was named 'BGRcast', determined daily conduciveness of weather conditions to epidemic development of BGR and forecasted risk of BGR development. All data that were used to develop and validate the BGRcast model were collected from field observations on disease incidence at Naju, Korea during 1998-2004 and 2010. In this study, we have proposed the environmental conduciveness as a measure of conduciveness of weather conditions for population growth of B. glumae and panicle infection in the field. The BGRcast calculated daily environmental conduciveness, Ci , based on daily minimum temperature and daily average relative humidity. With regard to the developmental stages of rice plants, the epidemic development of BGR was divided into three phases, i.e., lag, inoculum build-up and infection phases. Daily average of Ci was calculated for the inoculum build-up phase (Cinf ) and the infection phase (Cinc ). The Cinc and Cinf were considered environmental conduciveness for the periods of inoculum build-up in association with rice plants and panicle infection during the heading stage, respectively. The BGRcast model was able to forecast actual occurrence of BGR at the probability of 71.4% and its false alarm ratio was 47.6%. With the thresholds of Cinc = 0.3 and Cinf = 0.5, the model was able to provide advisories that could be used to make decisions on whether to spray bactericide at the pre- and post-heading stage.

  14. BGRcast: A Disease Forecast Model to Support Decision-making for Chemical Sprays to Control Bacterial Grain Rot of Rice

    PubMed Central

    Lee, Yong Hwan; Ko, Sug-Ju; Cha, Kwang-Hong; Park, Eun Woo

    2015-01-01

    A disease forecast model for bacterial grain rot (BGR) of rice, which is caused by Burkholderia glumae, was developed in this study. The model, which was named ‘BGRcast’, determined daily conduciveness of weather conditions to epidemic development of BGR and forecasted risk of BGR development. All data that were used to develop and validate the BGRcast model were collected from field observations on disease incidence at Naju, Korea during 1998–2004 and 2010. In this study, we have proposed the environmental conduciveness as a measure of conduciveness of weather conditions for population growth of B. glumae and panicle infection in the field. The BGRcast calculated daily environmental conduciveness, Ci, based on daily minimum temperature and daily average relative humidity. With regard to the developmental stages of rice plants, the epidemic development of BGR was divided into three phases, i.e., lag, inoculum build-up and infection phases. Daily average of Ci was calculated for the inoculum build-up phase (Cinf) and the infection phase (Cinc). The Cinc and Cinf were considered environmental conduciveness for the periods of inoculum build-up in association with rice plants and panicle infection during the heading stage, respectively. The BGRcast model was able to forecast actual occurrence of BGR at the probability of 71.4% and its false alarm ratio was 47.6%. With the thresholds of Cinc = 0.3 and Cinf = 0.5, the model was able to provide advisories that could be used to make decisions on whether to spray bactericide at the pre- and post-heading stage. PMID:26672893

  15. High-resolution mass spectrometric analysis of biomass pyrolysis vapors

    DOE PAGES

    Christensen, Earl; Evans, Robert J.; Carpenter, Daniel

    2017-01-19

    Vapors generated from the pyrolysis of lignocellulosic biomass are made up of a complex mixture of oxygenated compounds. Direct analysis of these vapors provides insight into the mechanisms of depolymerization of cellulose, hemicellulose, and lignin as well as insight into reactions that may occur during condensation of pyrolysis vapors into bio-oil. Studies utilizing pyrolysis molecular beam mass spectrometry have provided valuable information regarding the chemical composition of pyrolysis vapors. Mass spectrometers generally employed with these instruments have low mass resolution of approximately a mass unit. The presence of chemical species with identical unit mass but differing elemental formulas cannot bemore » resolved with these instruments and are therefore detected as a single ion. In this study we analyzed the pyrolysis vapors of several biomass sources using a high-resolution double focusing mass spectrometer. High-resolution analysis of pyrolysis vapors allowed for speciation of several compounds that would be detected as a single ion with unit mass resolution. Lastly, these data not only provide greater detail into the composition of pyrolysis vapors but also highlight differences between vapors generated from multiple biomass feedstocks.« less

  16. Flash vacuum pyrolysis of lignin model compounds

    SciTech Connect

    Cooney, M.J.; Britt, P.F.; Buchanan, A.C. III

    1997-03-01

    Despite the extensive research into the pyrolysis of lignin, the underlying chemical reactions that lead to product formation are poorly understood. Detailed mechanistic studies on the pyrolysis of biomass and lignin under conditions relevant to current process conditions could provide insight into utilizing this renewable resource for the production of chemicals and fuel. Currently, flash or fast pyrolysis is the most promising process to maximize the yields of liquid products (up to 80 wt %) from biomass by rapidly heating the substrate to moderate temperatures, typically 500{degrees}C, for short residence times, typically less than two seconds. To provide mechanistic insight into the primary reaction pathways under process relevant conditions, we are investigating the flash vacuum pyrolysis (FVP) of lignin model compounds that contain a {beta}-ether. linkage and {alpha}- or {gamma}-alcohol, which are key structural elements in lignin. The dominant products from the FVP of PhCH{sub 2}CH{sub 2}OPh (PPE), PhC(OH)HCH{sub 2}OPh, and PhCH{sub 2}CH(CH{sub 2}OH)OPh at 500{degrees}C can be attributed to homolysis of the weakest bond in the molecule (C-O bond) or 1,2-elimination. Surprisingly, the hydroxy-substituent dramatically increases the decomposition of PPE. It is proposed that internal hydrogen bonding is accelerating the reaction.

  17. Recent developments in fast pyrolysis of ligno-cellulosic materials.

    PubMed

    Kersten, Sascha; Garcia-Perez, Manuel

    2013-06-01

    Pyrolysis is a thermochemical process to convert ligno-cellulosic materials into bio-char and pyrolysis oil. This oil can be further upgraded or refined for electricity, transportation fuels and chemicals production. At the time of writing, several demonstration factories are considered worldwide aiming at maturing the technology. Research is focusing on understanding the underlying processes at all relevant scales, ranging from the chemistry of cell wall deconstruction to optimization of pyrolysis factories, in order to produce better quality oils for targeted uses. Among the several bio-oil applications that are currently investigated the production and fermentation of pyrolytic sugars explores the promising interface between thermochemistry and biotechnology.

  18. Catalytic pyrolysis of plastic wastes - Towards an economically viable process

    SciTech Connect

    McIntosh, M.J.; Arzoumanidis, G.G.; Brockmeier, F.E.

    1996-07-01

    The ultimate goal of our project is an economically viable pyrolysis process to recover useful fuels and/or chemicals from plastics- containing wastes. This paper reports the effects of various promoted and unpromoted binary oxide catalysts on yields and compositions of liquid organic products, as measured in a small laboratory pyrolysis reactor. On the basis of these results, a commercial scale catalytic pyrolysis reactor was simulated by the Aspen software and rough costs were estimated. The results suggest that such a process has potential economic viability.

  19. Effects of feedstock characteristics on microwave-assisted pyrolysis - A review.

    PubMed

    Zhang, Yaning; Chen, Paul; Liu, Shiyu; Peng, Peng; Min, Min; Cheng, Yanling; Anderson, Erik; Zhou, Nan; Fan, Liangliang; Liu, Chenghui; Chen, Guo; Liu, Yuhuan; Lei, Hanwu; Li, Bingxi; Ruan, Roger

    2017-04-01

    Microwave-assisted pyrolysis is an important approach to obtain bio-oil from biomass. Similar to conventional electrical heating pyrolysis, microwave-assisted pyrolysis is significantly affected by feedstock characteristics. However, microwave heating has its unique features which strongly depend on the physical and chemical properties of biomass feedstock. In this review, the relationships among heating, bio-oil yield, and feedstock particle size, moisture content, inorganics, and organics in microwave-assisted pyrolysis are discussed and compared with those in conventional electrical heating pyrolysis. The quantitative analysis of data reported in the literature showed a strong contrast between the conventional processes and microwave based processes. Microwave-assisted pyrolysis is a relatively new process with limited research compared with conventional electrical heating pyrolysis. The lack of understanding of some observed results warrant more and in-depth fundamental research. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Catalytic pyrolysis of palm kernel shell waste in a fluidized bed.

    PubMed

    Kim, Sung Won; Koo, Bon Seok; Lee, Dong Hyun

    2014-09-01

    The catalytic pyrolysis of palm kernel shell was investigated in a fluidized bed with zsm-5 and equilibrium FCC (Ecat) catalysts. Catalytic pyrolysis oil yields were remarkably reduced and gas yields were increased due to the higher catalytic reaction of primary volatiles compared to non-catalytic pyrolysis. Char yields were affected by temperature and the pore structure of the catalysts. The pyrolysis oil was characterized by lower H/C and O/C molar ratios due to aromatization and deoxygenation of volatiles by the catalysts. The catalytic pyrolysis oils contained more oxygen and nitrogen and less sulfur than petroleum oils. The oils had a high concentration of nitriles, with a carbon number distribution similar to fatty acids. The catalytic pyrolysis oils featured high nitriles yield with Ecat and high aromatics yield in the light fraction with zsm-5, due to characteristics of the catalyst. The catalytic pyrolysis oils showed potentials as feedstocks for bio-diesel and chemicals.