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  • 1.
    Anselmo, Ana Sofia
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Rysz, Jakub
    M. Smoluchowski Insitute of Physics, Jagiellonian University, Reymonta 4, Krakow 30–059, Poland.
    Bernasik, Andrzej
    Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, Krakow 30–059, Poland.
    Budkowski, Andrzej
    M. Smoluchowski Insitute of Physics, Jagiellonian University, Reymonta 4, Krakow 30–059, Poland.
    Andersson, Mats R.
    Department of Chemical and Biological Engineering, Chalmers University of Technology.
    van Stam, Jan
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Characterisation of vertical phase separation in polymer: fullerene blend films for photovoltaics by dSIMS and NEXAFS2011In: E-MRS 2011 Spring Meeting: Bilateral Energy Conference, Malden, MA: John Wiley & Sons, 2011, p. 62-63Conference paper (Refereed)
    Abstract [en]

    Morphological control and characterization of blend films is key in the development of viable polymer solar cells. Spontaneous formation of vertical compositional gradients during solution processing has been shown for polyfluorene:PCBM blends and rationalized with thermodynamic and kinetic models of nucleation and spinodal decomposition.[1, 2] The extent of vertical stratification is affected by polymer side-chain modification aimed at controlling polymer:fullerene miscibility.[3] Here we present high-resolution film morphology results for several polymer:fullerene systems as obtained from near-edge X-ray fine structure spectroscopy (NEXAFS) in partial and in total electron yield modes. Blend films were found to be polymer- enriched at the surface. Dynamic secondary ion mass spectrometry (dSIMS) and NEXAFS give compositional information at different depths, resulting in a more complete picture of the film morphology.

     

  • 2.
    Anselmo, Ana Sofia
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Rysz, Jakub
    M. Smoluchowski Insitute of Physics, Jagiellonian University, Reymonta 4, Krakow 30–059, Poland.
    Budkowski, Andrzej
    M. Smoluchowski Insitute of Physics, Jagiellonian University, Reymonta 4, Krakow 30–059, Poland.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    van Stam, Jan
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Polymer solar cells: Visualizing vertical phase separation in solution-processed films of polymer fullerene blends2012In: Proceedings of the 5th International Symposium Technologies for Polymer Electronics - TPE 12 / [ed] Hans-Klaus Roth, Klaus Heinemann, Ilmenau, Germany: Universitätsverlag Ilmenau , 2012, p. 125-128Conference paper (Refereed)
  • 3.
    Anselmo, Ana Sofia
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Molecular Orientation and Composition at the Surface of Spin-Coated Polyfluorene:Fullerene Blend Films2013In: Journal of Polymer Science Part B: Polymer Physics, ISSN 0887-6266, E-ISSN 1099-0488, Vol. 51, no 3, p. 176-182Article in journal (Refereed)
    Abstract [en]

    The surface composition in spin-coated films of polyfluorene:fullerene blends was determined quantitatively by near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. By comparing partial and total electron yield spectra, we found vertical compositional differences in the surface region. Furthermore, the orientation of the polymer chains was investigated by variable-angle NEXAFS. Blend films of poly[(9,9-dioctylfluorenyl-2,7-diyl)-co-5,5-(4′,7′-di-2-thienyl-2′,1′,3′-benzothiadiazole] with [6,6]-phenyl-C61-butyric acid methyl ester in two different blend ratios were studied. Results showed polymer enrichment of the surfaces for films with a polymer:fullerene weight ratio of 20:80 and of 50:50, spin-coated from both chlorobenzene and chloroform solutions. The angular dependence of the NEXAFS spectra of the pure polymer films showed a preferential plane-on orientation, which was slightly stronger in the subsurface region than at the surface. In blend films, this orientational preference was less pronounced and the difference between surface and subsurface vanished

  • 4.
    Anselmo, Ana Sofia
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Health, Science and Technology (starting 2013), Department of Engineering and Physics (from 2013).
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Photodegradation of the electronic structure of PCBM and C60 films in air2016In: Chemical Physics Letters, ISSN 0009-2614, E-ISSN 1873-4448, Vol. 652, p. 220-224Article in journal (Refereed)
    Abstract [en]

    Fullerenes are common electron acceptors in organic solar cells. Here the photostability in air of the electronic structures of spin-coated PCBM ([6,6]-phenyl-C61-butyric acid methyl ester) and evaporated C60 films are studied using ultraviolet photoelectron spectroscopy (UPS) and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. After exposing these materials in air to simulated sunlight, the filled and empty molecular orbitals are strongly altered, indicating that the conjugated π-system of the C60-cage has degraded. Even a few minutes in normal lab light induces changes. These results stress the importance of protecting fullerene-based films from light and air during processing, operation, and storage.

  • 5.
    Anselmo, Ana Sofia
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Wang, Ergang
    Department of Chemical and Biological Engineering, Chalmers University of Technology.
    Andersson, Mats R.
    Department of Chemical and Biological Engineering, Chalmers University of Technology.
    Hörmann, Ulrich
    Institute of Physics, Augsburg University.
    Opitz, Andreas
    Institute of Physics, Augsburg University.
    van Stam, Jan
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Surface Organization in Thin-Films of Conjugated Polymers for Organic Photovoltaics2011Conference paper (Other academic)
  • 6.
    Anselmo, Ana Sofia
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Wang, Ergang
    Chalmers University of Technology.
    Andersson, Mats R.
    Chalmers University of Technology.
    van Stam, Jan
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Molecular orientation and composition at the surface of APFO3:PCBM blend films2012In: Hybrid and Organics Photovoltaics Conference: Uppsala, Sweden, 2012 / [ed] Anders Hagfeldt, SEFIN, Castelló (Spain), 2012, p. 278-Conference paper (Refereed)
  • 7.
    Brumboiu, Iulia
    et al.
    Department of Physics and Astronomy, Uppsala University.
    Anselmo, Ana Sofia
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Brena, Barbara
    Department of Physics and Astronomy, Uppsala University.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Near-edge X-ray Absorption Fine Structure Study of the C60-derivative PCBM2013In: Chemical Physics Letters, ISSN 0009-2614, E-ISSN 1873-4448, Vol. 568-569, p. 130-134Article in journal (Refereed)
    Abstract [en]

    The fullerene derivative [6,6]-phenyl-C61-butyric acid methyl ester plays a key role for electron transport in polymer solar cells. We have studied the unoccupied molecular orbitals of PCBM by near edge X-ray absorption fine structure spectroscopy and were able to assign the main resonances to molecular moieties by comparison with calculated sum spectra of individual carbons. We analyzed specifically the origin of the high-energy shoulder to the first π-resonance and identified contributions from the lowest-energy transition of a specific carbon in the phenyl and from transitions to higher unoccupied orbitals of the unmodified carbons in the C60-cage.

  • 8.
    Dzwilewski, Andrzej
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Anselmo, Ana Sofia
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    The effect of light exposure on P3HT:PCBM films: a NEXAFS study2011Conference paper (Refereed)
    Abstract [en]

    A simple photolithography method was developed for patterning organic field effect transistors (OFETs) prepared from blends of poly(3-hexylthiophene), P3HT, and [6,6]-phenyl-C61-butyric acid methyl ester, PCBM.(1) This Photo-induced and Resist-free Imprint patterning (PRI) technique allows also the single solution step production of organic CMOS circuits.(2) It consists of two subsequent processing steps: 1) exposure: photo-irradiation of the P3HT:PCBM blend by visible laser light and 2) development: rinsing of the film in an organic solvent mixture that is selective for PCBM. As a result, two electronically different materials are obtained, i.e. the exposed and developed (ED) material, and the unexposed and developed (UD) material. The method is based on the modification of the PCBM component in the irradiated area, which becomes effectively insoluble in the solvent mixture, while the PCBM in the non-irradiated area is removed during development. Therefore, we expect that the UD material is pure P3HT, a hypothesis that is confirmed by the p-type conductivity of the ED region. Near-Edge X-ray Absorption Fine Structure spectroscopy (NEXAFS) was used to determine the surface composition of these films. C K-edge NEXAFS spectra of pristine, photo-exposed, and developed blend films, as well as films of the pure components were measured at the synchrotron facility MAX-lab in Lund, Sweden. The spectra for P3HT and PCBM are significantly different and the components can be clearly distinguished in the blend spectra. From the relative intensities of the P3HT and PCBM peaks, the actual blend composition can be estimated, both on the surface, using partial electron yield (PEY), and deeper in the sub-surface region of the film, using total electron yield (TEY). From the similarity of the spectra of the UD blend sample and the pure P3HT sample, we conclude that the remaining material after washing the pristine blend is indeed P3HT, and the ED blend sample retains its two-component character. The surface composition of the blend films is significantly more polymer-rich than the bulk blend ratio used to prepare the film. Both for the pristine blend and the photo-exposed blend differences are observed between the PEY and TEY spectra, indicating the existence of a polymer-enriched surface. Such gradients in thin films of P3HT:PCBM blends have been observed by others using variable-angle spectroscopic ellipsometry,(3) NEXAFS,(4) and neutron reflectometry,(5) and also in other polymer:PCBM blends by dynamic secondary ion mass spectrometry (d-SIMS).(6)

    References (1) Dzwilewski, A.; Wagberg, T.; Edman, L. J. Am. Chem.Soc. 2009, 131, 4006. (2) Dzwilewski, A.; Matyba, P.; Edman, L. J. Phys. Chem. B 2010, 114, 135. (3) Campoy-Quiles, M., et al., Nature Materials 2008, 7,158-164 (4) Germack,D.S. et al., Appl. Phys. Lett. 2009, 94, 233303. (5) Kiel, J.W. et al., Soft Matter 2010, 6, 641-646. (6) Björström, C.M. et al, J. Phys.: Condens. Matter 2005, 17, L529-L534.

  • 9.
    Dzwilewski, Andrzej
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Anselmo, Ana Sofia
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Light induced effects in PCBM:P3HT blend films2012In: Hybrid and Organics Photovoltaics Conference: Uppsala, Sweden, 2012 / [ed] Anders Hagfeldt, SEFIN, Castelló (Spain), 2012, p. 155-155Conference paper (Refereed)
  • 10.
    Dzwilewski, Andrzej
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Anselmo, Ana Sofia
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Zharnikov, Michael
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    X-ray absorption study of light induced effects in PCBM:P3HT blend films2011In: Photovoltaics at the nanoscale: Hasselt University (Belgium) 24-28 October 2011, Hasselt University, Belgium, 2011, p. 59-59Conference paper (Refereed)
  • 11.
    Heidkamp, Hannah
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Rogowski, Rafal
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    van Stam, Jan
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Carlsson, Gunilla
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Morphology of polymer blends in films made by dip-coating2011Conference paper (Refereed)
    Abstract [en]

    Thin spincoated polymer films are used in various applications and there has been anincreasing demand to understand and get precise control over the film formation process. One of the most exciting applications is organic solar cells which have an active layer made of a polymer based blend. The film morphology has a strong effect on the efficiency of solar cells and therefore it is crucial to understand the film formation process in order to tailor thedesired morphology [1].

    In this study we are combining and comparing results from three different deposition processes: drop-casting, sphere-on-flat arrangement and dip-coating. We are using dip-coating to produce thin films of polymer blends with different morphologies under controlled conditions. The main goal is to gain a deeper insight into the processes that occur while solvent evaporates and to understand why certain structures are formed.

    Drop-casting allows for little control of the structure formation. In the sphere-on-flat arrangement a droplet of a solution is constrained between a half-sphere and the substrate, which provides more controllable conditions for the deposition process. For more precise control, dip-coating can be used, where a substrate is withdrawn from a solution at a constant speed.

    In this study we have used the polymer poly(3-hexylthiophene) (P3HT) and the fullerene derivative [6,6]-phenyl-C61-butyric acid methyl ester (PCBM) dissolved in toluene. These components are the model system for studies on organic solar cells [1]. The dip-coated films show a wide variety of morphologies depending on the coating speed. This dependence can be rationalized by the different mechanisms occurring at low and high speeds: At low speeds, evaporation is dominant, [2] resulting in well ordered patterns. At high speeds, viscous forces become dominant, [2] yielding optically homogeneous films.

    [1] G. Dennler, M. C. Scharber, C. J. Brabec, Adv. Mat. 21, 1323-1338 (2009)

    [2] R. Z. Rogowski and A. A. Darhuber, Langmuir 26, 11485-93 (2010)

  • 12.
    Heidkamp, Hannah
    et al.
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    van Stam, Jan
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Carlsson, Gunilla
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Rogowski, Rafal
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Morphology of P3HT and PCBM blends in thin films obtained with different deposition methods2011Conference paper (Refereed)
    Abstract [en]

    Patterns and structures, formed when a semiconducting polymer blend in solution is subject to controlled evaporation, have been of great interest due to their influence on the performance of organic devices. By controlling the processes of pattern formation, function properties of organic semiconductor structures can be tailored, allowing for facile manufacturing of the active layers in organic devices, e.g. solar cells.

    By analyzing the morphologies of polymer blends resulting from different deposition methods, a deeper insight into the pattern formation process can be acquired. In this study, we have analyzed the morphology of blends of poly(3-hexylthiophene) (P3HT) and [6,6]-phenyl-C61-butyric acid methyl ester (PCBM) formed upon solvent evaporation. We used the following deposition methods: dip-coating, droplet evaporation within a constrained geometry and drop-casting. Dip-coated films revealed various types of morphology depending on the coating speed. At low coating speeds, where evaporation is the dominant factor, well-ordered patterns were obtained. When increasing the coating speed, viscous forces become dominant over evaporation yielding optically homogenous films [2]. Morphologically similar structures to those observed at low coating speeds, were also obtained with spatially constrained droplets. The blend morphologies were analyzed with polarized, fluorescence and atomic force microscopy [1].

    References:

    [1] C. M. Björström Svanström, J. Rysz, A. Bernasik, A. Budkowski, F. Zhang, O. Inganäs, M. R. Andersson, K. O. Magnusson, J. J. Benson-Smith, J. Nelson, and E. Moons, Adv. Mat. 21, 4398-4403 (2009)

    [2] R. Z. Rogowski and A. A. Darhuber, Langmuir 26, 11485-93 (2010)

  • 13.
    Moons, Ellen
    et al.
    Karlstad University, Faculty of Technology and Science, Materials Science. Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Anselmo, Ana Sofia
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Svensson, Krister
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    van Stam, Jan
    Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
    Vertical Phase Separation in Polymer:Fullerene Films for Photovoltaics2012In: Hybrid and Organics Photovoltaics Conference 2012: Uppsala, Sweden, 6th to 9th May 2012 / [ed] Anders Hagfeldt, Castelló, Spain: Society for Nanomolecular Photovoltaics (SEFIN) , 2012, p. 53-53Conference paper (Refereed)
  • 14.
    Talyzin, Alexandr
    et al.
    Department of Physics, Umeå University.
    Luzan, S.M.
    Department of Physics, Umeå University.
    Leifer, Klaus
    Division for Electron Microscopy and Nanoengineering, Department of Engineering Sciences, The Ångström Laboratory, Uppsala University, Box 534, SE-75121 Uppsala, Sweden.
    Akhtar, S.
    Division for Electron Microscopy and Nanoengineering, Department of Engineering Sciences, The Ångström Laboratory, Uppsala University, Box 534, SE-75121 Uppsala, Sweden.
    Fetzer, J
    Fetzpahs Consulting, P.O. Box 942, Pinole, California 94564, United States.
    Cataldo, F
    Istituto Nazionale di Astrofisica .
    Tsybin, Y.O.
    Biomolecular Mass Spectrometry Laboratory, Ecole Polytechnique Federale de Lausanne, 1015 Lausanne, Switzerland.
    Tai, C.W.
    Department of Materials and Environmental Chemistry, Stockholm University, S-106 91 Stockholm, Sweden.
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering.
    Moons, Ellen
    Karlstad University, Faculty of Technology and Science, Department of Physics and Electrical Engineering. Karlstad University, Faculty of Technology and Science, Materials Science.
    Coronene fusion by heat treatment: Road to nanographenes2011In: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 115, no 27, p. 13207-13214Article in journal (Refereed)
    Abstract [en]

    The reactions of coronene dehydrogenation and fusion upon heat treatment in the temperature range of 500700 C were studied using XRD, TEM, Raman, IR, and NEXAFS spectroscopy. The formation of a coronene dimer (dicoronylene) was observed at temperatures 530-550 C; dicoronylene can easily be separated using sublimation with a temperature gradient. An insoluble and not sublimable black precipitate was found to form at higher temperatures. Analysis of the data shows that dimerization of coronene is followed at 550600 C by oligomerization into larger molecules. Above 600 C amorphization of the material and formation of graphitic nanoparticles was observed. Coronene fusion by annealing is proposed as a road to synthesis of larger polycyclic aromatic hydrocarbons and nanographenes.

  • 15.
    Talyzin, Alexandr V.
    et al.
    Umea Univ, Dept Phys, SE-90187 Umea, Sweden..
    Luzan, Serhiy
    Umea Univ, Dept Phys, SE-90187 Umea, Sweden..
    Anoshkin, Ilya V.
    Aalto Univ, Dept Appl Phys, FI-00076 Espoo, Finland..
    Nasibulin, Albert G.
    Aalto Univ, Dept Appl Phys, FI-00076 Espoo, Finland..
    Kauppinnen, Esko I.
    Aalto Univ, Dept Appl Phys, FI-00076 Espoo, Finland..
    Dzwilewski, Andrzej
    Karlstad University, Faculty of Health, Science and Technology (starting 2013), Department of Engineering and Physics (from 2013).
    Kreta, Ahmed
    Natl Inst Chem, Ljubljana 1000, Slovenia..
    Jamnik, Janko
    Natl Inst Chem, Ljubljana 1000, Slovenia..
    Hassanien, Abdou
    Natl Inst Chem, Ljubljana 1000, Slovenia..
    Lundstedt, Anna
    Uppsala Univ, Dept Chem BMC, SE-75123 Uppsala, Sweden..
    Grennberg, Helena
    Uppsala Univ, Dept Chem BMC, SE-75123 Uppsala, Sweden..
    Hydrogen-Driven Cage Unzipping of C-60 into Nano-Graphenes2014In: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 118, no 12, p. 6504-6513Article in journal (Refereed)
    Abstract [en]

    Annealing of C-60 in hydrogen at temperatures above the stability limit of C H bonds in C60Hx (500-550 degrees C) is found to result in direct collapse of the cage structure, evaporation of light hydrocarbons, and formation of solid mixture composed of larger hydrocarbons and few-layered graphene sheets. Only a minor part of this mixture is soluble; this was analyzed using matrix-assisted laser desorption/ionization MS, Fourier transform infrared (FTIR), and nuclear magnetic resonance spectroscopy and found to be a rather complex mixture of hydrocarbon molecules composed of at least tens of different compounds. The sequence of most abundant peaks observed in MS, which corresponds to C2H2 mass difference, suggests a stepwise breakup of the fullerene cage into progressively smaller molecular fragments edge-terminated by hydrogen. A simple model of hydrogen-driven C-60 unzipping is proposed to explain the observed sequence of fragmentation products. The insoluble part of the product mixture consists of large planar polycyclic aromatic hydrocarbons, as evidenced by FTIR and Raman spectroscopy, and some larger sheets composed of few-layered graphene, as observed by transmission electron microscopy. Hydrogen annealing of C-60 thin films showed a thickness-dependent results with reaction products significantly different for the thinnest films compared to bulk powders. Hydrogen annealing of C-60 films with the thickness below 10 nm was found to result in formation of nanosized islands with Raman spectra very similar to the spectra of coronene oligomers and conductivity typical for graphene.

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