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  • 1. Dulebohn, Joel I.
    et al.
    Haefner, Steven C.
    Berglund, Kris
    Dunbar, Kim R.
    Reversible carbon monoxide addition to sol-gel derived composite films containing a cationic rhodium(I) complex: towards the development of a new class of molecule-based carbon monoxide sensors1992In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 4, no 3, p. 506-508Article in journal (Refereed)
  • 2.
    Dunuwila, Dilum D.
    et al.
    Michigan State University.
    Gagliardi, Charles D.
    Michigan State University.
    Berglund, Kris
    Application of controlled hydrolysis of titanium(IV) isopropoxide to produce sol-gel-derived thin films1994In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 6, no 9, p. 1556-1562Article in journal (Refereed)
    Abstract [en]

    A variety of porous optically transparent titanium carboxylate films that can be supported on silicate glass substrates have been developed. These films were made by spin casting polymeric solutions of titanium carboxylates processed using sol-gel techniques. The stability and the quality of these films have been qualitatively correlated to the extent of control of hydrolysis exerted by carboxylate modification of the precursor titanium(IV) isopropoxide. A series of carboxylic acids ranging from acetic acid to myristic acid has been used, and their effects on film quality and stability are presented.

  • 3.
    Grahn, Mattias
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Lobanova, Antonina
    Luleå tekniska universitet.
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Hedlund, Jonas
    Orientational analysis of adsorbates in molecular sieves by FTIR/ATR spectroscopy2008In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 20, no 19, p. 6270-6276Article in journal (Refereed)
    Abstract [en]

    ZnS ATR elements were coated with well-defined b-oriented ZSM-5 films by in situ growth. Both adsorption isotherms, as well as molecular orientation of p-xylene adsorbed in the films, were measured at 323 and 373 K by FTIR/ATR spectroscopy. The observed isotherms for the b-oriented ZSM-5 films in the present work were very similar to previously reported isotherms of supported MFI films, albeit the crystals in the latter films were aluminum free (silicalite-1) and orientated differently relative to the support surface than the crystals in the films studied in the present work. The novel technique facilitated, for the first time, the examination of how the tilt angle varies with loading and temperature. The data obtained in the present work showed that the p-xylene molecules were mainly oriented with their long axis parallel to the b-direction of the MFI crystals in concert with previously reported results based on FTIR microscopy, Monte Carlo simulations, NMR, and XRD data. At high concentrations, the tilt angle was in good agreement with observations by FTIR microscopy. It was also found that the orientation of the molecules changed with loading, this might be due to different adsorption geometries in the channel intersection as reported previously. The observed tilt angles may also be influenced from competitive adsorption on silanol groups, as was also indicated in the spectra. The results also indicate that the adsorption properties of zeolite films and powders may differ. Hence, adsorption parameters determined for zeolite powders may not necessarily be applicable to films.

  • 4.
    Maggioni, Gianluigi
    et al.
    Istituto Nazionale di Fisica Nucleare (INFN).
    Carturan, Sara
    Istituto Nazionale di Fisica Nucleare (INFN).
    Tonezzer, Michele
    Istituto Nazionale di Fisica Nucleare (INFN).
    Bonafini, Marco
    Istituto Nazionale di Fisica Nucleare (INFN).
    Vomiero, Alberto
    INFN Laboratori Nazionali di Legnaro.
    Quaranta, Alberto
    University of Trento, Department of Materials Engineering and Industrial Technologies.
    Maurizio, Chiara
    INFM-CNR Sensor Lab.
    Giannici, Francesco
    Department of Inorganic and Analytical Chemistry, University of Palermo.
    Scandurra, Antonino
    Laboratorio Superfici e Interfasi, Consorzio Catania Ricerche, Catania.
    D'Acapito, Francesco
    INFM-CNR Sensor Lab.
    Mea, Gianantonio Della
    Istituto Nazionale di Fisica Nucleare (INFN).
    Puglisi, Orazio
    Dipartimento di Scienze Chimiche, Università di Catania.
    Effects of heat treatments on the properties of copper phthalocyanine films deposited by glow-discharge-induced sublimation2006In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 18, no 17, p. 4195-4204Article in journal (Refereed)
    Abstract [en]

    Copper phthalocyanine films have been deposited by glow-discharge-induced sublimation. The films have undergone postdeposition heat treatments in air at 250 and 290°C for different times, ranging from 30 min to 14 h. The properties of as-deposited and heated films have been investigated by different techniques in order to determine the effects of heat treatments on the film properties. Fourier transform infrared analysis and UV-visible optical absorption analysis point out a gradual evolution of the film structure from a mixture of α and β polymorphs to the only β polymorph in the sample heated at 290°C for 14 h. A pronounced decrease of carbon and nitrogen atomic percentages against an oxygen increase in the heated films are shown by ion beam analyses (Rutherford backscattering spectrometry and nuclear reaction analysis) and X-ray photoelectron spectroscopy (XPS). X-ray absorption spectroscopy and XPS indicate that part of the copper phthalocyanine molecules decompose during heat treatments and the formation of copper oxide takes place. The replacement of copper phthalocyanine by copper oxide in the heated films accounts for the change of their surface electrical conductance and of their electrical response to NO 2. © 2006 American Chemical Society.

  • 5.
    Natile, Marta Maria
    et al.
    Universita Degli Studi di Padova.
    Ponzoni, Andrea
    University of Brescia, CNR IDASC SENSOR Lab.
    Concina, Isabella
    Department of Information Engineering, University of Brescia, CNR-INO SENSOR Lab.
    Glisenti, Antonella
    Istituto per l’Energetica e le Interfasi, Dipartimento di Scienze Chimiche, CNR and Università di Padova.
    Chemical tuning versus microstructure features in solid-state gas sensors: LaFe1-xGaxO3, a case study2014In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 26, no 4, p. 1505-1513Article in journal (Refereed)
    Abstract [en]

    A simple and cheap wet chemical approach is exploited to synthesize LaFe1-xGaxO3 (x = 0-1) crystalline perovskites. Ga doping level deeply influences not only the microstructure, but also the iron chemical features and consequently the responses to external chemicals. Sensitivity toward gases (NO2, CO, and ethanol), in fact, is driven by both Fe/Ga ratio and iron oxidation states, which are demonstrated playing a role much stronger than morphological parameters, such as grain size and specific surface area, usually dominating the performances of metal oxide based gas sensors. Results highlight that sensing behavior is tunable within a large extent by a simple and effective modulation of the chemical composition, obtaining sensitivities comparable with state of the art perovskite based gas sensors.

  • 6.
    Naydenov, Valeri
    et al.
    Luleå tekniska universitet.
    Tosheva, Lubomira
    Luleå tekniska universitet.
    Sterte, Johan
    Palladium-containing zeolite beta macrostructures prepared by resin macrotemplating2002In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 14, no 12, p. 4881-4885Article in journal (Refereed)
    Abstract [en]

    A multistep procedure for the preparation of palladium-containing zeolite beta spheres using anion-exchange resin beads as shape-directing macrotemplates is presented. In a first step, resin beads are hydrothermally treated with zeolite beta synthesis solutions, and as a result resin-zeolite beta composite particles are obtained. In a second step, anionic palladium precursor species are introduced into the composite using the residual ion-exchange capacity of the resin. Finally, the ion exchanger is removed by calcination, leaving self-bonded palladium-containing zeolite beta spheres. The spheres obtained by the procedure were characterized by AAS, XRD, SEM, EDS, UV-vis DRS spectroscopy, nitrogen adsorption measurements, and chemisorption. Materials with controlled macroshape, porosity, and palladium content were prepared by the method.

  • 7.
    Qinghua, Li
    et al.
    Luleå tekniska universitet.
    Creaser, Derek
    Luleå tekniska universitet.
    Sterte, Johan
    An investigation of the nucleation/crystallization kinetics of nanosized colloidal faujasite zeolites2002In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 14, no 3, p. 1319-1324Article in journal (Refereed)
    Abstract [en]

    two-stage varying-temperature technique was utilized to study the nucleation/crystallization kinetics of nanosized faujasite zeolites from clear solutions. At 100 C, the nucleation period of zeolite Y was determined to be about 6.5 days, which extended over almost the whole period of crystal growth. The crystallization kinetics of colloidal zeolite Y differed from those for another clear solution, colloidal zeolite system, namely, TPA-silicalite-1, where the nucleation and crystal growth were found to occur as separate processes. Despite the occurrence of simultaneous nucleation and crystal growth, the colloidal zeolite Y product had a crystal size distribution similar to that for TPA-silicalite-1. In addition, the influence of the growth-limiting nutrient (Na+) on the crystallization of zeolite Y was investigated. The sodium concentration in the synthesis solution could be controlled below a critical level to avoid the nucleation of zeolite A.

  • 8.
    Schäffer, Tilman E
    et al.
    Department of Physics, University of California.
    Ionescu-Zanetti, Cristian
    Department of Physics, University of California.
    Proksch, Roger
    Department of Physics, University of California.
    Fritz, Monika
    Department of Physics, University of California.
    Walters, Deron A.
    Department of Physics, University of California.
    Almqvist, Nils
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.
    Zaremba, Charlotte M.
    Materials Research Laboratory, University of California.
    Belcher, Angela M.
    Marine Biotechnology Center, Department of Molecular Biology, University of California.
    Smith, Bettye L.
    Department of Physics, University of California.
    Stucky, Galen D.
    Department of Chemistry, University of California, Santa Barbara.
    Morse, Daniel E.
    Marine Biotechnology Center, Department of Molecular Biology, University of California.
    Hansma, Paul K.
    Department of Physics, University of California.
    Does abalone nacre form by heteroepitaxial nucleation or by growth through mineral bridges?1997In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 9, p. 1731-1740Article in journal (Refereed)
    Abstract [en]

    We present experimental support for a model of abalone nacre growth that is based on mineral bridges between successive aragonite tablets rather than on heteroepitaxial nucleation. Interlamellar sheets of organic polymers delineate the aragonite tablets but allow the tablets to grow mineral bridges through pores in the sheets. Atomic force microscope images of interlamellar organic sheets from flat pearls made by Haliotis rufescens (red abalone; marine gastropod mollusk) reveal a fibrous core and holes of 5-50 nm in diameter. Scanning ion conductance microscopy shows that these holes are actually pores through the interlamellar sheets. With the help of statistical analysis we can associate the pore-to-pore spacings in the interlamellar sheets with the observed offsets of successive nacre tablets. These results, supplemented by AFM, SEM, and TEM images, support and extend the model of biofabrication of gastropod nacre which is based on mineral bridges between the aragonite tablets.

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  • 9.
    Severin, Kathryn G.
    et al.
    Michigan State University.
    Ledford, Jeffrey S.
    Michigan State University.
    Torgerson, Beatrice A.
    Michigan State University.
    Berglund, Kris
    Characterization of titanium and zirconium valerate sol-gel films1994In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 6, no 7, p. 890-898Article in journal (Refereed)
    Abstract [en]

    FTIR and XPS have been used to characterize titanium and zirconium valerate thin films prepared using sol-gel techniques. Films were prepared by hydrolysis of titanium(IV) isopropoxide or zirconium(IV) n-propoxide in excess valeric acid at room temperature. Film solution chemistry, from precursors to cast films, was followed with FTIR. The structure and chemical composition of films spin cast from fresh and day-old solutions were determined. Results of these studies suggest that all films consist of a metal-oxygen polymer backbone coordinated with bidentate valerate ligands. No evidence for the presence of alkoxide ligands has been found. A small amount of water is present in all cast films. While solution aging experiments indicate that the zirconium film structure does not change with solution reaction time, carboxylate ligand concentrations are higher in titanium films made from aged solutions. Titanium films made from aged solutions contain slightly less than 1.5 valerate ligands/titanium atom. Zirconium films are more highly carboxylated with almost two valerate groups per metal center.

  • 10.
    Zhang, Guangyu
    et al.
    Luleå tekniska universitet.
    Sterte, Johan
    Shoeman, Brian J.
    Luleå tekniska universitet.
    Preparation of colloidal suspensions of discrete TS-1 crystals1997In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 9, no 1, p. 210-217Article in journal (Refereed)
    Abstract [en]

    Stable colloidal suspensions containing discrete TS-1 crystals with average crystal sizes less than 100 nm and with a narrow particle size distribution have been synthesized from clear homogeneous solutions. The products were characterized with respect to crystallinity, crystal size and size distribution, Ti incorporation, specific surface areas, the nature of the Ti species in the products, and the colloidal crystals surface electric charge. The influence of several parameters including synthesis mixture composition and crystallization temperature on crystal size and Ti incorporation were investigated. The synthesis of colloidal crystals with an average size less than 100 nm is favored by low crystallization temperatures (100°C), a highly basic environment, concentrated mixtures, and low Ti contents in the synthesis solutions. The maximum incorporation of tetrahedrally coordinated Ti was 0.84 mol %. High crystallization temperatures (>100°C) favor products with a low Si/Ti molar ratio, but larger crystals are formed, >100 nm, and octahedrally coordinated Ti and extra-framework Ti are detected. A preliminary investigation of the clear hydrolyzed precursor solution and its freeze-dried amorphous equivalent showed that small particles with an average size of 4.8 nm exist in the solution and a certain degree of ordering resembling the MFI structure was present in the precursor particles

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