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At least 1,099 records · Page 61Linked to original sources
PubMed2005

Single-molecule studies of diffusion by oligomer-bound dyes in organically modified sol-gel-derived silicate films.

Single-molecule fluorescence spectroscopy is used to study dye diffusion within organically modified silicate (ORMOSIL) films. ORMOSIL films are prepared from sols containing tetraethoxysilane and isobutyltrimethoxysilane in 2:1 and 1:9 molar ratios. Nile red and a new silanized form of nile red that can be covalently attached to the silicate matrix are used as fluorescent probe molecules. The number and rate of single molecules diffusing through these films increases dramatically with increasing film organic content. Autocorrelation of the fluorescence images yields a quantitative measure of the relative populations of fixed and diffusing species. Surprisingly, both "free" and silicate-bound nile red exhibit relatively facile translational motions. Single-molecule/single-point fluorescence correlation spectroscopy (FCS) is used to measure the dye diffusion coefficients in submicrometer-scale film regions. The most common diffusion coefficients for "free" and silicate-bound nile red molecules in the 1:9 films are 3.9 x 10(-10) and 1.6 x 10(-10) cm(2)/s, respectively. The unexpectedly rapid diffusion of silicate-bound nile red is attributed to the presence of liquidlike silicate oligomers in the films. A lower bound for the molecular weight of the oligomers is estimated at 2900. Bulk solution-phase FCS experiments performed on "free" and silicate-bound nile red species extracted into chloroform solutions provide valuable support for these conclusions. Comparison of the results derived from experimental and simulated time transients indicates film heterogeneity occurs on sub-100-nm-length scales and likely results from the presence of inorganic- and organic-rich domains.

Journal Article↗
PubMed2006

Molecular adsorption to LiMo3Se3 nanowire film chemiresistors.

Thin films of metallic nanowire bundles derived from the Chevrel compound LiMo3Se3 undergo reversible increases of their electrical resistance (up to 70%) upon exposure to vapors of organic solvents (Qi, X. B.; Osterloh, F. E. J. Am. Chem. Soc. 2005, 127 (21), 7666-7667). Using quartz crystal microbalance measurements with four analytes, we demonstrate here that the temporal and steady-state resistance changes of the films depend on the time following the adsorption and on the number of molecules that adsorb to the nanowire films at a given pressure. The adsorption ability of the films and the corresponding film resistance increase in the row: hexane < THF < ethanol < DMSO, closely following the polarities of the solvents. On average, approximately 10(5) analyte molecules per LiMo3Se3 unit are required to produce a measurable electrical response. Atomic force microscopy scans on nanowire films reveal that analytes deposit on top of the nanowire bundles and cause the films to swell by approximately 6% in volume. The temporal and steady-state resistance data of the LiMo3Se3 chemiresistors can be explained by assuming that coating of the nanowire bundles with analyte molecules reduces the interwire charge transport in the films.

Journal Article↗
PubMed1997

Photo-cross-linked decyl methacrylate films for electrochemical and optical polyion probes.

Potentiometric and optical polyion probes based on photo-cross-linked thin films of decyl methacrylate (DMA) are described, and the effects of film composition on the response toward heparin are examined in detail. In accordance with existing theory governing potentiometric polyion response, lowering the amounts of plasticizer and tridodecylmethylammonium chloride ion exchanger within the film enhances its sensitivity toward heparin. Varying the cross-linker content of a DMA-based film, however, provides an additional mechanism to regulate its physical structure and, hence, the observed potentiometric polyion response. Films with low hexanedioldimethacrylate cross-linker content yield optimal potentiometric heparin detection limits (0.04 microM), suggesting a lower diffusion coefficient within such films, apparently due to interactions between adjacent pendant decyl groups. Increasing crosslinker content interrupts these interactions and facilitates diffusion. This knowledge is applied to optimize optical heparin sensing via DMA films covalently attached to glass substrates. When used in a limited volume/fixed exposure time measurement mode, such optically sensitive films can detect clinically relevant levels of heparin (0.5-5 units/mL) in undiluted human plasma.

Cross-Linking Reagents↗
PubMed2000

Open circuit reactions complicating the electroprecipitation of poly(vinylferricinium) films from methylene chloride

We describe an electrochemical quartz crystal microbalance interfacial gravimetric study of the electroprecipitation and dissolution of PVF+ClO4- (PVF = poly(vinylferrocene)) films exposed to methylene chloride solutions. Film deposition is diffusion controlled by the supply of PVF from the solution. Film solvent content is markedly dependent upon the deposition potential. The self-exchange process between surface-bound ferricinium sites and solution-phase ferrocene sites, which is responsible for film deposition under conditions of positive applied potential, is also responsible for film dissolution under open circuit conditions. Dependent upon the deposition potential, releasing the electrode from potential control may (not) result in transient deposition processes that temporarily increase surface coverage. Under all conditions, opening the circuit ultimately leads to reductive stripping of the film by solution-phase PVF. The dissolution rate is independent of applied potential, and is not limited by electron transfer at the outer film interface or by electron (and coupled ion) transport within the film; we speculate that polymer-based processes, such as chain disentanglement, are rate limiting.

Journal Article↗
PubMed1997

Cholesterol modifies the properties of surface films of dipalmitoylphosphatidylcholine plus pulmonary surfactant-associated protein B or C spread or adsorbed at the air-water interface.

Cholesterol is a substantial component of pulmonary surfactant (approximately 8 wt % or approximately 14 mol % of surfactant lipids). This study investigated the effect of cholesterol on the way in which hydrophobic SP-B and SP-C modulated the adsorption of lipid into the air-water interface and their respreading from collapsed phase produced on overcompression of the surface film. The properties of binary spread monolayers of SP-B or SP-C plus cholesterol (CH) were consistent with miscibility between the hydrophobic proteins and the sterol. Results from surface pressure versus area measurements at 23 degrees C on spread monolayers of dipalmitoylphosphatidylcholine (DPPC) plus SP-B in the presence of 8 wt % cholesterol implied that CH did not significantly affect the properties of the films of SP-B/(DPPC/CH) compared to those of binary SP-B/DPPC monolayers. In contrast, CH appeared to enhance the mixing of SP-C with DPPC/CH in ternary SP-C/(DPPC/CH) films compared to the miscibility of SP-C with DPPC in the SP-C/DPPC films. It is estimated that about 10 wt % SP-C might remain in the SP-C/(DPPC/CH) monolayers compressed to high surface pressures of about 72 mN/m, whereas SP-C at concentrations of > or = 5 wt % was squeezed out at pi approximately 50 mN/m from SP-C/DPPC films without cholesterol. Cholesterol reduced the stability of the films of SP-B/(DPPC/CH) and SP-C/(DPPC/CH) when they had been compressed to pi approximately 72 mN/m, in contrast to films of SP-B/DPPC and SP-C/DPPC which exhibited a relatively slow relaxation from the collapse pressure of 72 mN/m. Dynamic cyclic compression beyond collapse of SP-B/(DPPC/CH) and SP-C/(DPPC/CH) monolayers showed that cholesterol diminished their postcollapse respreading compared to the respreading of the protein/DPPC films without cholesterol. Cholesterol, at 8 wt %, inhibited the rate of adsorption to the air-water interface at 35 degrees C of aqueous dispersions of DPPC containing 2.5 or 5 wt % SP-B or SP-C. The results suggest that cholesterol has an apparent negative influence on the surfactant surface properties, which are generally considered to be important in surfactant function, although increasing protein concentrations can counteract some of the negative influences.

1,2-Dipalmitoylphosphatidylcholine↗
PubMedDate not supplied

Improvement of stability and cell adhesion properties of polyelectrolyte multilayer films by chemical cross-linking.

Poly(L-lysine)/hyaluronan (PLL/HA) films were chemically cross-linked with a water soluble carbodiimide (EDC) in combination with a N-hydroxysulfo-succinimide (NHS) to induce amide formation. Fourier transform infrared spectroscopy confirms the conversion of carboxylate and ammonium groups into amide bonds. Quartz crystal microbalance-dissipation reveals that the cross linking reaction is accompanied by a change in the viscoelastic properties of the films leading to more rigid films. After the cross-linking reaction, both positively and negatively ending films exhibit a negative zeta potential. It is shown by fluorescence recovery after photobleaching measured by confocal laser scanning microscopy that cross-linking dramatically reduces the diffusion of the PLL chains in the network. Cross linking also renders the films highly resistant to hyaluronidase, an enzyme that naturally degrades hyaluronan. Finally, the adhesion of chondrosarcoma cells on the films terminating either with PLL or HA is also investigated. Whereas the non cross-linked films are highly resistant to cell adhesion, the cells adhere and spread well on the cross-linked films.

Cell Adhesion↗
PubMedDate not supplied

Formaldehyde cross-linking of gliadin films: effects on mechanical and water barrier properties.

In this study, pioneering results on specific chemical modifications of wheat gluten gliadins and the corresponding impact on mechanical and water barrier properties of derived films are presented. Films were prepared from gliadins chemically treated with formaldehyde and subsequently mixed with different concentrations of glycerol as a plasticizing agent. Water vapor barrier and mechanical properties of the films were evaluated as a function of relative humidity and glycerol concentration. Formaldehyde treatment led to enhanced mechanical properties and, to a lesser extent, improved water barrier of the films, effects which point to the formation of new intermolecular bonds between monomeric gliadins. The occurrence of cross-linking was supported by SDS-PAGE analysis. Cross-linked films maintained their integrity after immersion in water and had similar optical properties to control films. The effect of glycerol and humidity on water vapor permeability and the mechanical properties of films was less acute when proteins were treated with formaldehyde. Thus, chemical treatment of proteins is shown to be a very effective route for optimizing the use of these films in packaging applications.

Cross-Linking Reagents↗
PubMedDate not supplied

Effect of water on the surface molecular mobility of poly(lactide) thin films: an atomic force microscopy study.

Physical properties associated with molecular mobility on the surface of thin films with 300 nm thickness for poly(lactide)s (PLAs) were studied under vacuum conditions as well as under aqueous conditions by using friction force mode atomic force microscopy (AFM). Two types of PLAs were applied for the experimental samples as uncrystallizable PLA (uc-PLA) and crystallizable PLA (c-PLA). The friction force on the surface of thin films was measured as a function of temperature to assess the surface molecular mobility both under vacuum and under aqueous conditions. A lower glass-transition temperature of the uc-PLA surface in water was detected than that under vacuum conditions. In the case of the c-PLA thin film, change in friction force was detected at a lower temperature under aqueous conditions than in vacuo. A morphological change was observed in the c-PLA thin film during heating process from room temperature to 100 degrees C by temperature-controlled AFM. The surface of the c-PLA thin film became rough due to the cold crystallization, and the crystallization of c-PLA molecules in water took place at a lower temperature than in vacuo. These friction force measurements and AFM observations suggest that molecular motion on the surface of the both uc- and c-PLA thin films is enhanced in the presence of water molecules. In addition, in situ AFM observation of the enzymatic degradation process for the c-PLA thin film crystallized at 160 degrees C was carried out in buffer solution containing proteinase K at room temperature. The amorphous region around the hexagonal crystal was eroded within 15 min. It has been suggested that the adsorption of water molecules on the PLA film surface enhances the surface molecular mobility of the glassy amorphous region of PLA and induces the enzymatic hydrolysis by proteinase K.

Adsorption↗
PubMedDate not supplied

Swelling behavior of hyaluronic acid/polyallylamine hydrochloride multilayer films.

The reversible swelling behavior of multilayer films containing hyaluronic acid and polyallylamine hydrochloride was investigated using in situ ellipsometry, since many of the natural functions and applied uses of hyaluronic acid are related to the extraordinary ability of this biopolymer to swell, and to respond conformationally to the local solution environment. This swelling was observed to be substantial, and depended strongly on the film thickness, the pH conditions used to prepare the films, and the swelling solution pH and ionic strength. The swelling results were also rationalized in terms of the dissociation behavior of the polyelectrolytes in the multilayer assemblies, measured by the zeta potential, on colloidal particles. The films were found to swell by as much as 8 times their dry thickness, and the extent of film hydration was observed to depend on the thickness of the films in a nonlinear fashion. This was related to the internal structure of the films, which is dictated by the assembly pH conditions. In addition, the swelling solution pH and ionic strength influence the electrostatic environment in the films and, in turn, have a substantial effect on the overall swelling behavior.

Hyaluronic Acid↗
PubMed2002

Effect of environmental conditions on the permeability of high density polyethylene film to fumigant vapors.

Soil fumigation in greenhouses or agricultural fields often includes tarping the soil surface with polyethylene (PE) films to contain the fumigant in the soil and reduce emissions to the atmosphere. Previous research has demonstrated that PE films are permeable to methyl bromide and other fumigant compounds. In these experiments, the effect of temperature, fumigant mixtures, condensed water, and field aging on the permeability of high-density polyethylene (HDPE) was determined. Mass transfer coefficients (h, a measure of permeability) of the fumigants methyl bromide, 1,3-dichloropropene, propargyl bromide, and chloropicrin across HDPE films were determined. In these studies, temperature and HDPE film type had the largest impact on the h of fumigant compounds across HDPE films. Other factors investigated, including fumigant mixtures, condensed water on the film, and field aging of UV-stabilized film, did not have a significant impact on h. The results of these experiments suggest that the permeability of an intact piece of an agricultural film will increase with increasing temperature but is relatively constant despite changes in other environmental conditions.

Fumigation↗
PubMed1996

Synthesis and Characterization of a New Series of Nickel(II) meso-Tetrakis (polyfluorophenyl)porphyrins Functionalized by Pyrrole Groups and Their Electropolymerized Films.

A new series of nickel(II) meso-tetrakis(polyfluorophenyl)porphyrins functionalized by pyrrole groups have been synthesized. Each new complex was isolated and characterized by (1)H NMR, (19)F NMR, IR, UV-visible spectroscopy, and mass spectrometry as well as electrochemistry. This is the first example of polyfluorinated substituted porphyrins where the four possible compounds have been obtained by functionalization of the para-fluorine substituents of the nickel(II) meso-tetrakis(pentafluorophenyl)porphyrin. This functionalization has allowed the preparation for the first time of polyfluorinated metalloporphyrin films by oxidative electropolymerization. Electrochemical stability studies of these polymeric films have shown better stability for films derived from the monomer having four pyrrole groups because of their high degree of cross-linking degree. A large difference of electroactive solute permeation has been found in the polymeric films which have been obtained by electropolymerization of monomers for which one pyrrole group has been substituted compared to those for which four pyrrole groups have been substituted. This could be related to quite rigid polymer structures for tetrasubstituted polymer films and molecular sieving properties of monosubstituted polymer films. The spectroelectrochemistry of a polymeric film on an OTE has established that the two-electron-oxidized species are stable in the film; likewise the singly and doubly electroreduced species are stable and are more likely ligand-centered.

Journal Article↗
PubMed2002

Ultrathin layered myoglobin-polyion films functional and stable at acidic pH values.

Cross-linking of myoglobin (Mb) promoted by 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide within films of polystyrene sulfonate after layer-by-layer self-assembly provided remarkable stabilization. Cross-linking greatly improved adhesion of the films to fused silica slides and allowed extensive optical studies over a wide pH range. Circular dichroism and visible absorbance spectra showed that Mb retained its native conformation when films were placed in solutions of pH as low as 2 and up to pH 11. Linear dichroism revealed an average orientation of the Mb iron heme cofactors of 58 degrees to the film normal. High concentrations of urea did denature the protein in the films, however. At pH 1, Mb in solution is fully unfolded but retained considerable alpha-helical content in the cross-linked films. Both the polyion film environment and cross-linking seem to play roles in stabilizing protein secondary structure and function at low pH. Cross-linked myoglobin-polyion films on pyrolytic graphite electrodes were used in strongly acidic solutions for the electrochemical catalytic reduction of trichloracetic acid, hydrogen peroxide, and oxygen. The pH-dependent catalytic reduction of trichloracetic acid was faster in 0.1 M HCl than in the medium pH range.

Animals↗
PubMed2003

Surface polymerization by ion-assisted deposition for polythiophene film growth.

Cationic polymerization is induced at the gas-solid interface by hyperthermal organic cations coincident on a surface with a thermal beam of organic monomers. This process, termed surface polymerization by ion-assisted deposition (SPIAD), produces films that maintain the chemical structure of the monomer. A polythiophene film is produced here by SPIAD with 100 eV thiophene ions and terthiophene monomers coincident on Si and indium tin oxide (ITO) substrates held under vacuum. X-ray photoelectron spectroscopy observes enhancement in film growth for SPIAD compared with either thiophene ion or terthiophene exposure alone. Polythiophene films grown by both mass-selected and nonmass-selected ions with coincident terthiophene dosing both display similar fluorescence intensities at two wavelengths characteristic of emission from films of the terthiophene monomer. Raman spectra of films from nonmass-selected ions display several vibrations also observed in terthiophene films. Ions therefore play a critical role in film growth from nonmass-selected ions, in addition to any radical or photochemically driven processes that may also occur.

Journal Article↗
PubMed2003

Origin of strong chiroptical activities in films of nonafluorenes with a varying extent of pendant chirality.

Novel nonafluorenes with a varying extent of pendant chirality were synthesized for an investigation of the origins of chiroptical activities in neat films. Thermal annealing of 4-microm-thick sandwiched films and of 90-nm-thick spin-cast films, all on surface-treated substrates, produced monodomain glassy films characterized as a right-handed cholesteric stack with a helical pitch length ranging from 180 to 534 nm and from 252 to 1151 nm, respectively. The observed strong circular dichroism (CD) and g(e) as functions of helical pitch length in single-substrate monodomain glassy cholesteric films were quantitatively interpreted with a circularly polarized fluorescence theory accounting for light absorption, emission, and propagation in a cholesteric stack. Although intertwined molecular helices were likely to be present, cholesteric stacking of rodlike molecules seemed to be the predominant contributor to the strong chiroptical activities. All the cholesteric stacks comprising a polydomain glassy film on an untreated substrate were found to contribute to CD and g(e) largely to the same extent as in a monodomain film. A circularly polarized blue organic light-emitting diode containing a nonafluorene film resulted in a g(e) of 0.35 with a luminance yield of 0.94 cd/A at 20 mA/cm(2), the best performance to date.

Journal Article↗
PubMed2005

Electrochemical deposition of mesoporous nickel hydroxide films from dilute surfactant solutions.

A series of micelle-templated mesoporous nickel hydroxide films were prepared by electrochemical deposition from dilute surfactant solutions by using different types of template and by varying plating solvent composition. Lamellar mesostructured Ni(OH)2 films are obtained with only anionic surfactant sodium dodecyl sulfate (SDS) as the template. In particular, a unique cooperative assembly fashion, that is, the combination between Ni2+ and a complex composed of the primary template SDS and a cosurfactant, such as triblock poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO) copolymers and poly(ethylene glycol), was explored, by which two-dimensional hexagonal mesoporous Ni(OH)2 films were electrodeposited. Meanwhile, the deposition medium also plays a crucial role in determining the mesostructure of Ni(OH)2 films. For the composite nickel hydroxide films deposited from aqueous solution or dilute aqueous solution of ethylene glycol (<20 wt %) in the presence of SDS or the SDS-poly(alkylene oxide) polymer complexes, a mixed lamellar phase with d(001) = 37.4 A and d(001) = 28.5 A was obtained. However, single lamellar phase with d(001) = 37.4 A was electrodeposited from concentrated aqueous solutions of ethylene glycol (> or = 20 wt %). Furthermore, such deposition baths have access to hexagonal mesoporous nickel hydroxide films with d(100) = 37.4 A at 70 degrees C with the SDS-poly(alkylene oxide) polymer complexes as the templates. Within the potential window for Ni(OH)2, the morphology and quality of mesostructured films are significantly dependent on the deposition potential, while the mesostructures of the composite films always remain unchanged.

Journal Article↗
PubMed2005

Surface-catalyzed growth of polymethylene-rich copolymer films on gold.

We report the preparation of a new class of copolymer films that consist of polymethylene (PM) with a low percentage ( approximately 1-4%) of randomly distributed ethyl ester side groups, consistent with poly(methylene-co-ethyl acetate). The films are prepared through a surface-catalyzed polymerization on gold surfaces upon exposure to a dilute solution of diazomethane (DM) and ethyl diazoacetate (EDA) in ether at 0 degrees C. While EDA alone does not polymerize at gold surfaces but DM does decompose on gold to grow PM films, the combined presence of EDA and DM results in dramatic enhancements in film growth and promotes an alternative mechanism for propagation as compared with that for the PM homopolymerization. The rate of copolymer film growth is constant over a approximately 24 h period, consistent with a controlled polymerization in which chain terminations are minimized. Carefully controlled experiments indicate that chain propagation does not occur at the outer film-solvent interface, but more likely, at the film-metal interface, suggesting a catalyzed insertion mechanism that extends the chain and pushes the outer chain termini further away from the metal-polymer interface. The results also suggest that adsorbed intermediates of EDA function as co-catalysts to promote the propagation reaction. Of particular importance for materials modification is that the ester side chains of these copolymer films can be hydrolyzed to carboxylate groups that exhibit pH-dependent wettability.

Journal Article↗
PubMed2004

Single-molecule spectroscopy studies of microenvironmental acidity in silicate thin films.

Single-molecule (SM) spectroscopic methods were employed to study single site variations in the acidity properties of sol-gel-derived silicate films. The pH-sensitive dye Carboxy SNARF-1 (C.SNARF-1) was used to sense film acidity. Its concentration in the films was maintained at nanomolar levels to allow for SMs to be spectroscopically interrogated. The ratio of C.SNARF-1 fluorescence at 580 nm (protonated form) and 640 nm (deprotonated form) was used to characterize local film pH. SM data were acquired both for "untreated" films and for those treated by immersion for either 1 or 8 h in phosphate solutions of different pH. The SM results prove that the spectral variability observed is dominated by static variations in the local matrix acidity. Shorter immersion times lead to relatively broad histograms and broad "titration" curves, providing clear evidence for kinetic limitations to access of certain film environments by the immersion solutions. Films subjected to longer immersion times generally exhibit narrower histograms. Particularly narrow distributions were obtained for films treated near pH 8-9, while much broader histograms were produced near pH 7. These results are attributed to the buffering effects of surface silanols near pH 9 and enhanced pH sensitivity of the dye near pH 7.

Journal Article↗
PubMed2004

TEM investigation of formation mechanism of monocrystal-thick b-oriented pure silica zeolite MFI film.

The first direct transmission electron microscopic (TEM) observation has been carried out on the continuous monocrystal-thick b-oriented pure silica zeolite MFI films produced by in situ crystallization. The self-supporting film samples for TEM study were fabricated by dissolving the steel substrate with acid. This TEM study is free of those artifacts that are typically associated with TEM sample preparations, and allows us to investigate the "true" structure and texture of a very large area of the film and at the same time to focus at will on each individual zeolite crystal in the film. Abundant TEM information including crystallographic orientation relationships among crystals in the film (both out-of-plane and in-plane), grain boundaries, and each crystal grain was obtained. This TEM investigation provides direct unambiguous new evidence to support the homogeneous nucleation mechanism, by which the films form through homogeneous nucleation and crystal growth in the bulk to form equal-sized disk-shape crystals, followed by self-assembly of these crystals onto the substrate to produce a two-dimensional close-packed structure. The last stage of the film formation involves simultaneous space-limited growth and rotation of the individual crystals to realize the in-plane crystallographic control within the film.

Journal Article↗