Science.gov

Sample records for microporous silica prepared

  1. Molecular imprinting of bulk, microporous silica

    NASA Astrophysics Data System (ADS)

    Katz, Alexander; Davis, Mark E.

    2000-01-01

    Molecular imprinting aims to create solid materials containing chemical functionalities that are spatially organized by covalent or non-covalent interactions with imprint (or template) molecules during the synthesis process. Subsequent removal of the imprint molecules leaves behind designed sites for the recognition of small molecules, making the material ideally suited for applications such as separations, chemical sensing and catalysis. Until now, the molecular imprinting of bulk polymers and polymer and silica surfaces has been reported, but the extension of these methods to a wider range of materials remains problematic. For example, the formation of substrate-specific cavities within bulk silica, while conceptually straightforward, has been difficult to accomplish experimentally. Here we describe the imprinting of bulk amorphous silicas with single aromatic rings carrying up to three 3-aminopropyltriethoxysilane side groups; this generates and occupies microporosity and attaches functional organic groups to the pore walls in a controlled fashion. The triethoxysilane part of the molecules' side groups is incorporated into the silica framework during sol-gel synthesis, and subsequent removal of the aromatic core creates a cavity with spatially organized aminopropyl groups covalently anchored to the pore walls. We find that the imprinted silicas act as shape-selective base catalysts. Our strategy can be extended to imprint other functional groups, which should give access to a wide range of functionalized materials.

  2. Counter-diffusion of isotopically labeled trichloroethylene in silica gel and geosorbent micropores: Model development

    SciTech Connect

    McMillan, S.A.; Werth, C.J.

    1999-07-01

    A new model was developed to determine if reduced uptake rates observed during isotope exchange experiments could plausibly be attributed to sterically hindered counter-diffusion in one-dimensional micropores. During exchange experiments, hydrogenated trichloroethylene ({sup 1}HTCE) was displaced with deuterated TCE (DTCE) in the slow-desorbing sites of a silica gel, a groundwater sediment, and a clay and silt fraction. To describe this process, the model accounts for co- and counter-diffusion of TCE isotopes in one-dimensional micropores, where each micropore type is defined by a single codiffusion rate constant and a single counter-diffusion rate constant. For silica gel, isotope exchange was simulated in a single micropore type. For geosorbents, isotope exchange was simulated in a distribution of micropore types characterized by a {gamma} distribution of diffusion rate constants. Simulation results indicate that (1) the proposed model accounts for the mechanisms controlling isotope exchange in the silica gel and the groundwater sediment and (2) the rate of counter-diffusion is up to 6 times slower than the rate of codiffusion. This suggests that steric hindrance between counter-diffusing sorbates can significantly affect mass transfer and, consequently, the transport of chemical mixtures in the subsurface.

  3. Blocked-micropores, surface functionalized, bio-compatible and silica-coated iron oxide nanocomposites as advanced MRI contrast agent

    NASA Astrophysics Data System (ADS)

    Darbandi, Masih; Laurent, Sophie; Busch, Martin; Li, Zi-An; Yuan, Ying; Krüger, Michael; Farle, Michael; Winterer, Markus; Vander Elst, Luce; Muller, Robert N.; Wende, Heiko

    2013-05-01

    Biocompatible magnetic nanoparticles have been found promising in several biomedical applications for tagging, imaging, sensing and separation in recent years. In this article, a systematic study of the design and development of surface-modification schemes for silica-coated iron oxide nanoparticles (IONP) via a one-pot, in situ method at room temperature is presented. Silica-coated IONP were prepared in a water-in-oil microemulsion, and subsequently the surface was modified via addition of organosilane reagents to the microemulsion system. The structure and the morphology of the as synthesized nanoparticles have been investigated by means of transmission electron microscopy (TEM) and measurement of N2 adsorption-desorption. Electron diffraction and high-resolution transmission electron microscopic (TEM) images of the nanoparticles showed the highly crystalline nature of the IONP structures. Nitrogen adsorption indicates microporous and blocked-microporous structures for the silica-coated and amine functionalized silica-coated IONP, respectively which could prove less cytotoxicity of the functionalized final product. Besides, the colloidal stability of the final product and the presence of the modified functional groups on top of surface layer have been proven by zeta-potential measurements. Owing to the benefit from the inner IONP core and the hydrophilic silica shell, the as-synthesized nanocomposites were exploited as an MRI contrast enhancement agent. Relaxometric results prove that the surface functionalized IONP have also signal enhancement properties. These surface functionalized nanocomposites are not only potential candidates for highly efficient contrast agents for MRI, but could also be used as ultrasensitive biological-magnetic labels, because they are in nanoscale size, having magnetic properties, blocked-microporous and are well dispersible in biological environment.

  4. Chemical reduction of three-dimensional silica micro-assemblies into microporous silicon replicas.

    PubMed

    Bao, Zhihao; Weatherspoon, Michael R; Shian, Samuel; Cai, Ye; Graham, Phillip D; Allan, Shawn M; Ahmad, Gul; Dickerson, Matthew B; Church, Benjamin C; Kang, Zhitao; Abernathy, Harry W; Summers, Christopher J; Liu, Meilin; Sandhage, Kenneth H

    2007-03-08

    The carbothermal reduction of silica into silicon requires the use of temperatures well above the silicon melting point (> or =2,000 degrees C). Solid silicon has recently been generated directly from silica at much lower temperatures (< or =850 degrees C) via electrochemical reduction in molten salts. However, the silicon products of such electrochemical reduction did not retain the microscale morphology of the starting silica reactants. Here we demonstrate a low-temperature (650 degrees C) magnesiothermic reduction process for converting three-dimensional nanostructured silica micro-assemblies into microporous nanocrystalline silicon replicas. The intricate nanostructured silica microshells (frustules) of diatoms (unicellular algae) were converted into co-continuous, nanocrystalline mixtures of silicon and magnesia by reaction with magnesium gas. Selective magnesia dissolution then yielded an interconnected network of silicon nanocrystals that retained the starting three-dimensional frustule morphology. The silicon replicas possessed a high specific surface area (>500 m(2) g(-1)), and contained a significant population of micropores (< or =20 A). The silicon replicas were photoluminescent, and exhibited rapid changes in impedance upon exposure to gaseous nitric oxide (suggesting a possible application in microscale gas sensing). This process enables the syntheses of microporous nanocrystalline silicon micro-assemblies with multifarious three-dimensional shapes inherited from biological or synthetic silica templates for sensor, electronic, optical or biomedical applications.

  5. Transport of pure components in pervaporation through a microporous silica membrane.

    PubMed

    Bettens, Ben; Dekeyzer, Sofie; Van der Bruggen, Bart; Degrève, Jan; Vandecasteele, Carlo

    2005-03-24

    The pervaporation mechanism of pure components through a commercial microporous silica membrane was studied by performing experiments using water, methanol, ethanol, 2-propanol, and n-propanol in the 40-80 degrees C temperature range. Experimental fluxes were correlated to feed temperature and viscosity. It was found that the permeation mechanism obeys the adsorption-diffusion description, covering both the microscopic models based on configurational (micropore) diffusion and on activated surface diffusion. The contribution of convection was negligible. Size parameters for the permeating molecules such as molecular weight, kinetic diameter, and effective diameter, which are expected to have an influence on diffusion, did not correlate with the flux, thus strongly emphasizing the importance of sorption as the rate-determining step for transport in the pervaporation process. This was confirmed by correlating parameters reflecting polarity with flux: an exponential relation between the Hansen polarity (especially the hydrogen bonding component) and the flux was observed. A similar correlation was found between the dielectric constant and the flux. Furthermore, the flux increases in the same direction as the hydrophilicity of the pure components (log P). The effects of membrane surface tension and contact angles are less outspoken, but experiments performed on glass supported and silica supported membrane top layers suggest an important influence of the sublayers on the flux.

  6. Hybrid Mesoporous Silicas and Microporous POSS-Based Frameworks Incorporating Evaporation-Induced Self-Assembly

    PubMed Central

    Li, Jheng-Guang; Chu, Wei-Cheng; Kuo, Shiao-Wei

    2015-01-01

    We fabricated a series of mesoporous silicas and mesoporous organosilicates with hierarchical porosity through evaporation-induced self-assembly using Pluronic F127 as a template in this study. We could tailor the mesophase of each mesoporous silica sample by varying the weight ratio of its two silica sources: tetraethyl orthosilicate (TEOS) and triethoxysilane hydrosilylated octavinyl polyhedral oligomeric silsesquioxane (OV-POSS-SILY). The mesophases ranged from an ordered body-centered cubic (bcc) structure (TEOS alone) to ordered face-centered cubic (fcc) structure (10 and 20 wt.% of OV-POSS-SILY) and finally to disordered spherical pores (≥30 wt.% of OV-POSS-SILY). We used small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM) to study the transformations of these mesophases, while N2 isotherm sorption curves revealed the porosities of these mesoporous silicate samples. Moreover, 29Si CP/MAS solid state nuclear magnetic resonance spectroscopy allowed us to analyze the compositions of the POSS-containing silicate frameworks. Such functional mesoporous silica samples incorporating microporous POSS building units have potential applications in various systems, including optical and electronic devices.

  7. The hydrogen-storing microporous silica 'Microcluster' reduces acetaldehyde contained in a distilled spirit.

    PubMed

    Kato, Shinya; Miwa, Nobuhiko

    2016-12-01

    Acetaldehyde is a detrimental substance produced in alcoholic liquor aging. We assessed an ability of hydrogen-storing microporous silica 'Microcluster' (MC+) to reduce acetaldehyde, as compared with autoclave-dehydrogenated MC+ (MC-). Acetaldehyde was quantified spectrophotometrically by an enzymatic method. Authentic acetaldehyde was treated by MC+ for 20min, and decreased from 43.4ppm to 10.9ppm, but maintained at 49.3ppm by MC-. On the other hand, acetaldehyde contained in a distilled spirit was decreased from 29.5ppm to 3.1ppm at 20min by MC+, but not decreased by MC-. Addition of MC+ or MC- to distilled water without acetaldehyde showed no seeming effect on the quantification used. Accordingly acetaldehyde in a distilled spirit is reduced to ethanol by hydrogen contained in MC+, but not by the silica moiety of MC+. Hydrogen gas of 1.2mL was released for 20min from MC+ of 0.59g in water, resulting in dissolved hydrogen of 1.09ppm and an oxidation- reduction potential of -687.0mV indicative of a marked reducing ability. Thus, MC+ has an ability to reduce acetaldehyde in a distilled spirit due to dissolved hydrogen released from MC+.

  8. Process for preparing polymer reinforced silica aerogels

    NASA Technical Reports Server (NTRS)

    Meador, Mary Ann B. (Inventor); Capadona, Lynn A. (Inventor)

    2011-01-01

    Process for preparing polymer-reinforced silica aerogels which comprises a one-pot reaction of at least one alkoxy silane in the presence of effective amounts of a polymer precursor to obtain a silica reaction product, the reaction product is gelled and subsequently subjected to conditions that promotes polymerization of the precursor and then supercritically dried to obtain the polymer-reinforced monolithic silica aerogels.

  9. Massive preparation of pitch-based organic microporous polymers for gas storage.

    PubMed

    Li, Wenqing; Zhang, Aijuan; Gao, Hui; Chen, Mingjie; Liu, Anhua; Bai, Hua; Li, Lei

    2016-02-14

    A general challenge for preparing organic microporous polymers (MOPs) is to use cheap and sustainable building blocks while retaining the advanced functions. We demonstrate a strategy to massively prepare pitch-based MOPs, which are thermally and chemically stable. A maximum BET surface area of 758 m(2) g(-1) and high gas storage capacity were achieved.

  10. Evaluation of a Cyclodextrin-silica Hybrid Microporous Composite for the Solid-phase Extraction of Polycyclic Aromatic Hydrocarbons.

    PubMed

    Soler-Seguí, Salomé; Belenguer-Sapiña, Carolinakn-Aut-Sei; Amorós, Pedro; Mauri-Aucejo, Adela

    2016-01-01

    Solid-phase extraction (SPE) coupled with high-performance liquid chromatography (HPLC) with fluorescence detection were employed to determine trace polycyclic aromatic hydrocarbons in water samples. In this way, the use of cartridges containing cyclodextrin-silica hybrid microporous solid phases was proposed. The experimental results indicated that the method provided relative standard deviations of below 15% and detection limits recorded were 12, 1.2, 12, 38, 4, 6 and 4 ng L(-1) for benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[g,h,i]perylene, indeno[1,2,3]pyrene, benzo[a]pyrene, dibenzo[a,h]anthracene and benzo[a]anthracene, respectively. Moreover, the method was successfully applied for the determination of these organic compounds in water samples, where they were found to be in the 7 to 580 ng L(-1) range. It can be concluded that the major advantages of cyclodextrin-silica hybrid microporous solid phases are that they reduce the consumption and the toxicity of the solvent and the time consumption of the sample treatment step.

  11. Procedure to prepare transparent silica gels

    NASA Technical Reports Server (NTRS)

    Barber, Patrick G. (Inventor); Simpson, Norman R. (Inventor)

    1987-01-01

    This invention relates to the production of silica gels and in particular to a process for the preparation of silica gels which can be used as a crystal growth medium that simulates the convectionless environment of space to produce structurally perfect crystals. Modern utilizations of substances in electronics, such as radio transmitters and high frequency microphones, often require single crystals with controlled purity and structural perfection. The near convectionless environment of silica gel suppresses nucleation, thereby reducing the competitive nature of crystal growth. This competition limits the size and perfection of the crystal; and it is obviously desirable to suppress nucleation until, ideally, only one crystal grows in a predetermined location. A silica gel is not a completely convectionless environment like outer space, but is the closest known environment to that of outer space that can be created on Earth.

  12. Microporous structure with layered interstitial surface treatment, and method and apparatus for preparation thereof

    NASA Technical Reports Server (NTRS)

    Koontz, Steven L. (Inventor)

    1994-01-01

    A microporous structure with layered interstitial surface treatments, and method and apparatus for preparation thereof is presented. The structure is prepared by sequentially subjecting a uniformly surface-treated structure to atomic oxygen treatment to remove an outer layer of surface treatment to a generally uniform depth, and then surface treating the so exposed layer with another surface treating agent. The atomic oxygen/surface treatment steps may optionally be repeated, each successive time to a lesser depth, to produce a microporous structure having multilayered surface treatments. The apparatus employs at least one side arm from a main atomic oxygen-containing chamber. The side arm has characteristic relaxation times such that a uniform atomic oxygen dose rate is delivered to a specimen positioned transversely in the side arm spaced from the main gas chamber.

  13. Microporous structure with layered interstitial surface treatment, and method and apparatus for preparation thereof

    NASA Technical Reports Server (NTRS)

    Koontz, Steven L. (Inventor)

    1992-01-01

    A microporous structure with layered interstitial surface treatments, and the method and apparatus for its preparation are disclosed. The structure is prepared by sequentially subjecting a uniformly surface treated structure to atomic oxygen treatment to remove an outer layer of surface treatment to a generally uniform depth, and then surface treating the so exposed layer with another surface treating agent. The atomic oxygen/surface treatment steps may optionally be repeated, each successive time to a lesser depth, to produce a microporous structure having multilayered surface treatments. The apparatus employs at least one side arm from a main oxygen-containing chamber. The side arm has characteristic relaxation times such that a uniform atomic oxygen dose rate is delivered to a specimen positioned transversely in the side arm spaced from the main gas chamber.

  14. Preparation and characterization of microporous fibers for sample preparation and LC-MS determination of drugs.

    PubMed

    Buszewski, Boguslaw; Nowaczyk, Jacek; Ligor, Tomasz; Olszowy, Pawel; Ligor, Magdalena; Wasiniak, Bartlomiej; Miekisch, Wolfram; Schubert, Jochen K; Amann, Anton

    2009-07-01

    The aim of this study was the preparation of polypyrrole (PPy) fibers for solid phase microextraction (SPME). PPy coatings were obtained during the electrochemical polymerization process. The utility of various metal wires (Fe, Cu, Ag, Cu/Ag, kanthal and medical stainless steel) as a support for polymers was compared. Various experimental conditions of the synthesis process such as scan rate, voltage limits and number of scans and deposition time were applied. The average polymer thickness was in the range of 7-125 microm and its weight was in the scope of 0.65-5.6 mg. Different techniques, mainly elemental analysis, Fourier transform infrared spectroscopy, microscopy, and chromatography were performed for the characterization of obtained fibers with microporous structure. The extraction efficiency of cardiovascular drugs (metoprolol, propranolol, oxprenolol, propafenone and mexiletine) by means of fibers was tested. The concentration of mentioned compounds in standard solution was in the span of 10-150 ng/mL. LC-MS was employed for determination of drugs in desorption solution. LODs varied from 0.013 to 1.51 ng/mL for metoprolol and mexiletine respectively. The repeatability of extraction was obtained with the RSD values lower than 10%.

  15. Preparation and characterization of microporous poly(D,L-lactic acid) film for tissue engineering scaffold.

    PubMed

    Shi, Shuai; Wang, Xiu Hong; Guo, Gang; Fan, Min; Huang, Mei Juan; Qian, Zhi Yong

    2010-11-24

    We prepared a series of microporous films based on poly(d,l-lactic acid) (PLA) via phase separation. According to scanning electron microscopy (SEM), a 3-dimensional foamy structure with multimicrometer scale pores on the air surface of film could be observed. As the morphology of PLA film could not be stabilized using solvent-nonsolvent phase separation, we investigated the effect of temperature, air movement, and concentration on the properties of microporous PLA films. The results show that when the temperature was 25°C in a vacuum, it was easy to prepare PLA film with micropores, and it was stable. As the relationship between the morphology and formation factors was clear and the morphology of the PLA film was controllable, we studied the PLA film's potential use for cell culture. SEM results showed that NIH3T3 cell could be adhered on the surface of film well after incubation for 2 days. Meanwhile, in vitro culture experiments revealed the great biocompatibility of the scaffold for adsorption and proliferation of fibroblasts.

  16. Phenomena affecting morphology of microporous poly(acrylonitrile) prepared via phase separation from solution

    SciTech Connect

    Legasse, R.R.; Weagley, R.J.; Leslie, P.K.; Schneider, D.A.

    1990-01-01

    This paper is concerned with controlling the morphology of microporous polymers prepared via thermal demixing of solutions. 2 wt % solutions of poly(acrylonitrile) in maleic anhydride, a poor solvent, are first cooled to produce separated polymer-rich and solvent-rich phases. Removing the solvent by freeze drying then produces a microporous material having a density of 33 mg/cm{sup 3}, a void fraction of 97%, and a pore size of about 10 {mu}m. We find that the morphology cannot be explained by existing models, which focus on phase diagrams and kinetics of phase transformations during cooling of the solution. In conflict with those models, we find that two radically different morphologies can be produced even when the polymer concentration and cooling path are held strictly constant. A hypothesis that polymer degradation causes the different morphologies is not supported by GPC, {sup 13}C NMR, and FTIR experiments. Instead, we offer evidence that the different microporous morphologies are caused by different polymer conformations in solutions having the same concentration and temperature. 11 refs., 3 figs.

  17. Modulation of microporous/mesoporous structures in self-templated cobalt-silica

    PubMed Central

    Martens, Dana L.; Wang, David K.; Motuzas, Julius; Smart, Simon; da Costa, João C. Diniz

    2015-01-01

    Finite control of pore size distributions is a highly desired attribute when producing porous materials. While many methodologies strive to produce such materials through one-pot strategies, oftentimes the pore structure requires post-treatment modification. In this study, modulation of pore size in cobalt-silica systems was investigated by a novel, non-destructive, self-templated method. These systems were produced from two cobalt-containing silica starting materials which differed by extent of condensation. These starting materials, sol (SG′) and xerogel (XG′), were mixed with pure silica sol to produce materials containing 5–40 mol% Co. The resultant SG-series materials exhibited typical attributes for cobalt-silica systems: mesoporous characteristics developed at high cobalt concentrations, coinciding with Co3O4 formation; whereas, in the XG-series materials, these mesoporous characteristics were extensively suppressed. Based on an examination of the resultant materials a mechanism describing the pore size formation and modulation of the two systems was proposed. Pore size modulation in the XG-series was caused, in part, by the cobalt source acting as an autogenous template for the condensation of the silica network. These domains could be modified when wetted, allowing for the infiltration and subsequent condensation of silica oligomers into the pre-formed, mesoporous cages, leading to a reduction in the mesoporous content of the final product. PMID:25609189

  18. Preparation of microporous melamine-based polymer networks in an anhydrous high-temperature miniemulsion.

    PubMed

    Schwab, Matthias Georg; Crespy, Daniel; Feng, Xinliang; Landfester, Katharina; Müllen, Klaus

    2011-11-15

    We report the first example of a successful preparation of a microporous organic polymer within the droplet phase of an inverse non-aqueous miniemulsion. Stable nanoparticles with enhanced specific surface area could be obtained despite the harsh conditions regarding reaction temperature (180 °C) and time (72 h) needed for building melamine-based Schiff base networks. Our new flexible method can in principle be applied to other water-sensitive protocols suitable for the bulk synthesis of MOPs that are based on Friedel-Crafts, Sonogashira-Hagihara or Yamamoto chemistry.

  19. Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

    PubMed

    Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

    2016-08-15

    Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction.

  20. High surface area microporous activated carbons prepared from Fox nut (Euryale ferox) shell by zinc chloride activation

    NASA Astrophysics Data System (ADS)

    Kumar, Arvind; Mohan Jena, Hara

    2015-11-01

    High surface area microporous activated carbon has been prepared from Fox nutshell (Euryale ferox) by chemical activation with ZnCl2 as an activator. The process has been conducted at different impregnation (ZnCl2/Fox nutshell) ratios (1-2.5) and carbonization temperatures (500-700 °C). The thermal decomposition behavior of Fox nutshell and impregnated Fox nutshell has been carried out by thermogravimetric analysis. The pore properties including the BET surface area, micropore surface area, micropore volume, and pore size distribution of the activated carbons have been determined by nitrogen adsorption-desorption isotherms at -196 °C using the BET, t-plot method, DR, and BJH methods. The BET surface area, the microporous surface area, total pore volume, and micropore volume have been obtained as 2869 m2/g, 2124 m2/g, 1.96 cm3/g, and 1.68 cm3/g, respectively, and the microporosity percentage of the prepared activated carbon is 85.71%. The prepared activated carbons have been also characterized with instrumental methods such as Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and field emission scanning electron microscopy (FESEM).

  1. Charge transfer mechanism in titanium-doped microporous silica for photocatalytic water-splitting applications

    DOE PAGES

    Sapp, Wendi; Koodali, Ranjit; Kilin, Dmitri

    2016-02-29

    Solar energy conversion into chemical form is possible using artificial means. One example of a highly-efficient fuel is solar energy used to split water into oxygen and hydrogen. Efficient photocatalytic water-splitting remains an open challenge for researchers across the globe. Despite significant progress, several aspects of the reaction, including the charge transfer mechanism, are not fully clear. Density functional theory combined with density matrix equations of motion were used to identify and characterize the charge transfer mechanism involved in the dissociation of water. A simulated porous silica substrate, using periodic boundary conditions, with Ti4+ ions embedded on the inner poremore » wall was found to contain electron and hole trap states that could facilitate a chemical reaction. A trap state was located within the silica substrate that lengthened relaxation time, which may favor a chemical reaction. A chemical reaction would have to occur within the window of photoexcitation; therefore, the existence of a trapping state may encourage a chemical reaction. Furthermore, this provides evidence that the silica substrate plays an integral part in the electron/hole dynamics of the system, leading to the conclusion that both components (photoactive materials and support) of heterogeneous catalytic systems are important in optimization of catalytic efficiency.« less

  2. Charge transfer mechanism in titanium-doped microporous silica for photocatalytic water-splitting applications

    SciTech Connect

    Sapp, Wendi; Koodali, Ranjit; Kilin, Dmitri

    2016-02-29

    Solar energy conversion into chemical form is possible using artificial means. One example of a highly-efficient fuel is solar energy used to split water into oxygen and hydrogen. Efficient photocatalytic water-splitting remains an open challenge for researchers across the globe. Despite significant progress, several aspects of the reaction, including the charge transfer mechanism, are not fully clear. Density functional theory combined with density matrix equations of motion were used to identify and characterize the charge transfer mechanism involved in the dissociation of water. A simulated porous silica substrate, using periodic boundary conditions, with Ti4+ ions embedded on the inner pore wall was found to contain electron and hole trap states that could facilitate a chemical reaction. A trap state was located within the silica substrate that lengthened relaxation time, which may favor a chemical reaction. A chemical reaction would have to occur within the window of photoexcitation; therefore, the existence of a trapping state may encourage a chemical reaction. Furthermore, this provides evidence that the silica substrate plays an integral part in the electron/hole dynamics of the system, leading to the conclusion that both components (photoactive materials and support) of heterogeneous catalytic systems are important in optimization of catalytic efficiency.

  3. Process for Preparing Epoxy-Reinforced Silica Aerogels

    NASA Technical Reports Server (NTRS)

    Meador, Mary Ann B (Inventor)

    2016-01-01

    One-pot reaction process for preparing epoxy-reinforced monolithic silica aerogels comprising the reaction of at least one silicon compound selected from the group consisting of alkoxysilanes, orthosilicates and combination thereof in any ratio with effective amounts of an epoxy monomer and an aminoalkoxy silane to obtain an epoxy monomer-silica sol in solution, subsequently preparing an epoxy-monomer silica gel from said silica sol solution followed by initiating polymerization of the epoxy monomer to obtain the epoxy-reinforced monolithic silica aerogel.

  4. Adsorption of CO{sub 2} on microporous materials. 1: On activated carbon and silica gel

    SciTech Connect

    Berlier, K.; Frere, M.

    1997-05-01

    Adsorption isotherms of carbon dioxide (CO{sub 2}) at temperatures ranging from 278 K to 328 K (seven temperatures) and at pressures up to 3300 kPa on activated carbon and on silica gel are presented. These experimental results are useful as they allow one to broaden, the T, P domain of CO{sub 2} adsorption. These data, together with more classical ones (obtained at low temperature and low pressure (Berlier and Frere, 1996)), will make possible the test of theoretical developments for the prediction of adsorption isotherms in a range of temperature and pressure conditions never studied before.

  5. Electric double-layer capacitance of microporous carbon nano spheres prepared through precipitation of aromatic resin pitch

    NASA Astrophysics Data System (ADS)

    Lee, Sang-Ick; Mitani, Satoshi; Park, Chul Wan; Yoon, Seong-Ho; Korai, Yozo; Mochida, Isao

    Microporous carbon nano sphere (MCNS) was successfully prepared through the precipitation method of an aromatic isotropic pitch in water without any activation. MCNS was composed of nano spheres with diameter ranging from 100 to 300 nm, which were interlinked together to form a three-dimensional network in a MCNS particle. There were a number of mesopores among the nano carbon spheres, while micropores were developed within a nanosphere. These structural features enabled MCNS to have high specific capacitance as high as 154 F g -1 by cyclic voltammetry (CV) and capacitance per surface area of 0.62 F m -2 as an electrode for the inorganic capacitor, respectively.

  6. Preparation and Mechanism of Controllable Micropores on Bioceramic TiO2 Coatings by Plasma Electrolytic Oxidation

    NASA Astrophysics Data System (ADS)

    Wang, Hong-Yuan; Zhu, Rui-Fu; Lu, Yu-Peng; Xiao, Gui-Yong; Ma, Jie; Yuan, Y. F.

    2013-09-01

    Porous titania coatings with Ca and P elements were synthesized by plasma electrolytic oxidation (PEO). The treatment was carried out in an electrolyte containing calcium acetate monohydrate and disodium phosphate dodecahydrate (Ca/P = 5), and 4-20 μm micropores were prepared on the coatings by applied pulse frequencies of 200-1000 Hz. The surface structure, chemical composition of the TiO2 coatings, and time-dependent variation of electric currents were studied. The result revealed that the coating micropores, which could be controlled in size, increased with higher frequency, and the coatings mainly consisted of anatase and rutile phases with varying fractions. Based on our experiment, the formation mechanism of micropores and phases of the PEO coatings was further discussed in details.

  7. Spontaneous waveguide Raman spectroscopy of self-assembled monolayers in silica micropores.

    PubMed

    Calkins, Jacob A; Peacock, Anna C; Sazio, Pier J A; Allara, David L; Badding, John V

    2011-01-18

    Advances in nanoscience are critically dependent on the ability to control and probe chemical and physical phenomena in confined geometries. A key challenge is to identify confinement structures with high surface area to volume ratios and controlled surface boundaries that can be probed quantitatively at the molecular level. Herein we report an approach for probing molecular structures within nano- to microscale pores by the application of spontaneous Raman spectroscopy. We demonstrate the method by characterization of the structural features of picomole quantities of well-organized octadecyltrichlorosilane (OTS) monolayers self-assembled on the interior pore surfaces of high aspect ratio (1 μm diameter × 1-10 cm length), near-atomically smooth silica microstructured optical fibers (MOFs). The simple Raman backscattering collection geometry employed is well suited for a wide variety of diagnostic applications as demonstrated by tracking the combustion of the hydrocarbon chains of the OTS self-assembled monolayer (SAM) and spectral confirmation of the formation of an adsorbed monolayer of human serum albumin (HSA) protein. Using this MOF Raman approach, molecular processes in precisely defined, highly confined geometries can be probed at high pressures and temperatures, with a wide range of excitation wavelengths from the visible to the near-IR, and under other external perturbations such as electric and magnetic fields.

  8. Silica scintillating materials prepared by sol-gel methods

    SciTech Connect

    Werst, D.W.; Sauer, M.C. Jr.; Cromack, K.R.; Lin, Y.; Tartakovsky, E.A.; Trifunac, A.D.

    1993-12-31

    Silica was investigated as a rad-hard alternative to organic polymer hosts for organic scintillators. Silica sol-gels were prepared by hydrolysis of tetramethoxysilane in alcohol solutions. organic dyes were incorporated into the gels by dissolving in methanol at the sol stage of gel formation. The silica sol-gel matrix is very rad-hard. The radiation stability of silica scintillators prepared by this method is dye-limited. Transient radioluminescence was measured following excitation with 30 ps pulses of 20 MeV electrons.

  9. Microporous Organic Polymers Based on Hyper-Crosslinked Coal Tar: Preparation and Application for Gas Adsorption.

    PubMed

    Gao, Hui; Ding, Lei; Bai, Hua; Li, Lei

    2017-02-08

    Hyper-crosslinked polymers (HCPs) are promising materials for gas capture and storage, but high cost and complicated preparation limit their practical application. In this paper, a new type of HCPs (CTHPs) was synthesized through a one-step mild Friedel-Crafts reaction with low-cost coal tar as the starting material. Chloroform was utilized as both solvent and crosslinker to generate a three-dimensional crosslinked network with abundant micropores. The maximum BET surface area of the prepared CTHPs could reach up to 929 m(2)  g(-1) . Owing to the high affinity between the heteroatoms on the coal-tar building blocks and the CO2 molecules, the adsorption capacity of CTHPs towards CO2 reached up to 14.2 wt % (1.0 bar, 273 K) with a high selectivity (CO2 /N2 =32.3). Furthermore, the obtained CTHPs could adsorb 1.27 wt % H2 at 1.0 bar and 77.3 K, and also showed capacity for the capture of high organic vapors at room temperature. In comparison with other reported porous organic polymers, CTHPs have the advantages of low-cost, easy preparation, and high gas-adsorption performance, making them suitable for mass production and practical use in the future.

  10. Photoluminescence decay dynamics of transparent silica glass prepared from nanometer-sized silica particles

    SciTech Connect

    Yamada, Tomoko; Uchino, Takashi

    2005-08-22

    The time-resolved photoluminescence (PL) decays are measured for transparent amorphous silica prepared from solid-phase sintering of nanometer-sized silica particles, which has recently been shown to exhibit a unique white PL emission under ultraviolet excitation [T. Uchino and T. Yamada, Appl. Phys. Lett. 85, 1164 (2004)]. Unlike usual PL processes observed in normal silica glass, it is shown that the present PL results from trapping-controlled migration of photoexcited carriers and their radiative recombination.

  11. Photoluminescence decay dynamics of transparent silica glass prepared from nanometer-sized silica particles

    NASA Astrophysics Data System (ADS)

    Yamada, Tomoko; Uchino, Takashi

    2005-08-01

    The time-resolved photoluminescence (PL) decays are measured for transparent amorphous silica prepared from solid-phase sintering of nanometer-sized silica particles, which has recently been shown to exhibit a unique white PL emission under ultraviolet excitation [T. Uchino and T. Yamada, Appl. Phys. Lett. 85, 1164 (2004)]. Unlike usual PL processes observed in normal silica glass, it is shown that the present PL results from trapping-controlled migration of photoexcited carriers and their radiative recombination.

  12. Preparation and Characterization of Colloidal Silica Particles under Mild Conditions

    ERIC Educational Resources Information Center

    Neville, Frances; Zin, Azrinawati Mohd.; Jameson, Graeme J.; Wanless, Erica J.

    2012-01-01

    A microscale laboratory experiment for the preparation and characterization of silica particles at neutral pH and ambient temperature conditions is described. Students first employ experimental fabrication methods to make spherical submicrometer silica particles via the condensation of an alkoxysilane and polyethyleneimine, which act to catalyze…

  13. Preparation and supercapacitive behaviors of the ordered mesoporous/microporous chromium carbide-derived carbons

    NASA Astrophysics Data System (ADS)

    Wu, Chun; Gao, Jiao; Zhao, Qinglan; Zhang, Youwei; Bai, Yansong; Wang, Xingyan; Wang, Xianyou

    2014-12-01

    A series of ordered mesoporous/microporous carbon materials derived from chromium carbide-derived carbons (CDCs) are prepared by nanocasting the chromic acetate and furfuryl alcohol precursor into SBA-15 and subsequent chlorination. The structure and morphology of the CDCs are characterized by N2 adsorption/desorption isotherm, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that all of the synthesized CDCs present large specific surface area and pore volume. Especially, the CDCs-2 prepared at the mass ratio of 1/1 (chromic acetate/furfuryl alcohol) exhibits the chain-like morphology with high surface area (1236 m2 g-1), large pore volume (0.76 cm3 g-1), and the good mesopore size centered at 3.43 nm. The electrochemical properties of all the CDCs are studied by cyclic voltammetry, constant current charge/discharge, electrochemical impedance spectroscopy and cycle life measurements in 6 M KOH electrolyte. The results display that the sample CDCs-2 exhibits a high capacitance of 242.7 F g-1 at the current density of 1 A g-1 and good cycling stability with coulombic efficiency of 100% over 10000 cycles.

  14. Compressible and monolithic microporous polymer sponges prepared via one-pot synthesis

    PubMed Central

    Lim, Yoonbin; Cha, Min Chul; Chang, Ji Young

    2015-01-01

    Compressible and monolithic microporous polymers (MPs) are reported. MPs were prepared as monoliths via a Sonogashira–Hagihara coupling reaction of 1,3,5-triethynylbenzene (TEB) with the bis(bromothiophene) monomer (PBT-Br). The polymers were reversibly compressible, and were easily cut into any form using a knife. Microscopy studies on the MPs revealed that the polymers had tubular microstructures, resembling those often found in marine sponges. Under compression, elastic buckling of the tube bundles was observed using an optical microscope. MP-0.8, which was synthesized using a 0.8:1 molar ratio of PBT-Br to TEB, showed microporosity with a BET surface area as high as 463 m2g–1. The polymer was very hydrophobic, with a water contact angle of 145° and absorbed 7–17 times its own weight of organic liquids. The absorbates were released by simple compression, allowing recyclable use of the polymer. MPs are potential precursors of structured carbon materials; for example, a partially graphitic material was obtained by pyrolysis of MP-0.8, which showed a similar tubular structure to that of MP-0.8. PMID:26534834

  15. Compressible and monolithic microporous polymer sponges prepared via one-pot synthesis

    NASA Astrophysics Data System (ADS)

    Lim, Yoonbin; Cha, Min Chul; Chang, Ji Young

    2015-11-01

    Compressible and monolithic microporous polymers (MPs) are reported. MPs were prepared as monoliths via a Sonogashira-Hagihara coupling reaction of 1,3,5-triethynylbenzene (TEB) with the bis(bromothiophene) monomer (PBT-Br). The polymers were reversibly compressible, and were easily cut into any form using a knife. Microscopy studies on the MPs revealed that the polymers had tubular microstructures, resembling those often found in marine sponges. Under compression, elastic buckling of the tube bundles was observed using an optical microscope. MP-0.8, which was synthesized using a 0.8:1 molar ratio of PBT-Br to TEB, showed microporosity with a BET surface area as high as 463 m2g-1. The polymer was very hydrophobic, with a water contact angle of 145° and absorbed 7-17 times its own weight of organic liquids. The absorbates were released by simple compression, allowing recyclable use of the polymer. MPs are potential precursors of structured carbon materials; for example, a partially graphitic material was obtained by pyrolysis of MP-0.8, which showed a similar tubular structure to that of MP-0.8.

  16. Preparation of stable ultrahydrophobic and superoleophobic silica-based coating.

    PubMed

    Nimittrakoolchai, On-Uma; Supothina, Sitthisuntorn

    2012-06-01

    Silica-Based coatings having excellent water- and oil-repellent properties and good weathering stability have been deposited onto glass surface by a simple one-step dip coating technique. To achieve ultra water repellency and super oil repellency, the chemical composition of SiO2 nanoparticle employed as surface roughness enhancer and trichloro(1H,1H,2H,2H-perfluorooctyl)silane employed as surface-energy reducing substance was varied. At the optimum synthesis condition, the coating exhibited very high contact angles of 173.2, 146.7 and 147.6 degrees for water, ethylene glycol and seed oil, respectively. The achievement of excellent water- and oil-repellency is also described based on the presence of air trapped in micropore of the coating in addition to its high surface roughness and low surface free energy. The coatings have good weathering stability based on natural and accelerated weathering tests indicating feasibility for practical use.

  17. Preparation and characterization of silymarin synchronized-release microporous osmotic pump tablets

    PubMed Central

    Zeng, Qi-ping; Liu, Zhi-hong; Huang, Ai-wen; Zhang, Jing; Song, Hong-tao

    2016-01-01

    The pharmacological activity of herbal medicine is an overall action of each component in accordance with their original proportion. An efficient, sustained, and controlled-release drug delivery system of herbal medicine should ensure the synchronized drug release of each active component during the entire release procedure. In this study, silymarin (SM), a poorly soluble herbal medicine, was selected as a model drug to develop a synchronized-release drug delivery system: an SM microporous osmotic pump (MPOP) tablet. The SM was conjugated with phospholipid (SM phytosome complex, SM-PC) to improve the solubility, and the difference in the apparent octanol–water partition coefficient between the two components was significantly reduced. The dissolution rate of SM-PC was significantly higher than SM active pharmaceutical ingredients and was the same as that of the commercial SM capsule. The SM-PC was used to generate the MPOP tablet. SM was mixed with poly(ethylene) oxide and sodium chloride (an osmotic agent) to form the MPOP core, followed by coating with cellulose acetate and poly(ethylene) oxide to generate the SM MPOP. The results demonstrated that SM MPOP could synchronically and sustainably release the five active components within 12 hours (the similar coefficient f2 between two components was >65), and the average cumulative release rate was 85%. Fitting of the drug-release curve showed a zero-order release profile for SM MPOP. Our study showed that the phytosome complex technique combined with the MPOP system will achieve synchronized release of the various active components of herbal medicine and have potential applications in developing sustained release preparations in herbal medicine. PMID:26889080

  18. Solid State Electrolytes Prepared from PEO (360) Silanated Silica

    NASA Technical Reports Server (NTRS)

    Maitra, P.; Ding, J.; Liu, B.; Wunder, S. L.; Lin, H.-P.; Chua, D.; Salomon, M.

    2002-01-01

    All solid state composite electrolytes were prepared using fumed silica (SiO2) silanated with an oligomeric polyethylene oxide (PEO) silane containing 6-9 ethylene oxide repeat units, a PEO matrix and LiClO4 (8/1 O/Li). The PEO-silane covalently attached to the silica was amorphous, with a T(sub g) that increased from -90 C to -53 C after attachment. The conductivity of films prepared using the PEO-silanated silica increased to approx. 6 x 10(exp -5) S/cm at RT compared with approx. 1 x 10(-5) S/cm for films prepared with unsilanated SiO2.

  19. Drug silica nanocomposite: preparation, characterization and skin permeation studies.

    PubMed

    Pilloni, Martina; Ennas, Guido; Casu, Mariano; Fadda, Anna Maria; Frongia, Francesca; Marongiu, Francesca; Sanna, Roberta; Scano, Alessandra; Valenti, Donatella; Sinico, Chiara

    2013-01-01

    The aim of this work was to evaluate silica nanocomposites as topical drug delivery systems for the model drug, caffeine. Preparation, characterization, and skin permeation properties of caffeine-silica nanocomposites are described. Caffeine was loaded into the nanocomposites by grinding the drug with mesoporous silica in a ball mill up to 10 h and the efficiency of the process was studied by XRPD. Formulations were characterized by several methods that include FTIR, XRPD, SEM and TEM. The successful loading of caffeine was demonstrated by XRPD and FTIR. Morphology was studied by SEM that showed particle size reduction while TEM demonstrated formation of both core-shell and multilayered caffeine-silica structures. Solid-state NMR spectra excluded chemical interactions between caffeine and silica matrix, thus confirming that no solid state reactions occurred during the grinding process. Influence of drug inclusion in silica nanocomposite on the in vitro caffeine diffusion into and through the skin was investigated in comparison with a caffeine gel formulation (reference), using newborn pig skin and vertical Franz diffusion cells. Results from the in vitro skin permeation experiments showed that inclusion into the nanocomposite reduced and delayed caffeine permeation from the silica nanocomposite in comparison with the reference, independently from the amount of the tested formulation.

  20. Ion channel mimetic membranes and silica nanotubes prepared from porous aluminum oxide templates

    NASA Astrophysics Data System (ADS)

    Mitchell, David Tanner

    Chapter 1 provides background information on the template synthesis of nanomaterials. The template synthesis method is examined with special attention to the use of membranes containing monodisperse cylindrical pores as templates. Several examples of the utility of template-synthesized nanomaterials are given. The production of one type of template membrane, nanopore alumina, is reviewed. Reviews of sol-gel and silane chemistry are also provided. In Chapter 2, a sol-gel template synthesis process is used to produce silica nanotubes within the pores of alumina templates. The nanotubes can be modified using a variety of chemistries, typically via a silanization process. Because the nanotubes are formed in a template, the interior and exterior surface can be modified independently. Modified nanotubes can be used for drug detoxification or as extractants for the removal of metal ions. The nanotube surface can also be biotinylated, which causes binding to avidinated surfaces. Composite microtubes of silica and various polymers are also prepared. Additionally, Au nanowires are shown to assemble with colloidal Au particles using dithiols as linkers. Chapter 3 describes the attachment of proteins onto template-synthesized silica nanotubes. The proteins are covalently linked via an aldehyde silane bridge that binds to pendant primary amino moieties on the protein. Protein-modified nanotubes function as highly specific extractants. Avidin-modified nanotubes extract biotin-coated Au nanoparticles from solution with high extraction efficiency. Immunoprotein-modified nanotubes extract the corresponding antibody from solution with high specificity. Antibody-modified nanotubes extract one enantiomer from a racemic mix. Enzymes, including drug detoxification enzymes, were also attached to the nanotubes and were shown to retain their catalytic activity. Immunoproteins on the outside of nanotubes can be used to direct nanotube binding, creating specific labeling agents. Chapter 4

  1. Solar-grade silicon prepared by carbothermic reduction of silica

    NASA Technical Reports Server (NTRS)

    Aulich, H. A.; Schulze, F. W.; Urbach, H. P.; Lerchenberger, A.

    1986-01-01

    An advanced carbothermic reduction (ACR) process was developed to produce solar grade (SC) silicon from high purity silica and carbon. Preparation of starting materials and operation of the arc furnace to product high purity silicon is described. Solar cells prepared from single crystal SG-Si had efficiencies of up to 12.3% practically identical to cells made from electronic grade silicon. The ACR process is not in the pilot stage for further evaluation.

  2. Preparation of microporous films with sub nanometer pores and their characterization using stress and FTIR measurements

    SciTech Connect

    Samuel, J.; Hurd, A.J.; Swoll, F. van; Frink, L.J.D.; Contakes, S.C.; Brinker, C.J. |

    1996-06-01

    The authors have used a novel technique, measurement of stress isotherms in microporous thin films, as a means of characterizing porosity. The stress measurement was carried out by applying sol-gel thin films on a thin silicon substrate and monitoring the curvature of the substrate under a controlled atmosphere of various vapors. The magnitude of macroscopic bending stress developed in microporous films depends on the relative pressure and molar volume of the adsorbate and reaches a value of 180 MPa for a relative vapor pressure, P/Po = 0.001, of methanol. By using a series of molecules, and observing both the magnitude and the kinetics of stress development while changing the relative pressure, they have determined the pore size of microporous thin films. FTIR measurements were used to acquire adsorption isotherms and to compare pore emptying to stress development, about 80% of the change in stress takes place with no measurable change in the amount adsorbed. The authors show that for sol-gel films, pore diameters can be controlled in the range of 5--8 {angstrom} by ``solvent templating``.

  3. Preparation of EPR/silica filler by a co-irradiation method forming PP/EPR/silica nanocomposites

    NASA Astrophysics Data System (ADS)

    Qian, Jun; Dang, Shuaiying; Huang, Zhijuan; Xu, Yongshen

    2012-01-01

    This paper presents a novel approach to prepare ethylene-propylene rubber (EPR)/silica filler by co-irradiation method forming polypropylene (PP)/EPR/silica nanocomposites. The grafting of maleic anhydride (MAH) on EPR was first studied by co-irradiation in the micro-suspension without any chemical initiator, and the effects of MAH concentration and the total co-irradiation dose on the graft degree of MAH were investigated. Then PP/EPR/silica nanocomposites were successfully prepared by blending of PP matrix and EPR/silica filler, which was obtained by co-irradiation using a mixture of EPR/MAH microsuspension in xylene and tetraethoxysilane/KH560 sol in formic acid. FTIR and SEM results showed that the reactions between MAH on EPR chains and KH560 surrounding silica particles were adopted to form the EPR/silica filler with strong bonding and well silica dispersion. Mechanical properties of PP/EPR/silica nanocomposites with different silica contents and the comparisons with PP, PP/EPR and PP/silica films were studied. The rigid silica particles were trapped in EPR shell and well dispersed in PP/EPR/silica nanocomposites with good compatibility and strong interfacial adhesion, achieving overall improvements in stiffness, strength and toughness compared with pure PP.

  4. Preparation of a new micro-porous poly(methyl methacrylate)-grafted polyethylene separator for high performance Li secondary battery

    NASA Astrophysics Data System (ADS)

    Gwon, Sung-Jin; Choi, Jae-Hak; Sohn, Joon-Yong; Ihm, Young-Eon; Nho, Young-Chang

    2009-10-01

    In this study, micro-porous poly(methyl methacrylate)-grafted polyethylene separators (PE-g-PMMA) were prepared by a radiation-induced graft polymerization of methyl methacrylate onto a conventional PE separator followed by a phase inversion. After the phase inversion, the micro-pores were generated in the grafted PMMA layer. The prepared micro-porous PE-g-PMMA separators showed an improved electrolyte uptake and ionic conductivity due to their improved affinity with a liquid electrolyte and the presence of pores in the grafted PMMA layer. The PE-g-PMMA separators exhibited a lower thermal shrinkage compared to the original PE separator. The PE-g-PMMA separators showed a better oxidation stability up to 5.0 V when compared to the original PE separator (4.5 V).

  5. Nitrogen-containing microporous conjugated polymers via carbazole-based oxidative coupling polymerization: preparation, porosity, and gas uptake.

    PubMed

    Chen, Qi; Liu, De-Peng; Luo, Min; Feng, Li-Juan; Zhao, Yan-Chao; Han, Bao-Hang

    2014-01-29

    Facile preparation of microporous conjugated polycarbazoles via carbazole-based oxidative coupling polymerization is reported. The process to form the polymer network has cost-effective advantages such as using a cheap catalyst, mild reaction conditions, and requiring a single monomer. Because no other functional groups such as halo groups, boric acid, and alkyne are required for coupling polymerization, properties derived from monomers are likely to be fully retained and structures of final polymers are easier to characterize. A series of microporous conjugated polycarbazoles (CPOP-2-7) with permanent porosity are synthesized using versatile carbazolyl-bearing 2D and 3D conjugated core structures with non-planar rigid conformation as building units. The Brunauer-Emmett-Teller specific surface area values for these porous materials vary between 510 and 1430 m(2) g(-1) . The dominant pore sizes of the polymers based on the different building blocks are located between 0.59 and 0.66 nm. Gas (H2 and CO2 ) adsorption isotherms show that CPOP-7 exhibits the best uptake capacity for hydrogen (1.51 wt% at 1.0 bar and 77 K) and carbon dioxide (13.2 wt% at 1.0 bar and 273 K) among the obtained polymers. Furthermore, its high CH4 /N2 and CO2 /N2 adsorption selectivity gives polymer CPOP-7 potential application in gas separation.

  6. Preparation of nitrogen-doped cotton stalk microporous activated carbon fiber electrodes with different surface area from hexamethylenetetramine-modified cotton stalk for electrochemical degradation of methylene blue

    NASA Astrophysics Data System (ADS)

    Li, Kunquan; Rong, Zhang; Li, Ye; Li, Cheng; Zheng, Zheng

    Cotton-stalk activated carbon fibers (CSCFs) with controllable micropore area and nitrogen content were prepared as an efficient electrode from hexamethylenetetramine-modified cotton stalk by steam/ammonia activation. The influence of microporous area, nitrogen content, voltage and initial concentration on the electrical degradation efficiency of methylene blue (MB) was evaluated by using CSCFs as anode. Results showed that the CSCF electrodes exhibited excellent MB electrochemical degradation ability including decolorization and COD removal. Increasing micropore surface area and nitrogen content of CSCF anode leaded to a corresponding increase in MB removal. The prepared CSCF-800-15-N, which has highest N content but lowest microporous area, attained the best degradation effect with 97% MB decolorization ratio for 5 mg/L MB at 12 V in 4 h, implying the doped nitrogen played a prominent role in improving the electrochemical degradation ability. The electrical degradation reaction was well described by first-order kinetics model. Overall, the aforesaid findings suggested that the nitrogen-doped CSCFs were potential electrode materials, and their electrical degradation abilities could be effectively enhanced by controlling the nitrogen content and micropore surface area.

  7. Polydisperse spherical colloidal silica particles: Preparation and application

    NASA Astrophysics Data System (ADS)

    Kong, Hui; Huo, Junchao; Liang, Chenliang; Li, Shasha; Liu, Weili; Song, Zhitang

    2016-11-01

    A new industrial method has been developed to produce polydisperse spherical colloidal silica particles with a very broad particle size, ranging from 20-95 nm. The process uses a reactor in which the original seed solution is heated to 100°C, and then active silicic acid and the seed solution are titrated to the reactor continuously with a constant rate. The original seeds and the titrated seeds in the reactor will go through different particle growth cycles to form different particle sizes. Both the particles’ size distribution and morphology have been characterized by dynamic light scattering (DLS) and the focus ion beam (FIB) system. In addition, the as-prepared polydisperse colloidal silica particle in the application of sapphire wafer’s chemical mechanical polishing (CMP) process has been tested. The material removal rate (MRR) of this kind of abrasive has been tested and verified to be much faster than traditional monodisperse silica particles. Finally, the mechanism of sapphire CMP process by this kind of polydisperse silica particles has been investigated to explore the reasons for the high polishing rate. Project supported by the National Major Scientific and Technological Special Project during the Twelfth Five-year Plan Period of China (Grant No. 2009ZX02030-1), the National Natural Science Foundation of China (Grant No. 51205387), the Science and Technology Commission of Shanghai, China (Grant No. 11nm0500300), and the Science and Technology Commission of Shanghai, China (Grant No. 14XD1425300).

  8. Preparation and in vitro evaluation of porous silica gels.

    PubMed

    Gallardo, Janet; Galliano, Pablo G; Porto López, J M

    2002-11-01

    Porous silica gels with high surface areas were prepared from tetraethylothosilicate and polyacrylic acid (PAA) of high molecular weight in acidic media by a sol-gel method. PAA content and ageing temperatures were varied in order to obtain different microstructures. Samples were sintered at temperatures up to 400 degrees C, and subjected to in vitro evaluation by soaking them in acellular inorganic solutions at 37 degrees C and pH 7.3. Surface precipitation of carbonate-apatite on some of the gels was observed by FTIR spectroscopy, scanning electron microscopy and EPMA. Silica dissolution and re-precipitation phenomena were also observed. The relationship between both phenomena during the in vitro test is discussed mainly in terms of structural and microstructural features of the gel.

  9. Preparation of antibacterial silver-doped silica glass microspheres.

    PubMed

    Kawashita, Masakazu; Toda, Shogo; Kim, Hyun-Min; Kokubo, Tadashi; Masuda, Noriaki

    2003-08-01

    Various types of inorganic substances doped with silver ions have been developed as antibacterial materials, and some have already been commercialized. Colorless and chemically durable materials that slowly release silver ions are, however, still need to be developed. The present authors have previously shown that when a silica glass doped with silver and aluminium ions is prepared using the sol-gel method, the resultant product is colorless, chemically durable, and slowly releases silver ions into water over a long period. The doped silica glass takes a form of microspheres <1 microm in diameter, it is easily mixed with organic polymers, and the mixture can be formed into a thin film or fine fibers, etc. We report on the preparation of silver doped silica glass microspheres having a diameter =1 microm, using the sol-gel method. Initially, tetraethoxysilane was partially prehydrolyzed by water in ethanol, and then aluminium triisopropoxide was added to the solution to form Si-O-Al bonds. Finally, an ammonia solution containing silver nitrate was added to form silica microspheres doped with silver ion together with aluminium ions. The results show monodispersed microspheres 0.4-0.6 microm in diameter were obtained with nominal compositions of Si/Al/Ag = 1/0.01-0.03/0.003-0.03, with a molar ratio of Al/Ag = 1-3.3. The microspheres were colorless, showed a high chemical durability, and slowly released silver ions into water at 37 degrees C. Microspheres with the composition Si/Al/Ag = 1/0.01/0.01 showed excellent antibacterial activity against Escherichia coli. The minimum inhibitory concentration (MIC) of the microspheres was 400, which is less than the MIC value (800) of commercial antibacterial materials.

  10. Preparing two-dimensional microporous carbon from Pistachio nutshell with high areal capacitance as supercapacitor materials

    NASA Astrophysics Data System (ADS)

    Xu, Jiandong; Gao, Qiuming; Zhang, Yunlu; Tan, Yanli; Tian, Weiqian; Zhu, Lihua; Jiang, Lei

    2014-07-01

    Two-dimensional (2D) porous carbon AC-SPN-3 possessing of amazing high micropore volume ratio of 83% and large surface area of about 1069 m2 g-1 is high-yield obtained by pyrolysis of natural waste Pistachio nutshells with KOH activation. The AC-SPN-3 has a curved 2D lamellar morphology with the thickness of each slice about 200 nm. The porous carbon is consists of highly interconnected uniform pores with the median pore diameter of about 0.76 nm, which could potentially improve the performance by maximizing the electrode surface area accessible to the typical electrolyte ions (such as TEA+, diameter = ~0.68 nm). Electrochemical analyses show that AC-SPN-3 has significantly large areal capacitance of 29.3/20.1 μF cm-2 and high energy density of 10/39 Wh kg-1 at power of 52/286 kW kg-1 in 6 M KOH aqueous electrolyte and 1 M TEABF4 in EC-DEC (1:1) organic electrolyte system, respectively.

  11. Preparing two-dimensional microporous carbon from Pistachio nutshell with high areal capacitance as supercapacitor materials

    PubMed Central

    Xu, Jiandong; Gao, Qiuming; Zhang, Yunlu; Tan, Yanli; Tian, Weiqian; Zhu, Lihua; Jiang, Lei

    2014-01-01

    Two-dimensional (2D) porous carbon AC-SPN-3 possessing of amazing high micropore volume ratio of 83% and large surface area of about 1069 m2 g−1 is high-yield obtained by pyrolysis of natural waste Pistachio nutshells with KOH activation. The AC-SPN-3 has a curved 2D lamellar morphology with the thickness of each slice about 200 nm. The porous carbon is consists of highly interconnected uniform pores with the median pore diameter of about 0.76 nm, which could potentially improve the performance by maximizing the electrode surface area accessible to the typical electrolyte ions (such as TEA+, diameter = ~0.68 nm). Electrochemical analyses show that AC-SPN-3 has significantly large areal capacitance of 29.3/20.1 μF cm−2 and high energy density of 10/39 Wh kg−1 at power of 52/286 kW kg−1 in 6 M KOH aqueous electrolyte and 1 M TEABF4 in EC-DEC (1:1) organic electrolyte system, respectively. PMID:24986670

  12. Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

    PubMed Central

    Gorka, Caroline A.

    2014-01-01

    A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The procedure requires 15-20 min of preparation time, during which a liquid precursor mixture is prepared and poured into wells of a metal mold that is placed between the platens of a hydraulic hot press, followed by several hours of processing within the hot press. The precursor solution consists of a 1.0:12.0:3.6:3.5 x 10-3 molar ratio of tetramethylorthosilicate (TMOS):methanol:water:ammonia. In each well of the mold, a porous silica sol-gel matrix forms. As the temperature of the mold and its contents is increased, the pressure within the mold rises. After the temperature/pressure conditions surpass the supercritical point for the solvent within the pores of the matrix (in this case, a methanol/water mixture), the supercritical fluid is released, and monolithic aerogel remains within the wells of the mold. With the mold used in this procedure, cylindrical monoliths of 2.2 cm diameter and 1.9 cm height are produced. Aerogels formed by this rapid method have comparable properties (low bulk and skeletal density, high surface area, mesoporous morphology) to those prepared by other methods that involve either additional reaction steps or solvent extractions (lengthier processes that generate more chemical waste).The rapid supercritical extraction method can also be applied to the fabrication of aerogels based on other precursor recipes. PMID:24637334

  13. Preparing silica aerogel monoliths via a rapid supercritical extraction method.

    PubMed

    Carroll, Mary K; Anderson, Ann M; Gorka, Caroline A

    2014-02-28

    A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The procedure requires 15-20 min of preparation time, during which a liquid precursor mixture is prepared and poured into wells of a metal mold that is placed between the platens of a hydraulic hot press, followed by several hours of processing within the hot press. The precursor solution consists of a 1.0:12.0:3.6:3.5 x 10(-3) molar ratio of tetramethylorthosilicate (TMOS):methanol:water:ammonia. In each well of the mold, a porous silica sol-gel matrix forms. As the temperature of the mold and its contents is increased, the pressure within the mold rises. After the temperature/pressure conditions surpass the supercritical point for the solvent within the pores of the matrix (in this case, a methanol/water mixture), the supercritical fluid is released, and monolithic aerogel remains within the wells of the mold. With the mold used in this procedure, cylindrical monoliths of 2.2 cm diameter and 1.9 cm height are produced. Aerogels formed by this rapid method have comparable properties (low bulk and skeletal density, high surface area, mesoporous morphology) to those prepared by other methods that involve either additional reaction steps or solvent extractions (lengthier processes that generate more chemical waste).The rapid supercritical extraction method can also be applied to the fabrication of aerogels based on other precursor recipes.

  14. Microporous alumina ceramic membranes

    DOEpatents

    Anderson, M.A.; Guangyao Sheng.

    1993-05-04

    Several methods are disclosed for the preparation microporous alumina ceramic membranes. For the first time, porous alumina membranes are made which have mean pore sizes less than 100 Angstroms and substantially no pores larger than that size. The methods are based on improved sol-gel techniques.

  15. Microporous alumina ceramic membranes

    DOEpatents

    Anderson, Marc A.; Sheng, Guangyao

    1993-01-01

    Several methods are disclosed for the preparation microporous alumina ceramic membranes. For the first time, porous alumina membranes are made which have mean pore sizes less than 100 Angstroms and substantially no pores larger than that size. The methods are based on improved sol-gel techniques.

  16. Emergence of Zeolite Analogs and other Microporous Crystals in an Atomic Lattice Model of Silica and Related Materials.

    PubMed

    Jin, Lin; Auerbach, Scott M; Monson, Peter A

    2012-03-15

    The potential of tailored nanopores to transform technologies such as drug delivery, biofuel production, and optical-electronic devices depends on fundamental knowledge of the self-assembly of ordered nanoporous solids. Atomic-level geometries of critical nuclei that lead to such solids have remained hidden in the nanoscale blind spot between local (<0.5 nm) and collective (>5 nm) probes of structure. Heroic efforts at molecular simulation of nanopore formation have provided massive libraries of hypothetical structures; (1-5) however, to date no statistical simulation has generated a crystallization pathway from random initial condition to ordered nanoporous solid, until now. In this work, we show that a recently developed atomic lattice model of silica and related materials can form ordered nanoporous solids with a rich variety of structures including known chalcogenides, zeolite analogs, and layered materials. We find that whereas canonical Monte Carlo simulations of the model consistently produce the amorphous solids studied in our previous work, parallel tempering Monte Carlo gives rise to ordered nanoporous solids. The utility of parallel tempering highlights the existence of barriers between amorphous and crystalline phases of our model. Moreover, the self-assembly or nanoporous crystalline phases in the model open the door to detailed understanding of nanopore nucleation.

  17. Preparation of aqueous core/silica shell microcapsules.

    PubMed

    Bean, Keith; Black, Camilla F; Govan, Norman; Reynolds, Paul; Sambrook, Mark R

    2012-01-15

    Water core/silica shell microcapsules are prepared via the hydrolysis and subsequent polycondensation of tetraethoxysilane in a surfactant stabilised water-in-oil emulsion. The relationship between preparative conditions, including pH and silane concentration, has been related to final particle structure. Furthermore, the nature of the catalyst has been found to affect the mechanism by which the shells are formed, with an interfacial polymerisation proposed for ammonium hydroxide catalysed synthesis in agreement with previous reports and a new colloidosome assembly process for sodium hydroxide catalysis. In both cases shell aging processes are observed to continue beyond initial shell formation suggesting that trans-shell diffusion of reactants may be feasible, or that rapid hydrolysis is required in order to load high concentrations of the reactants into the internal phase before significant shell formation.

  18. Preparation of silica or alumina pillared crystalline titanates

    SciTech Connect

    Udomsak, S.; Nge, R.; Dufner, D.C.; Anthony, R.G.; Lott, S.E.

    1994-05-01

    Layered crystalline titanates (CT) [Anthony and Dosch, US Patent 5 177 045 (1993)] are pillared with tetraethyl orthosilicate, 3-aminopropyltrimethoxysilane, and aluminum acetylacetonate to prepare porous and high surface area supports for sulfided NiMo catalyst. Tetra-ethyl orthosilicate or aluminum acetylacetonate intercalated CT are prepared by stepwise intercalation. First, the basal distance is increased by n-alkylammonium ions prior to intercalation with inorganic compounds. However, an aqueous solution of 3-aminopropyltrimethoxysilane could directly pillar CT without first swelling the titanate with n-alkylamine. The catalytic activities for hydrogenation of pyrene of sulfided NiMo supported silica or alumina pillared CT were higher than those of commercial catalysts (Shell324 and Amocat1C). The silicon and aluminum contents of the pillared CT, used as supports, have a considerable effect on the catalytic activities and physical properties of the supports.

  19. Nanosized microporous crystals: emerging applications.

    PubMed

    Mintova, Svetlana; Jaber, Maguy; Valtchev, Valentin

    2015-10-21

    This review highlights recent developments in the synthesis and unconventional applications of nanosized microporous crystals including framework (zeolites) and layered (clays) type materials. Owing to their microporous nature nanosized zeolites and clays exhibit novel properties, different from those of bulk materials. The factors controlling the formation of nanosized microporous crystals are first revised. The most promising approaches from the viewpoint of large-scale production of nanosized zeolites and clays are discussed in depth. The preparation and advanced applications of nanosized zeolites and clays in free (suspension and powder forms) and fixed (films) forms are summarized. Further the review emphasises the non-conventional applications of new porous materials. A comprehensive analysis of the emerging applications of microporous nanosized crystals in the field of semiconductor industry, optical materials, chemical sensors, medicine, cosmetics, and food industry is presented. Finally, the future needs and perspectives of nanosized microporous materials (zeolites and clays) are addressed.

  20. Preparation, characterization, and silanization of 3D microporous PDMS structure with properly sized pores for endothelial cell culture.

    PubMed

    Zargar, Reyhaneh; Nourmohammadi, Jhamak; Amoabediny, Ghassem

    2016-01-01

    Nowadays, application of porous polydimethylsiloxane (PDMS) structure in biomedical is becoming widespread, and many methods have been established to create such structure. Although the pores created through these methods are mostly developed on the outer surface of PDMS membrane, this study offers a simple and cost-efficient technique for creating three-dimensional (3D) microporous PDMS structure with appropriate pore size for endothelial cell culture. In this study, combination of gas foaming and particulate leaching methods, with NaHCO3 as effervescent salt and NaCl as progen are used to form a 3D PDMS sponge. The in situ chemical reaction between NaHCO3 and HCl resulted in the formation of small pores and channels. Moreover, soaking the samples in HCl solution temporarily improved the hydrophilicity of PDMS, which then facilitated the penetration of water for further leaching of NaCl. The surface chemical modification process was performed by (3-aminopropyl)triethoxysilane to culture endothelial cells on porous PDMS matrix. The results are an indication of positive response of endothelial cells to the fabricated PDMS sponge. Because of simplicity and practicality of this method for preparing PDMS sponge with appropriate pore size and biological properties, the fabricated matrix can perfectly be applied to future studies in blood-contacting devices.

  1. Effect of preparation parameters on the microporous structure of Ni/SiO{sub 2} catalysts

    SciTech Connect

    Castillon, F.F.; Bodganchikova, N.; Fuentes, S.; Avalos, M.

    1996-12-31

    In this work the authors report the synthesis of Ni/SiO{sub 2} catalysts promoted by group 2 (IIA) cations (calcium and barium) which are currently used as hydrogenation catalysts. The effect of the preparation parameters-aging, base agent, and type of cation, on the surface area of catalysts--is evaluated. Catalysts were prepared by precipitation of the precursor silicic acid, along with nickel nitrate and calcium and barium carbonates, with NaOH, NH{sub 4}OH and Na{sub 2}CO{sub 3} as precipitating agents. Catalysts were characterized by diffuse reflectance spectra (DRS) and by BET-surface area measurements. Results are discussed in terms of sol-gel chemistry.

  2. Preparation and Application of Hollow Silica/magnetic Nanocomposite Particle

    NASA Astrophysics Data System (ADS)

    Wang, Cheng-Chien; Lin, Jing-Mo; Lin, Chun-Rong; Wang, Sheng-Chang

    The hollow silica/cobalt ferrite (CoFe2O4) magnetic microsphere with amino-groups were successfully prepared via several steps, including preparing the chelating copolymer microparticles as template by soap-free emulsion polymerization, manufacturing the hollow cobalt ferrite magnetic microsphere by in-situ chemical co-precipitation following calcinations, and surface modifying of the hollow magnetic microsphere by 3-aminopropyltrime- thoxysilane via the sol-gel method. The average diameter of polymer microspheres was ca. 200 nm from transmission electron microscope (TEM) measurement. The structure of the hollow magnetic microsphere was characterized by using TEM and scanning electron microscope (SEM). The spinel-type lattice of CoFe2O4 shell layer was identified by using XRD measurement. The diameter of CoFe2O4 crystalline grains ranged from 54.1 nm to 8.5 nm which was estimated by Scherrer's equation. Additionally, the hollow silica/cobalt ferrite microsphere possesses superparamagnetic property after VSM measurement. The result of BET measurement reveals the hollow magnetic microsphere which has large surface areas (123.4m2/g). After glutaraldehyde modified, the maximum value of BSA immobilization capacity of the hollow magnetic microsphere was 33.8 mg/g at pH 5.0 buffer solution. For microwave absorption, when the hollow magnetic microsphere was compounded within epoxy resin, the maximum reflection loss of epoxy resins could reach -35dB at 5.4 GHz with 1.9 mm thickness.

  3. Preparation, characterization, and catalytic activity of zirconocene bridged on surface of silica gel

    NASA Astrophysics Data System (ADS)

    El Majdoub, Lotfia; Shi, Yasai; Yuan, Yuan; Zhou, Annan; Abutartour, Abubaker; Xu, Qinghong

    2015-10-01

    Zirconocene catalyst supported on silica gel was prepared for olefin polymerization by surface modification of calcined silica with SiCl4, and the reaction between the modified silica and cyclopentadienyl sodium and ZrCl4. The catalyst was characterized by using Fourier-transform infrared (FT-IR) spectrometer, thermogravimetric (TG), and differential scanning calorimetric (DSC) analytic spectrometer. It was found that the metallocene structure could be formed and connected on silica surface by chemical bond. Initial catalytic tests showed that the supported metallocene was catalytically active (methylaluminoxane as a cocatalyst), producing polymer with higher molecular weight than the metallocene just immobilized on the surface of silica gel.

  4. Microporous Ni@NiO nanoparticles prepared by chemically dealloying Al3Ni2@Al nanoparticles as a high microwave absorption material

    NASA Astrophysics Data System (ADS)

    Pang, Yu; Xie, Xiubo; Li, Da; Chou, Wusheng; Liu, Tong

    2017-03-01

    The Al3Ni2@Al nanoparticles (NPs) were prepared from Ni45Al55 master alloy by hydrogen plasma-metal reaction method, and were subsequently dealloyed to produce porous Ni@NiO NPs of 36 nm. The pore size ranges from 0.7 to 1.6 nm, leading to large specific surface area of 69.5 m2/g and big pore volume of 0.507 cc/g. The saturation magnetization (MS) and coercivity (HC) of the microporous Ni@NiO NPs are 11.5 emu/g and 5.2 Oe. They exhibit high microwave absorption performance with a minimum reflection coefficient (RC) of -86.9 dB and an absorption bandwidth of 2.6 GHz (RC≤-10 dB) at thickness of 4.5 mm. The enhanced microwave absorption properties are attributed to the synergistic effect of the magnetic Ni core and dielectric NiO shell, and the micropore architecture. The NPs with micropore morphology and core/shell structure open a new way to modify the microwave absorption performance.

  5. Preparation and Characterization of Single Ion Conductors from High Surface Area Fumed Silica

    NASA Technical Reports Server (NTRS)

    Zhang, H.; Maitra, P.; Liu, B.; Wunder, S. L.; Lin, H.-P.; Salomon, M.; Hagedorn, Norman H. (Technical Monitor)

    2002-01-01

    Anions that can form dissociative salts with Li(+) have been prepared and covalently attached to high surface area fumed silica. When blended with polyethylene oxide (PEO), the functionalized fumed silica suppresses the crystallization of the PEO, provides dimensional stability, and serves as a single ion conductor. Since functionalized fumed silica is easily dispersed in common polar solvents, it can be incorporated in both the polymer electrolyte and the electrodes.

  6. Preparation and characterization of titania-deposited silica composite hollow fiber membranes with high hydrothermal stability.

    PubMed

    Kwon, Young-Nam; Kim, In-Chul

    2013-11-01

    Hydrothermal stability of a porous nickel-supported silica membrane was successfully improved by deposition of titania multilayers on colloidal silica particles embedded in the porous nickel fiber support. Porous nickel-supported silica membranes were prepared by means of a dipping-freezing-fast drying (DFF) method. The titania layers were deposited on colloidal silica particles by repeating hydrolysis and condensation reactions of titanium isopropoxide on the silica particle surfaces. The deposition of thin titania layers on the nickel-supported silica membrane was verified by various analytical tools. The water flux and the solute rejection of the porous Ni fiber-supported silica membranes did not change after titania layer deposition, indicating that thickness of titania layers deposited on silica surface is enough thin not to affect the membrane performance. Moreover, improvement of the hydrothermal stability in the titania-deposited silica membranes was confirmed by stability tests, indicating that thin titania layers deposited on silica surface played an important role as a diffusion barrier against 90 degrees C water into silica particles.

  7. Preparation of silica coatings heavily doped with spiropyran using perhydropolysilazane as the silica source and their photochromic properties.

    PubMed

    Yamano, Akihiro; Kozuka, Hiromitsu

    2009-04-30

    Silica coatings doped with spiropyran (SP) were prepared using xylene solutions of perhydropolysilazane (PHPS) as the silica source, where the SP-doped PHPS coatings were prepared by spin-coating and the PHPS-to-silica conversion was achieved by exposing the coatings to the vapor from aqueous ammonia at room temperature. The films could be heavily doped with SP at SP/(SP + PHPS) mass ratio as high as 0.2. The as-deposited SP-doped PHPS films were transparent and light-yellow, which turned to red as the PHPS-to-silica conversion proceeded, where the absorbance at 500 nm increased. When the films were stored in air in the dark for 73 h after the exposure treatment, the absorbance at 500 nm further increased, where the film turned from red to dark red. The SP-doped silica coatings thus obtained showed reversible photochromic reaction, where the absorbance at 500 nm decreased and increased when the films were irradiated with visible and ultraviolet light, respectively. The pencil hardness of the films was higher than 9H at a load of 1 kg, while significant amount of SP was leached out when the films were soaked in xylene.

  8. [Preparation of porous silica microspheres with high porosity using base-dissolving method].

    PubMed

    Zhao, Rui; Li, Xinhui; Liu, Guoquan

    2005-11-01

    A novel method was proposed and studied for the preparation of porous silica with high porosity using base-dissolving technology. The relationships between the removal of silica and the base concentration, the reaction temperature as well as the reaction time were evaluated. The amount of silica removed from silica spheres was increased and silica-dissolving rate was also accelerated along with the increase of NaOH concentration. This was due to the damage of some inner walls of the porous silica and the dissolution of small fragments into the base solution. The amount of silica removed was in direct proportion to the reaction temperature and reaction time. Moreover, the specific pore volumes were linearly increased along with the increase of the amount of silica removed. The treated silica particles remained as homogeneous spheres and the changes of the particle diameter were not observed. Under the optimized conditions with the NaOH solution of 1.25 mol/L, the reaction temperature of 25 degrees C and the reaction time of 3.0 h, the original silica spheres with the diameter of 4 - 5 microm, the pore size of 8 nm and the specific pore volume (V(p)) of 1.4 cm3/g were modified to the high-porosity silica with the diameter of 4 - 5 microm, the pore size of 14 nm and the V(p) of 3.2 cm3/g. The porosity of the silica microspheres was changed from 75% to 88%. This high-porosity silica was suitable for the preparation of high performance gel filtration packings.

  9. Preparation and characterization of microporous layers on titanium by anodization in sulfuric acid with and without hydrogen charging.

    PubMed

    Tanaka, Shin-ichi; Fukushima, Yuriko; Nakamura, Isao; Tanaki, Toshiyuki; Jerkiewicz, Gregory

    2013-04-24

    The formation of microporous oxide layers on titanium (Ti) by anodization in sulfuric acid (H2SO4) solution and the influence of prior hydrogen charging on their properties are examined using electrochemical techniques, scanning electron microscopy, grazing incident X-ray diffraction, and X-ray photoelectron spectroscopy. When Ti is anodized in 1 M aqueous H2SO4 solution at a high direct current (DC) potential (>150 V) for 1 min, a porous surface layer develops, and the process takes place with spark-discharge. Under these conditions, oxygen evolution at the Ti electrode proceeds vigorously and concurrently with the formation of anodic oxide. The oxygen gas layer adjacent to the Ti surface acts as an insulator and triggers spark-discharge; the latter stimulates the development of pores. In the absence of spark-discharge, the oxide layer has extended surface roughness but low porosity. A porous oxide layer can be prepared by applying a lower DC voltage (130 V) and without spark-discharge, but Ti requires prior hydrogen charging by cathodic polarization in 1 M aqueous H2SO4 solution. Mott-Schottky measurements indicate that the oxide layers are n-type semiconductors and that the charge carrier density in the anodic oxide layer on the hydrogen-charged Ti is lower than in the case of untreated Ti. The hydrogen charging also affects the flat band potential of the anodic oxide layers on Ti by increasing its value. The reduced charge carrier density brought about by hydrogen charging decreases the oxide layer conductivity and creates favorable conditions for its electrical breakdown that stimulates the development of pores. The porous layer on the hydrogen-charged Ti consists of anatase and rutile phases of TiO2; it has the same chemical composition as the porous layer obtained on untreated Ti. X-ray photoelectron spectroscopy measurements show that prior hydrogen charging does not affect the thickness of anodic oxides on Ti. The porous oxide layer on Ti enables the

  10. The preparation of core-shell magnetic silica nanospheres for enhancing magnetism and fluorescence intensity.

    PubMed

    Yoo, Jeong Ha; Kim, Jong Sung

    2013-11-01

    Recently, magnetic and luminescent composite silica with structure of micro- and nanospheres containing both magnetic (Fe3O4) nanoparticles (MPs) and quantum dots (QDs) has attracted great interests. In this study, we have prepared core-shell structure of silica spheres in which magnets are incorporated into silica core and QDs into a mesoporous silica shell by using C18-TMS (octade-cyltrimethoxysilane). MPs were synthesized by a co-precipitation method from ferrous and ferric solutions with a molecular ratio of 2:3. Monodisperse magnetic silica cores have been prepared via sol-gel reaction of TEOS (tetraethoxysilane) and water using base catalyst. The size of magnetic silica nanospheres was confirmed by dynamic laser light scattering system (DLS) and scanning electoron microscope (SEM). The pore volume and surface area were calculated by using BET after calcination. The core-shell structure plays an important role in providing more domains for MPs in silica Core and QDs in silica shell. QDs were incorporated into the mesoporous shell by hydrophobic interactions. Magnetic characterization was performed using a superconducting quantum interference device (SQUID). The optical properties of the particles were characterized with UV/Vis spectrometer, PL spectrometer, and fluorescence microscope.

  11. Preparation and performance of nano silica/Nafion composite membrane for proton exchange membrane fuel cells

    NASA Astrophysics Data System (ADS)

    Wang, Keping; McDermid, Scott; Li, Jing; Kremliakova, Natalia; Kozak, Paul; Song, Chaojie; Tang, Yanghua; Zhang, Jianlu; Zhang, Jiujun

    Composite membranes made from Nafion ionomer with nano phosphonic acid-functionalised silica and colloidal silica were prepared and evaluated for proton exchange membrane fuel cells (PEMFCs) operating at elevated temperature and low relative humidity (RH). The phosphonic acid-functionalised silica additive obtained from a sol-gel process was well incorporated into Nafion membrane. The particle size determined using transmission electron microscope (TEM) had a narrow distribution with an average value of approximately 11 nm and a standard deviation of ±4 nm. The phosphonic acid-functionalised silica additive enhanced proton conductivity and water retention by introducing both acidic groups and porous silica. The proton conductivity of the composite membrane with the acid-functionalised silica was 0.026 S cm -1, 24% higher than that of the unmodified Nafion membrane at 85 °C and 50% RH. Compared with the Nafion membrane, the phosphonic acid-functionalised silica (10% loading level) composite membrane exhibited 60 mV higher fuel cell performance at 1 A cm -2, 95 °C and 35% RH, and 80 mV higher at 0.8 A cm -2, 120 °C and 35% RH. The fuel cell performance of composite membrane made with 6% colloidal silica without acidic group was also higher than unmodified Nafion membrane, however, its performance was lower than the acid-functionalised silica additive composite membrane.

  12. A hydrothermal peroxo method for preparation of highly crystalline silica-titania photocatalysts.

    PubMed

    Krivtsov, Igor; Ilkaeva, Marina; Avdin, Viacheslav; Khainakov, Sergei; Garcìa, Jose R; Ordòñez, Salvador; Dìaz, Eva; Faba, Laura

    2015-04-15

    A new completely inorganic method of preparation of silica-titania photocatalyst has been described. It has been established that the addition of silica promotes crystallinity of TiO2 anatase phase. Relative crystallinity and TiO2 crystal size in the silica-titania particles increase with the silica content until SiO2/TiO2 molar ratio of 0.9, but at higher molar ratios they start to decrease. The single-source precursor containing peroxo titanic (PTA) and silicic acids has been proved to be responsible for high crystallinity of TiO2 encapsulated into amorphous silica. It has been proposed that peroxo groups enhance rapid formation of crystalline titania seeds, while silica controls their growth. It has been concluded from the TEM that the most morphologically uniform anatase crystallites covered with SiO2 particles are prepared at SiO2/TiO2 molar ratio of 0.4. This sample, according to (29)Si NMR, also shows the high content of hydroxylated silica Q(3) and Q(2) groups, and it is the most photocatalytically active in UV-assisted decomposition of methylene blue among the tested materials. It has been determined that the increase in the amount of the condensed Q(4) silica in the mixed oxides leads to the decrease in photocatalytic performance of the material, despite its better crystallinity. High crystallinity, low degree of incorporation of Ti atoms in SiO2 in the mixed oxide and adsorption of methylene blue in the vicinity of photoactive sites on the hydroxylated silica have been considered as the main factors determining the high degradation degree of methylene blue in the presence of silica-titania.

  13. [Preparation and enantioseparation performance of β-cyclodextrin-silica hybrid chiral stationary phases].

    PubMed

    Wang, Litao; Dong, Shuqing; Zhang Zhixin; Wang, Yangjun; Zhang, Xiaoli; Zhang, Xia; Zhang, Pengyun; Zhao, Liang

    2016-01-01

    A simple preparation method for β-cyclodextrin-silica hybrid chiral stationary phases was developed. Firstly, the β-cyclodextrin-silica derivative was synthesized by the reaction of 3-aminopropyltriethoxysilane and monochlorotriazinyl β-cyclodextrin under weak base condition. Spherical β-cyclodextrin-silica hybrid materials with β-cyclodextrin in the surface of pores by covalent bonding were prepared using 1,2-bis(triethoxysilyl) ethane and the β-cyclodextrin-silica derivative under the alkaline condition by one-step polymerization reaction. The β-Cyclodextrin-silica hybrid chiral stationary phases could be directly used as high performance liquid chromatographic packings after the template removal. The hybrid materials prepared in this paper possessed regular spherical morphology, good monodispersion, high specific surface area, good mechanical property, high chemical stability and simple preparation process. It combined the chiral recognition performance of β-cyclodextrin and the outstanding performance of organic-inorganic hybrid material. The effect of the composition, ratio and pH of mobile phase on chiral separation was investigated, and the best chiral separation conditions had been optimized. The baseline chiral separations for five chiral compounds were obtained under the optimal conditions. The results of enantioseparation showed that the hybrid chiral stationary phases had favorable chiral recognition ability. Compared with the traditional preparation process of chiral stationary phases, a new thought for new type of chiral stationary phase is provided by the present method in this paper.

  14. Hydrothermal preparation of hybrid carbon/silica monolithic capillary column for liquid chromatography.

    PubMed

    Yang, Peiling; Wang, Wentao; Xiao, Xing; Jia, Li

    2014-08-01

    A simple, easy and economical approach for the preparation of a hybrid carbon/silica monolithic capillary column was described for the first time by using silica monolith as framework in combination with hydrothermal carbonization at 180°C. During the preparation process, formamide was introduced to the reaction solutions to reduce the dissolution rate of monolithic silica skeleton and its optimal concentration was 1.5 M. Fourier transform infrared spectrometry, scanning electron microscopy, energy dispersive X-ray spectrometry, and inverse size exclusion chromatography were carried out to characterize the as-prepared column. The results demonstrated that carbon spheres ranging from 150 to 1000 nm were successfully attached to the surface of silica skeleton. The prepared hybrid carbon/silica column had a permeability of 4.4 × 10(-14) m(2). Chromatographic performance of the column was evaluated by separation of various compounds including alkylbenzenes, nucleosides and bases, and aromatic acids. The column exhibited an efficiency of 75,000 plates/m for butylbenzene at the optimal linear velocity of 0.23 mm/s. The successful separation of these compounds and the study on mechanism indicated that the column can be applied in mixed-mode chromatography.

  15. Self-immobilization and/or thermal treatment for preparing silica-poly(methyloctylsiloxane) stationary phases.

    PubMed

    Bottoli, Carla B G; Vigna, Camila R M; Fischer, Gerd; Albert, Klaus; Collins, Kenneth E; Collins, Carol H

    2004-03-19

    Batches of poly(methyloctylsiloxane) (PMOS)-loaded silica were prepared by the deposition of PMOS, into the pores of HPLC silica. Portions of PMOS-loaded silica were allowed to remain at ambient temperature, without further treatment for 2, 9, 20, 31, 51, 105 and 184 days after preparation to undergo self-immobilization (irreversible adsorption of a layer of polymer on silica at ambient temperature in the absence of initiators). Other portions were subjected to a thermal treatment (100 degrees C for 4h) after 1, 2, 5, 7, 9, 15, 20, 25, 70, 111 and 184 days. Self-immobilized and thermally treated samples were characterized by % C, 29Si cross-polarization magic angle spinning (CP/MAS) NMR spectroscopy and reversed-phase column performance. The results show that thermal immobilization accelerates the distribution and rearrangement of the polymer on the silica surface. However, from the time that a monolayer has been formed by self-immobilization (approximately 100 days for PMOS on Kromasil silica), the thermal treatment does not alter this configuration and, thus, does not change the resulting chromatographic parameters.

  16. Facile preparation of mesoporous carbon-silica-coated graphene for the selective enrichment of endogenous peptides.

    PubMed

    Zhang, Quanqing; Zhang, Qinghe; Xiong, Zhichao; Wan, Hao; Chen, Xiaoting; Li, Hongmei; Zou, Hanfa

    2016-01-01

    A sandwich-like composite composed of ordered mesoporous carbon-silica shell-coated graphene (denoted as graphene@mSiO2-C) was prepared by an in-situ carbonation strategy. A mesoporous silica shell was synthesized by a sol-gel method, and cetyltrimethyl ammonium bromide inside the mesopores were in-situ carbonized as a carbon source to obtain a carbon-silica shell. The resulting mesoporous carbon-silica material with a sandwich structure possesses a high surface area (600 m(2) g(-1)), large pore volume (0.587 cm(3) g(-1)), highly ordered mesoporous pore (3 nm), and high carbon content (30%). This material shows not only high hydrophobicity of graphene and mesoporous carbon but also a hydrophilic silica framework that ensures excellent dispersibility in aqueous solution. The material can capture many more peptides from bovine serum albumin tryptic digests than mesoporous silica shell-coated graphene, demonstrating great enrichment efficiency for peptides. Furthermore, the prepared composite was applied to the enrichment of low-abundance endogenous peptides in human serum. Based on Matrix-Assisted Laser Desorption/ Ionization Time of Flight Mass Spectrometry identification, the graphene@mSiO2-C could efficiently size-exclude proteins and enriches the low-abundant peptides on the graphene and mesoporous carbon. And based on the LC-MS/MS results, 892 endogenous peptides were obtained by graphene@mSiO2-C, hinting at its great potential in peptides analysis.

  17. In vitro efficacies of oils, silicas and plant preparations against the poultry red mite Dermanyssus gallinae.

    PubMed

    Maurer, Veronika; Perler, Erika; Heckendorn, Felix

    2009-06-01

    The aim of this study was to test the effectiveness of physically acting substances (oils and silicas) and plant preparations for the control of the poultry red mite Dermanyssus gallinae (De Geer 1778). Reproduction and survival of fed D. gallinae females were evaluated in vitro for a total of 168 h using the "area under the survival curve" (AUC) to compare survival of the mites between treatments. Four oils (two plant oils, one petroleum spray oil and diesel), one soap, three silicas (one synthetic amorphous silica, one diatomaceous earth (DE) and one DE with 2% pyrethrum extract) and seven plant preparations (derived from Chrysanthemum cineariaefolium, Allium sativum, Tanacetum vulgare, Yucca schidigera, Quillaja saponaria, Dryopteris filix-mas, and Thuja occidentalis) were tested at various concentrations. All the oils, diesel and soap significantly reduced D. gallinae survival. All silicas tested inhibited reproduction. DE significantly reduced mite survival, but amorphous silica was less effective in vitro. Except for pure A. sativum juice and the highest concentration of C. cineariaefolium extract, the plant preparations tested resulted in statistically insignificant control of D. gallinae.

  18. Fabrication of Hollow Microporous Carbon Spheres from Hyper-Crosslinked Microporous Polymers.

    PubMed

    Wang, Kewei; Huang, Liang; Razzaque, Shumaila; Jin, Shangbin; Tan, Bien

    2016-06-01

    Porous carbon materials prepared from the porous organic polymers are currently the subject of extensive investigation. On the basis of their interesting applications, it is highly desirable to develop new synthetic methodologies to obtain carbon materials with controllable pore size and morphology. Herein, a facile synthesis of hollow microporous carbon spheres (HCSs) from hollow microporous organic capsules (HMOCs) with a good control over the pore morphology, hollow cavity, and the shell thickness is reported. The highly porous hollow carbon spheres are prepared by the pyrolysis of HMOCs-based microporous polymers. The synthetic parameters, such as hypercrosslinking and pyrolysis conditions, are optimized to modify the porous structures and the properties. The morphology and porosity as well as energy storage applications of the microporous structures HCSs, derived through a combination of divinylbenzene-crosslinking and micropore-generating hypercrosslinking, are discussed. These findings provide a new benchmark for fabricating well-defined HCSs with great promise for various applications.

  19. Moisture Transport in Silica Gel Particle Beds: I. Theoretical Study

    SciTech Connect

    Pesaran, A. A.; Mills, A. F.

    1986-08-01

    Diffusion mechanisms of moisture within silica gel particles are investigated. It is found that for microporous silica gel surface diffusion is the dominant mechanism of moisture transport, while for macroporous silica gel both Knudsen and surface diffusion are important.

  20. [Response surface method optimize of nano-silica solid dispersion technology assistant enzymatic hydrolysis preparation genistein].

    PubMed

    Jin, Xin; Zhang, Zhen-Hai; Zhu, Jing; Sun, E; Yu, Dan-Hong; Chen, Xiao-Yun; Liu, Qi-Yuan; Ning, Qing; Jia, Xiao-Bin

    2012-04-01

    This article reports that nano-silica solid dispersion technology was used to raise genistein efficiency through increasing the enzymatic hydrolysis rate. Firstly, genistin-nano-silica solid dispersion was prepared by solvent method. And differential scanning calorimetry (DSC) and transmission electron microscopy (TEM) were used to verify the formation of solid dispersion, then enzymatic hydrolysis of solid dispersion was done by snailase to get genistein. With the conversion of genistein as criteria, single factor experiments were used to study the different factors affecting enzymatic hydrolysis of genistin and its solid dispersion. And then, response surface method was used to optimize of nano-silica solid dispersion technology assistant enzymatic hydrolysis. The optimum condition to get genistein through enzymatic hydrolysis of genistin-nano-silica solid dispersion was pH 7.1, temperature 52.2 degrees C, enzyme concentration 5.0 mg x mL(-1) and reaction time 7 h. Under this condition, the conversion of genistein was (93.47 +/- 2.40)%. Comparing with that without forming the genistin-nano-silica solid dispersion, the conversion increased 2.62 fold. At the same time, the product of hydrolysis was purified to get pure genistein. The method of enzymatic hydrolysis of genistin-nano-silica solid dispersion by snailase to obtain genistein is simple, efficiency and suitable for the modern scale production.

  1. Highly ordered poly(thiophene)s prepared in mesoporous silica nanoparticles.

    PubMed

    Seo, Seogjae; Kim, Jeonghun; Kim, Byeonggwan; Vinu, Ajayan; Kim, Eunkyoung

    2011-05-01

    Nanostructured PEDOT was synthesized using mesoporous silica as a nano-template. The polymerization of thiophene monomers was performed with an oxidant and mesoporous silica nanoparticles. The silica particles took essential role in absorbing monomers and oxidant molecules, and growth of polymers inside their pores. As prepared polymer/silica composite was treated with HF solution to remove silica template to result in 1D wire structure and mesh type porous 3D structures from SBA-15 and KIT-6 template, respectively. The average size of the poly(thiophene) wires was 10 15 nm, which was matched well to the pores size of the silica templates, as determined from an electron microscopy. At optimized condition, the room temperature electrical conductivities of the PEDOT grown from SBA-15 and KIT-6 template were similar as 1.1 and 1.0 S/cm, respectively. However, the evolution of the PEDOT conductivity versus temperature was different depending on the templates. These results gave a unique chance to tailor made 3 dimensional structure as well as properties of conductive polymer.

  2. Effect of various structure directing agents on the physicochemical properties of the silica aerogels prepared at an ambient pressure

    NASA Astrophysics Data System (ADS)

    Sarawade, Pradip B.; Shao, Godlisten N.; Quang, Dang Viet; Kim, Hee Taik

    2013-12-01

    We studied the effects of various surfactants on the textural properties (BET surface area, pore size, and pore volume) of the silica aerogels prepared at an ambient pressure. A simple surface modification of silica gel prepared at an ambient pressure through hydrolysis and polycondensation of TEOS as a silica precursor was conducted using various structure directing agents. The treatment was found to induce a significant difference in the porosity of the silica aerogel. Highly porous silica aerogels with bimodal porous structures were prepared by modifying the surface of the silica wet-gel (alcogel) with trimethylchlorosilane (TMCS) in order to preserve its porosity. The samples were analyzed by small-angle X-ray scattering and nitrogen adsorption. In this work, a possible new type of highly porous hydrophobic silica aerogel with a bimodal porous structure is presented. A hydrophilic extremely porous (high surface area and large pore volume) silica aerogel was obtained by heating the as-synthesized hydrophobic silica aerogel at 400 °C for 1 h. There was a significant effect of structure directing agent on the textural properties, such as specific surface area, pore size distribution and cumulative pore volume of the silica aerogels.

  3. Preparation of monolithic silica-chitin composite under extreme biomimetic conditions.

    PubMed

    Bazhenov, Vasilii V; Wysokowski, Marcin; Petrenko, Iaroslav; Stawski, Dawid; Sapozhnikov, Philipp; Born, René; Stelling, Allison L; Kaiser, Sabine; Jesionowski, Teofil

    2015-05-01

    Chitin is a widespread renewable biopolymer that is extensively distributed in the natural world. The high thermal stability of chitin provides an opportunity to develop novel inorganic-organic composites under hydrothermal synthesis conditions in vitro. For the first time, in this work we prepared monolithic silica-chitin composite under extreme biomimetic conditions (80°C and pH 1.5) using three dimensional chitinous matrices isolated from the marine sponge Aplysina cauliformis. The resulting material was studied using light and fluorescence microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy. A mechanism for the silica-chitin interaction after exposure to these hydrothermal conditions is proposed and discussed.

  4. Silica coating of luminescent quantum dots prepared in aqueous media for cellular labeling

    SciTech Connect

    Ma, Yunfei; Li, Yan Zhong, Xinhua

    2014-12-15

    Graphical abstract: A facile route based on modified Stöber method was used for the synthesis of silica coated QDs (QD@SiO{sub 2}) starting from aqueously prepared CdTe/CdS QDs. The resultant QD@SiO{sub 2} exhibited a significant increase in emission efficiency compared with that of the initial QDs, along with a small size (∼5 nm in diameter), great stability and low cytotoxicity, which makes it a good candidate as robust biomarker. - Highlights: • We present a facile modified Stöber method to prepare highly luminescent QD@SiO{sub 2}. • The PL efficiency of QDs increases significantly after silica coating. • QD@SiO{sub 2} exhibits small size (∼5 nm) and great dispersibility in aqueous solution. • QD@SiO{sub 2} presents extraordinary photo and colloidal stability. • The silica shell eliminates QD cytotoxicity, providing the access of bioconjugation. - Abstract: Silica coating is an effective approach for rendering luminescent quantum dots (QDs) with water dispersibility and biocompatibility. However, it is still challenging to prepare silica-coated QDs (QD@SiO{sub 2}) with high emission efficiency, small size and great stability in favor for bioapplication. Herein, we reported a modified Stöber method for silica coating of aqueously-prepared CdTe/CdS QDs. With the coexistence of Cd{sup 2+} and thioglycolic acid (TGA), a thin silica shell was formed around QDs by the hydrolysis of tetraethyl orthosilicate (TEOS). The resultant QD@SiO{sub 2} with a small size (∼5 nm in diameter) exhibits significantly higher emission efficiencies than that of the initial QDs. Also, QD@SiO{sub 2} has extraordinary photo and colloidal stability (pH range of 5–13, 4.0 M NaCl solution). Protected by the silica shell, the cytotoxicity of QDs could be reduced. Moreover, the QD@SiO{sub 2} conjugated with folic acid (FA) presents high specific binding toward receptor-positive HeLa cells over receptor-negative A549 cells.

  5. Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia

    NASA Astrophysics Data System (ADS)

    Ward, Antony J.; Pujari, Ajit A.; Costanzo, Lorenzo; Masters, Anthony F.; Maschmeyer, Thomas

    2011-12-01

    A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

  6. Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia

    PubMed Central

    2011-01-01

    A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%. PMID:21711725

  7. Preparation of Metalloporphyrin-Bound Superparamagnetic Silica Particles via "Click" Reaction.

    PubMed

    Hollingsworth, Javoris V; Bhupathiraju, N V S Dinesh K; Sun, Jirun; Lochner, Eric; Vicente, M Graça H; Russo, Paul S

    2016-01-13

    A facile approach using click chemistry is demonstrated for immobilization of metalloporphyrins onto the surface of silica-coated iron oxide particles. Oleic-acid stabilized iron oxide nanocrystals were prepared by thermal decomposition of iron(III) acetylacetonate. Their crystallinity, morphology, and superparamagnetism were determined using X-ray diffraction, transmission electron microscopy, and a superconducting quantum interference device. Monodisperse core-shell particles were produced in the silica-coating of iron oxide via microemulsion synthesis. Surface modification of these particles was performed in two steps, which included the reaction of silica-coated iron oxide particles with 3-bromopropyltrichlorosilane, followed by azido-functionalization with sodium azide. Monoalkylated porphyrins were prepared using the Williamson ether synthesis of commercially available tetra(4-hydroxyphenyl) porphyrin with propargyl bromide in the presence of a base. (1)H NMR and matrix-assisted laser desorption ionization confirmed the identity of the compounds. The prepared monoalkyne porphyrins were zinc-metalated prior to their introduction to azide-functionalized, silica-coated iron oxide particles in the click reaction. X-ray photoelectron spectroscopy, thermogravimetric analysis, and Fourier transform infrared spectroscopy were used to characterize the surface chemistry after each step in the reaction. In addition, particle size was determined using dynamic light scattering and microscopy. The presented methodology is versatile and can be extended to other photoreactive systems, such as phthalocyanines and boron-dipyrromethane, which may lead to new materials for optical, photonic, and biological applications.

  8. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    NASA Astrophysics Data System (ADS)

    Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

    2014-11-01

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound.

  9. A simple method for preparation of transparent hydrophobic silica-based coatings on different substrates

    NASA Astrophysics Data System (ADS)

    Wang, Fang; Wang, Xiufang; Xie, Anjian; Shen, Yuhua; Duan, Wei; Zhang, Ye; Li, Jialin

    2012-01-01

    A facile, inexpensive, and general approach is explored for the fabrication of transparent silica/organic silicon hybrid sol, which could form transparent hydrophobic coatings on different substrates conveniently. The sol was prepared by using hexamethyldisilazane (HMDS) as a surface-modifying agent and the source of base catalyst required for the hydrolysis of tetraethoxysilane (TEOS). The resulting silica-based coatings on glass slide have shown an optical transmission over the visible range up to 89% (in reference to 100% transmission defined by a plain glass substrate) and high thermal stability. The water contact angle of the film reached 152○. Hydrophobic coatings with excellent optical transmittance were also successfully formed on writing paper and aluminum foils. The transparent hydrophobic silica-based hybrid sol will have potential applications in creating outdoor building glass, protecting paper files from moisture and preventing metals from corrosion.

  10. Feasibility of the preparation of silica monoliths for gas chromatography: fast separation of light hydrocarbons.

    PubMed

    Azzouz, Imadeddine; Essoussi, Anouar; Fleury, Joachim; Haudebourg, Raphael; Thiebaut, Didier; Vial, Jerome

    2015-02-27

    The preparation conditions of silica monoliths for gas chromatography were investigated. Silica-based monolithic capillary columns based on sol-gel process were tested in the course of high-speed gas chromatographic separations of light hydrocarbons mixture (C1-C4). The impact of modifying the amount of porogen and/or catalyst on the monolith properties were studied. At the best precursor/catalyst/porogen ratio evaluated, a column efficiency of about 6500 theoretical plates per meter was reached with a very good resolution (4.3) for very light compounds (C1-C2). The test mixture was baseline separated on a 70cm column. To our knowledge for the first time a silica-based monolithic capillary column was able to separate light hydrocarbons from methane to n-butane at room temperature with a back pressure in the range of gas chromatography facilities (under 4.1bar).

  11. Preparation of bifunctional mesoporous silica nanoparticles by orthogonal click reactions and their application in cooperative catalysis.

    PubMed

    Dickschat, Arne T; Behrends, Frederik; Bühner, Martin; Ren, Jinjun; Weiss, Mark; Eckert, Hellmut; Studer, Armido

    2012-12-21

    The synthesis of bifunctional mesoporous silica nanoparticles is described. Two chemically orthogonal functionalities are incorporated into mesoporous silica by co-condensation of tetraethoxysilane with two orthogonally functionalized triethoxyalkylsilanes. Post-functionalization is achieved by orthogonal surface chemistry. A thiol-ene reaction, Cu-catalyzed 1,3-dipolar alkyne/azide cycloaddition, and a radical nitroxide exchange reaction are used as orthogonal processes to install two functionalities at the surface that differ in reactivity. Preparation of mesoporous silica nanoparticles bearing acidic and basic sites by this approach is discussed. Particles are analyzed by solid state NMR spectroscopy, elemental analysis, infrared-spectroscopy, and scanning electron microscopy. As a first application, these particles are successfully used as cooperative catalysts in the Henry reaction.

  12. Silica hydride intermediate for octadecylsilica and phenyl bonded phase preparation via heterogeneous hydrosilation in supercritical carbon dioxide.

    PubMed

    Scully, N M; Ashu-Arrah, B A; Nagle, A P; Omamogho, J O; O'Sullivan, G P; Friebolin, V; Dietrich, B; Albert, K; Glennon, J D

    2011-04-15

    Investigations into the preparation of silica hydride intermediate in supercritical carbon dioxide (sc-CO(2)) that avoids the use of organic solvents such as toluene or dioxane are described. The effects of reaction temperature, pressure and time on the surface coverage of the supercritical fluid generated silica hydride intermediate were studied. Under optimised supercritical conditions of 120°C, 483 bar and 3 h reaction time, silica hydride (Si-H) conversion efficiencies of ca. 40% were achieved for the hydride intermediate prepared from a monofunctional silane reagent (dimethylmethoxysilane). Si-H conversion efficiencies (as determined from (29)Si CP-MAS NMR spectral analysis) for the hydride intermediate prepared from triethoxysilane (TES) in sc-CO(2) were found to be comparable to those obtained using a TES silanisation approach in an organic solvent. (13)C and (29)Si CP-MAS-NMR spectroscopy was employed to provide a complete structural assignment of the silica hydride intermediates. Furthermore, supercritical CO(2) was subsequently employed as a reaction medium for the heterogenous hydrosilation of silica hydride with octadecene and with styrene, in the presence of a free radical initiator. These supercritical fluid generated reversed-phase materials were prepared in a substantially reduced reaction time (3 h) compared to organic solvent based methods (100 h reaction time). Silica functionalisation in sc-CO(2) presents an efficient and clean alternative to organic solvent based methods for the preparation of important silica hydride intermediate and silica bonded stationary phases via a hydrosilation approach.

  13. Preparation of silver nanoparticle containing silica micro beads and investigation of their antibacterial activity

    NASA Astrophysics Data System (ADS)

    Quang, Dang Viet; Sarawade, Pradip B.; Hilonga, Askwar; Kim, Jong-Kil; Chai, Young Gyu; Kim, Sang Hoon; Ryu, Jae-Yong; Kim, Hee Taik

    2011-05-01

    Silver nanoparticle containing silica micro beads (Ag-NPBs) were successfully prepared by using sodium silicate, a cheap precursor, involving chemical reductive method. First, silica gel was synthesized and crushed into micro beads which have sizes ranging from 0.5 to 1 mm. Silica micro beads were then modified with 3-aminopropyltriethoxysilane to graft amino functional groups onto their surface. Silver ions were loaded onto the surface of the modified silica and reduced to silver crystal by adding NaBH 4. The presence of silver nanoparticles as well as structure of materials was characterized with FT-IR, XRD, BET, FE-SEM, TEM, UV-vis spectrophotometer, and optical microscope. Silver nanoparticles with an average size about 5 nm were found in the pore and on the surface of amino functionalized silica beads. Ag-NPBs samples were tested for their antibacterial activity against Escherichia coli ( E. coli). The antibacterial activity was examined by both zone inhibition and test tube test method. Biological results indicated that the synthesized materials have an excellent antibacterial performance against E. coli which was completely inhibited after 5 min contact with Ag-NPBs.

  14. Preparation and characterization of hydrophobic silica aerogel sphere products by co-precursor method

    NASA Astrophysics Data System (ADS)

    Yu, Huijun; Liang, Xiaofeng; Wang, Junxia; Wang, Minmin; Yang, Shiyuan

    2015-10-01

    In the present paper, silica aerogel balls were prepared using methyltriethoxysilane (MTES) and tetraethoxysilane (TEOS) co-precursor with different MTES/TEOS molar ratio (I) by two-step acid-base catalyzed sol-gel process and molding technology followed by the carbon dioxide supercritical drying. The physical properties of various silica aerogels whose I varied from 0 to 1.0 were studied by BET and SEM. Approving aerogel ball was obtained by using acetone as exchanging solvent at I of 0.8. Better properties are less crack, little shrinking percentage (17%), low apparent density (0.103 g/cm3), large surface area (996.35 m2/g) and high pore volume (3.32 cm3/g). Characterized by contact angle measurements and thermal stability, the characterizations of aerogel spheres were strongly affected by the MTES/TEOS molar ratio. Hydrophobic property increased with the increase in I value, and silica aerogels at I = 0.8 and 1.0 have a superhydrophobic characterization with the highest contact angle (152°). The TG-DTA analysis shows that the silica aerogel spheres transform hydrophobic to hydrophilic at around 450 °C, which is due to oxidation of Si-CH3 to Si-OH groups. The surface chemical modification was confirmed by FT-IR spectrums, which demonstrated that Si-CH3 groups be beneficial to molding of silica aerogels.

  15. Preparation of antibacterial composite material of natural rubber particles coated with silica and titania

    NASA Astrophysics Data System (ADS)

    Wisutiratanamanee, Apisit; Poompradub, Sirilux; Poochinda, Kunakorn

    2014-06-01

    Silica coating, followed by titania coating, was performed over spray-dried natural rubber (NR) compound for physical and anti-bacterial characterizations. Titania has a strong photo-oxidative catalytic property, which can disinfect bacteria, but may degrade NR. Therefore, silica coating was intended to form a barrier between NR and titania. First, NR particles were prepared by spray-drying of NR compound latex, formulated for household glove products, mixed with sodium dodecyl sulfate (SDS) to reduce particle agglomeration. The factorial experimental design was employed to investigate the effects of nozzle flow rate (500-700 Lh-1), inlet air temperature (110-150 °C), SDS content (35-55 phr) and mass flow rate (1.2-1.7 g rubber/min) on NR yield and moisture content. Then, the NR compound particles prepared at the optimum condition were coated with silica, using tetraethoxysilane (TEOS) as the precursor, by chemical vapor deposition (CVD) at 60 °C for 2-48 hours. Next, the particles were coated with titania using titanium tetrafluoride (TiF4) by liquid phase deposition (LPD) at 60 ºC for 4-8 hours. The NR composites were characterized for surface morphology by SEM, silica and titania content by TGA and EDX. The NR composites were found to cause more than 99% reduction of Escherichia coli and Staphylococcus aureus under 1-hour exposure to natural light.

  16. Preparing hydrophobic nanocellulose-silica film by a facile one-pot method.

    PubMed

    Le, Duy; Kongparakul, Suwadee; Samart, Chanatip; Phanthong, Patchiya; Karnjanakom, Surachai; Abudula, Abuliti; Guan, Guoqing

    2016-11-20

    Hydrophobic nanocellulose-silica film was successfully prepared by a facile one-pot method using tetraethoxysilane (TEOS) and dodecyl triethoxylsilane (DTES). Morphological characterization of the hydrophobic nanocellulose-silica (NC-SiO2-DTES) film showed well self-assembled DTES modified silica spherical nanoparticles with the particle sizes in the range of 88-126nm over the nanocellulose film. The hydrophobicity of the NC-SiO2-DTES film was achieved owing to the improvement of roughness of the nanocellulose film by coating dodecyl- terminated silica nanoparticles. An increase in DTES loading amount and reaction time increased the hydrophobicity of the film, and the optimum condition for NC-SiO2-DTES film preparation was achieved at DTES/TEOS molar ratio of 2.0 for 8h reaction time. Besides, the NC-SiO2-DTES film performed superoleophilic property with octane and hexadecane contact angles of 0°. It also showed an excellent hydrophobic property over all pH values ranged from 1 to 14.

  17. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    SciTech Connect

    Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

    2014-11-15

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol.

  18. Sol-gel preparation of silica and titania thin films

    NASA Astrophysics Data System (ADS)

    Thoř, Tomáš; Václavík, Jan

    2016-11-01

    Thin films of silicon dioxide (SiO2) and titanium dioxide (TiO2) for application in precision optics prepared via the solgel route are being investigated in this paper. The sol-gel process presents a low cost approach, which is capable of tailoring thin films of various materials in optical grade quality. Both SiO2 and TiO2 are materials well known for their application in the field of anti-reflective and also highly reflective optical coatings. For precision optics purposes, thickness control and high quality of such coatings are of utmost importance. In this work, thin films were deposited on microscope glass slides substrates using the dip-coating technique from a solution based on alkoxide precursors of tetraethyl orthosilicate (TEOS) and titanium isopropoxide (TIP) for SiO2 and TiO2, respectively. As-deposited films were studied using spectroscopic ellipsometry to determine their thickness and refractive index. Using a semi-empirical equation, a relationship between the coating speed and the heat-treated film thickness was described for both SiO2 and TiO2 thin films. This allows us to control the final heat-treated thin film thickness by simply adjusting the coating speed. Furthermore, films' surface was studied using the white-light interferometry. As-prepared films exhibited low surface roughness with the area roughness parameter Sq being on average of 0.799 nm and 0.33 nm for SiO2 and TiO2, respectively.

  19. Incorporation of anti-inflammatory agent into mesoporous silica

    NASA Astrophysics Data System (ADS)

    Rodrigues Braz, Wilson; Lamec Rocha, Natállia; de Faria, Emerson H.; Silva, Márcio L. A. e.; Ciuffi, Katia J.; Tavares, Denise C.; Furtado, Ricardo Andrade; Rocha, Lucas A.; Nassar, Eduardo J.

    2016-09-01

    The unique properties of macroporous, mesoporous, and microporous systems, including their ability to accommodate molecules of different sizes inside their pores and to act as drug delivery systems, have been the object of extensive studies. In this work, mesoporous silica with hexagonal structure was obtained by template synthesis via the sol-gel process. The resulting material was used as support to accommodate the anti-inflammatory agent indomethacin. The alkaline route was used to prepare the mesoporous silica; cetyltrimethylammonium bromide was employed as porogenic agent. The silica particles were functionalized with 3-aminopropyltriethoxysilane alkoxide (APTES) by the sol-gel post-synthesis method. Indomethacin was incorporated into the silica functionalized with APTES and into non-functionalized silica. The resulting systems were characterized by x-ray diffraction (XRD), specific area, infrared spectroscopy, and thermal analyses (TGA). XRD attested to formation of mesoporous silica with hexagonal structure. This structure remained after silica functionalization with APTES and incorporation of indomethacin. Typical infrared spectroscopy vibrations and organic material decomposition during TGA confirmed silica functionalization and drug incorporation. The specific surface area and pore volume of the functionalized material incorporated with indomethacin decreased as compared with the specific surface area and pore volume of the non-functionalized silica containing no drug, suggesting both the functionalizing agent and the drug were present in the silica. Cytotoxicity tests conducted on normal fibroblasts (GM0479A) cells attested that the silica matrix containing indomethacin was less toxic than the free drug.

  20. Incorporation of anti-inflammatory agent into mesoporous silica.

    PubMed

    Braz, Wilson Rodrigues; Rocha, Natállia Lamec; de Faria, Emerson H; Silva, Márcio L A E; Ciuffi, Katia J; Tavares, Denise C; Furtado, Ricardo Andrade; Rocha, Lucas A; Nassar, Eduardo J

    2016-09-23

    The unique properties of macroporous, mesoporous, and microporous systems, including their ability to accommodate molecules of different sizes inside their pores and to act as drug delivery systems, have been the object of extensive studies. In this work, mesoporous silica with hexagonal structure was obtained by template synthesis via the sol-gel process. The resulting material was used as support to accommodate the anti-inflammatory agent indomethacin. The alkaline route was used to prepare the mesoporous silica; cetyltrimethylammonium bromide was employed as porogenic agent. The silica particles were functionalized with 3-aminopropyltriethoxysilane alkoxide (APTES) by the sol-gel post-synthesis method. Indomethacin was incorporated into the silica functionalized with APTES and into non-functionalized silica. The resulting systems were characterized by x-ray diffraction (XRD), specific area, infrared spectroscopy, and thermal analyses (TGA). XRD attested to formation of mesoporous silica with hexagonal structure. This structure remained after silica functionalization with APTES and incorporation of indomethacin. Typical infrared spectroscopy vibrations and organic material decomposition during TGA confirmed silica functionalization and drug incorporation. The specific surface area and pore volume of the functionalized material incorporated with indomethacin decreased as compared with the specific surface area and pore volume of the non-functionalized silica containing no drug, suggesting both the functionalizing agent and the drug were present in the silica. Cytotoxicity tests conducted on normal fibroblasts (GM0479A) cells attested that the silica matrix containing indomethacin was less toxic than the free drug.

  1. Using Silica Sol as a Nanoglue to Prepare Nanoscale Mesoporous Composite Gel and Aerogels

    DTIC Science & Technology

    2000-03-31

    entitled: "USING SILICA SOL AS A NANOGLUE TO PREPARE NANOSCALE MESOPOROUS COMPOSITE GEL AND AEROGELS" Request for release for publication. REF...L. Anderson, Karen E. Swider Lyons, Ceha I. Merzbacher, Joseph V. Ryan and Veronica M. Cepak 3 MESOPOROUS COMPOSITE GELS AND AEROGELS 4 5 6 1...to mesoporous composite gels and aerogels and their various uses. 9 10 2. Description of the Background Art 11 Xerogels and aerogels

  2. A new generation of more pH stable reversed phases prepared by silanization of zirconized silica.

    PubMed

    Silva, César R; Airoldi, Claudio; Collins, Kenneth E; Collins, Carol H

    2008-05-16

    To further extend our studies in the search for reversed phases with enhanced durability at high pH, zirconized silica has now been explored as an alternative support. The synthesis of the new stationary phases involves silanization of a zirconium-modified silica support with a C(18) trifunctional silane, followed by endcapping. The chromatographic properties of the C(18) phases based on zirconized silica are similar to their titanized silica counterparts. Accelerated high pH stability tests, using phosphate mobile phases and elevated temperature, have shown that the zirconized silica phases have promising advantages not only over similarly prepared non-metalized phases but also over titanized silica C(18) phases.

  3. Microporous activated carbons prepared from palm shell by thermal activation and their application to sulfur dioxide adsorption.

    PubMed

    Guo, Jia; Lua, Aik Chong

    2002-07-15

    Textural characterization of activated carbons prepared from palm shell by thermal activation with carbon dioxide (CO(2)) gas is reported in this paper. Palm shell (endocarp) is an abundant agricultural solid waste from palm-oil processing mills in many tropical countries such as Malaysia, Indonesia, and Thailand. The effects of activation temperature on the textural properties of the palm-shell activated carbons, namely specific surface area (BET method), porosity, and microporosity, were investigated. The activated carbons prepared from palm shell possessed well-developed porosity, predominantly microporosity, leading to potential applications in gas-phase adsorption for air pollution control. Static and dynamic adsorption tests for sulfur dioxide (SO(2)), a common gaseous pollutant, were carried out in a thermogravimetric analyzer and a packed column configuration respectively. The effects of adsorption temperature, adsorbate inlet concentration, and adsorbate superficial velocity on the adsorptive performance of the prepared activated carbons were studied. The palm-shell activated carbon was found to have substantial capability for the adsorption of SO(2), comparable to those of some commercial products and an adsorbent derived from another biomass.

  4. Characteristics of microporous/mesoporous carbons prepared from rice husk under base- and acid-treated conditions.

    PubMed

    Liou, Tzong-Horng; Wu, Shao-Jung

    2009-11-15

    The study reports the preparation of activated carbon with a high surface area from rice husk using chemical activation with H(3)PO(4) and ZnCl(2). Activated carbon prepared from rice husk usually exhibits low specific surface areas due to its high ash content. However, experimental results show that base-leaching and acid-washing processes can effectively enhance the adsorption capacity of rice-husk carbon. The study also investigates the effects of preparation parameters on the surface characteristics of the carbon. These parameters include the kind of activating agent, before and after treatment procedures, impregnation ratio and activation temperature. The chemical and physical properties of samples were examined by EA, ICP-MS, XRD, FTIR, SEM and a N(2)-adsorption meter. The surface areas obtained from ZnCl(2) and H(3)PO(4) activation are as high as 2434 and 1741 m(2)/g, respectively. These values are higher than that of activated carbon treated with neither base nor acid (1262 and 508 m(2)/g for ZnCl(2) and H(3)PO(4) activation). Thermogravimetric analysis shows that the activation process can be divided into three parts based on temperature zones. The results of this study will be useful in developing resource recovery systems for agricultural biomass.

  5. The Preparation of Magnetic Silica Nanospheres and Incorporation of CdSe/ZnS Quantum Dots-DNA Probe.

    PubMed

    Do, Youngjin; Kim, Jongsung

    2016-03-01

    Silica nanospheres containing magnetic particles were prepared, and CdSe/ZnS QDs functionalized with carboxyl group were incorporated into the silica nanospheres by EDC/NHS coupling reaction. The silica nanospheres were prepared by a co-precipitation of ferrous and ferric solutions followed by the sol-gel reaction of TEOS (tetraethoxysilane) and APTES (3-aminopropyltriethoxysilane) using base catalyst. The size of magnetic silica nanospheres was confirmed by Transmission electron microscope (TEM). Thiol group modified single stranded oligonucleotides were immobilized on the surface of QDs and fluorescence quenching by intercalation dye (TOTO-3) after hybridization with target oligonucleotide was observed. The fluorescence from QDs could be quenched by intercalating dye (TOTO-3) after hybridization of target DNA to probe DNA. This shows that the magnetic silica-QD-DNA probe can be used to detect specific DNA.

  6. Preparation and properties of aqueous castor oil-based polyurethane-silica nanocomposite dispersions through a sol-gel process.

    PubMed

    Xia, Ying; Larock, Richard C

    2011-09-01

    Waterborne castor oil-based polyurethane-silica nanocomposites with the polymer matrix and silica nanoparticles chemically bonded have been successfully prepared through a sol-gel process. The formation of silica nanoparticles in water not only reinforces the resulting coatings, but also increases the crosslink density of the nanocomposites. The (29)Si solid state NMR spectrum indicates the formation of silica and the TEM indicates that the nanoparticles are embedded in the polymers, resembling a core-shell structure. The silica nanoparticles in the polymer matrix play an important role in improving both the mechanical properties and the thermal stabilities of the resulting nanocomposites. This work provides an effective and promising way to prepare biorenewable, high performance nanocomposite coatings.

  7. Preparation and characterization of kasuga-silica-conjugated nanospheres for sustained antimicrobial activity

    NASA Astrophysics Data System (ADS)

    Ding, Guanglong; Li, Deguang; Liu, Yao; Guo, Mingcheng; Duan, Yongheng; Li, Jianqiang; Cao, Yongsong

    2014-11-01

    Controlled release formulation of pesticides is highly desirable for attaining the most effective utilization of the pesticide as well as reducing environmental pollution. Nano-sized controlled release formulations can provide better penetration through cuticle and deliver the active ingredients efficiently to the targeted tissue. In this study, a novel strategy for the preparation of a nanoconjugate derived from kasugamycin with amino-modified silica was developed. The kasugamycin was connected with amino-modified silica matrix by an amide bond, which could avoid the initial burst release effectively and prolong the duration remarkably. The results showed the kasuga-silica can protect kasugamycin against photo-degradation effectively and the release rate of the active ingredient of nanoconjugate was related to the temperature, pH value, and the particle size (52.5-315.4 nm). With reduced particle size as well as increased temperature and acidity, the release of the active ingredient was faster. This amide linkage of kasuga-silica could be degraded by amidase effectively. This nanoconjugate displayed a better and a sustained bactericidal efficacy against E. coli than kasugamycin technical, which makes it a potential candidate as a controlled release conjugate for kasugamycin in the future.

  8. Consecutively Preparing D-Xylose, Organosolv Lignin, and Amorphous Ultrafine Silica from Rice Husk

    PubMed Central

    Zhang, Hongxi; Ding, Xuefeng; Wang, Zichen; Zhao, Xu

    2014-01-01

    Rice husk is an abundant agricultural by-product reaching the output of 80 million tons annually in the world. The most common treatment method of rice husk is burning or burying, which caused serious air pollution and resource waste. In order to solve this problem, a new method is proposed to comprehensively utilize the rice husk in this paper. Firstly, the D-xylose was prepared from the semicellulose via dilute acid hydrolysis. Secondly, the lignin was separated via organic solvent pulping from the residue. Finally, the amorphous ultrafine silica was prepared via pyrolysis of the residue produced in the second process. In this way, the three main contents of rice husk (semicellulose, lignin, and silica) are consecutively converted to three fine chemicals, without solid waste produced. The yields of D-xylose and organosolv lignin reach 58.2% and 58.5%, respectively. The purity and specific surface of amorphous ultrafine silica reach 99.92% and 225.20 m2/g. PMID:25140120

  9. Preparation and characterization of Ag nanoparticle-embedded blank and ligand-anchored silica gels.

    PubMed

    Im, Hee-Jung; Lee, Byung Cheol; Yeon, Jei-Won

    2013-11-01

    Ag nanoparticles, used for halogen (especially iodine) adsorption and an evaluation of halogen behavior, were embedded in synthesized inorganic-organic hybrid gels. In particular, an irradiation method using an electron beam plays a part in introducing Ag nanoparticles to the organofunctionalized silica gels from AgNO3 solutions in a simple way at atmospheric pressure and room temperature. For preparation of the Ag nanoparticle-embedded inorganic-organic hybrid gels, ligands of ethylenediamine (NH2CH2CH2NH-, TMSen) and mercapto (HS-) functionalized three-dimensional porous SiO2 sol-gels were first synthesized through hydrolysis and condensation reactions, and Ag nanoparticles were then embedded into the ethylenediamine- and mercapto-anchored silica gels each, through electron-beam irradiation. The addition of ligands yielded larger average pore sizes than the absence of any ligand. Moreover, the ethylenediamine ligand led to looser structures and better access of the Ag nanoparticles to the ethylenediamine-anchored gel. As a result, more Ag nanoparticles were introduced into the ethylenediamine-anchored gel. The preparation and characterization of Ag nanoparticle-embedded blank and ligand-anchored silica gels are discussed in detail.

  10. Preparation of hollow silica nanospheres in O/W microemulsion system by hydrothermal temperature changes

    NASA Astrophysics Data System (ADS)

    Wang, Dandan; Li, Xiuyan; Liu, Zuohua; Shi, Xue; Zhou, Guowei

    2017-01-01

    Hollow silica nanospheres with wrinkled or smooth surfaces were successfully fabricated through a hydrothermal method. In this method, oil-in-water microemulsion (composed of cyclohexane, water, ethanol, and cetyltrimethylammonium bromide), and polyvinylpyrrolidone were utilized as template and capping agent, respectively. In such a facile synthesis, we can well realize the morphological transformation of spheres with radially oriented mesochannels to hollow structures of silica nanoparticle only by regulating the hydrothermal temperature from 100 °C to 200 °C. Synthesized samples with different mesostructures were then used as supports to immobilize Candida rugosa lipase (CRL). The immobilized CRL was employed as a new biocatalyst for biodiesel production through the esterification of heptanoic acid with ethanol. The conversion ratio of heptanoic acid with ethanol catalyzed by the immobilized CRL was also evaluated. Results of this study suggest that the prepared samples have potential applications in biocatalysis.

  11. Preparation of superhydrophobic and transparent micro-nano hybrid coatings from polymethylhydroxysiloxane and silica ormosil aerogels

    NASA Astrophysics Data System (ADS)

    Nagappan, Saravanan; Park, Jin Joo; Park, Sung Soo; Ha, Chang-Sik

    2014-12-01

    Superhydrophobic and transparent polymethylhydroxysiloxane (PMHOS)/silica ormosil aerogel hybrids were prepared successfully by mixing of PMHOS with various weight percentages of silica ormosil aerogels (as synthesized from methyltriethoxysilane (MTES) and methyltrimethoxysilane (MTMS) precursors) in separate seal perfume glass vials. The hybrids were spin coated on glass substrate at 1000 rpm for 60 seconds and used for further analysis. The surface morphology and chemical compositions of the hybrids were analyzed by high resolution scanning electron microscopy, high resolution transmission electron microscopy, atomic force spectroscopy, adsorption and desorption isotherm, and X-ray photoelectron spectroscopy. The transparency, thermal decomposition and static contact angle (SCA) of each sample were measured by UV-Visible spectrophotometer, TGA and drop shape analysis system, respectively. The spin coated substrates showed good superhydrophobic properties, thermal stability as well as transparency on the glass substrates.

  12. Aliphatic polyurethane-silica nanocomposites prepared by the parallel synthesis: Morphology and mechanical characteristics

    NASA Astrophysics Data System (ADS)

    Gofman, I. V.; Sukhanova, T. E.; Vylegzhanina, M. É.; Abalov, I. V.; Stepanova, I. S.; Trofimov, A. E.; Ten'kovtsev, A. V.

    2010-03-01

    Films of aliphatic polyurethane-silica composites containing up to 27.3 mol % of SiO2 nanoparticles have been prepared by the parallel synthesis using the sol-gel technology. It has been revealed that the variations in the mechanical properties of these materials with increasing concentration of nanoparticles exhibit a nontrivial behavior: the ultimate strain gradually increases, whereas the elastic modulus and the yield stress decrease. A correlation of the changes observed in the mechanical characteristics with an increase in the free volume of the material with increasing silica concentration has been established. Atomic-force microscopy has confirmed the existence of a developed system of nanopores with characteristic sizes from 15 to 100 nm in the materials under investigation.

  13. Preparation and characterization of coatings with a high reflectivity on planar substrates and inside silica tubes

    NASA Astrophysics Data System (ADS)

    Bartoň, Ivo; Matějec, Vlastimil; Mrázek, Jan; Podrazký, Ondřej

    2015-01-01

    The paper presents results on preparation and characterization of highly reflective coatings on planar substrates and inside silica tubes. Coatings are designed for a maximum reflectivity at a wavelength of 550 nm and consist of several pairs of oxide layers. Each pair is composed of one layer with a high refractive index and one layer with a low refractive index with a refractive-index contrast of about 1.1. The layers were prepared by the sol-gel method. High-index layers were applied from a sol based on titanium butoxide while a sol of tetramethoxysilane was use for low-index layers. The sols were deposited onto silica slides or onto walls of silica tubes by using the dip-coating technique. Applied gel layers were thermally treated at temperatures up to 450 °C in order to obtain densified layers with thicknesses 50-100 nm. Coatings with one to five pairs of layers were fabricated. Prepared coatings were characterized by transmission and reflection spectrometry in a wavelength range from 190 to- 1100 nm, by contact profilometry, and by spectral ellipsometry. Thicknesses and refractive indices of coatings were determined from these measurements. For normal light incidence a reflectivity higher than 99% in a wavelength range of 500-650 nm was measured by transmission spectrometry on coatings prepared from four or five pairs of layers. Similar reflectivity values were determined for angles of incidence of 15, 30, 45 and 60 degrees by using reflection spectrometry. Transmission spectra measured on the coated tubes which show interference bands are also presented in the paper.

  14. Design of silica carrier for controlled release of molsidomine: effect of preparation methods of silica matrixes and their composites with molsidomine on the drug release kinetics in vitro.

    PubMed

    Parfenyuk, Elena V; Dolinina, Ekaterina S

    2014-11-01

    Biodegradable, controlled-release carrier materials with non-toxic degradation products are very valuable for delivery of cardiovascular drugs. This study is a part of development of novel form of vasodilator molsidomine to improve pharmacokinetic and consumer properties of the drug. It focuses on the effect of preparation methods of the drug-silica composites on their release kinetics. Phenyl modified silica materials prepared by different ways were studied as potential carriers for molsidomine. The composites of molsidomine with the modified silica were synthesized via one-step sol-gel route and adsorption. The drug was adsorbed onto the phenyl modified silica prepared by co-condensation and grafting. Furthermore, the one-step sol-gel derived composites were prepared at pH 4.4 (the isoelectric point of the drug) and pH 6.3 (the zero point of charge of the silica). In vitro release kinetics of molsidomine from the synthesized composites in simulated gastric (pH 1.6) and simulated blood (pH 7.4) media was studied. Our findings demonstrate that the release of the drug can be controlled by manipulating the synthesis ways and changing the sol-gel pH. The comparative analysis of molsidomine release profiles from the composites prepared by one-step sol-gel synthesis at different pH and adsorption allows to reveal perspective composites which exhibit sustained release of molsidomine for about 36h in acidic medium close to the zero order release kinetics.

  15. Acrylate-silica polymer nanocomposites obtained by sol-gel reactions. Structure, properties and scaffold preparation

    NASA Astrophysics Data System (ADS)

    Rodriguez Hernandez, Jose Carlos

    The manuscript deals with the development and characterization of hybrid materials based on poly(hydroxyethyl acrylate) (hereafter PHEA) reinforced by the inclusion of an amorphous silica phase. Both phases were simultaneously synthesized: the organic phase underwent a free radical polymerization reaction induced by the small addition of a thermal initiator (benzoyl peroxide); besides, silica (SiO2) was polymerized by an acid catalyzed sol-gel reaction of the silicon alkoxide tetraethoxysilane (hereafter TEOS). The sol-gel reaction conditions where silicon dioxide is formed influence the final silica structure: degree of condensation, linear versus branched intermediate species, average size, and so on. Some of the key parameters to control SiO2 topology on sol-gel derived composites include the catalyst nature used to increase the alkoxide reactivity (as well as its amount, pH), the available water to hydrolyze the silica precursor (referred to the stoichiometric amount needed to fully hydrolyze one molecule of TEOS) and ratio between the organic and inorganic phases on the final hybrid. The former (catalyst) and the second (water) conditions were fixed so as to synthesize materials with silica average sizes around tens of nanometres (nanocomposites); the latter, the relative ratio between organic and inorganic phases, was systematically changed. Besides, it is introduced a methodology to prepare a new kind of scaffolds made by nanocomposites whose pore morphology consists of a cylindrical channel mesh, which are perpendicular between themselves. The procedure is based on the well-known method of intermediate templates, this time prepared by a stack of woven fabrics which are first pressed and afterwards sintered. After the filling of the holes left inside the template by the monomeric solution and subsequent thermal polymerization, templates are removed by the selective solvent of the material it is made up. A suitable template preparation is found to be crucial

  16. Facile preparation of organic-silica hybrid monolith for capillary hydrophilic liquid chromatography based on "thiol-ene" click chemistry.

    PubMed

    Chen, Ming-Luan; Zhang, Jun; Zhang, Zheng; Yuan, Bi-Feng; Yu, Qiong-Wei; Feng, Yu-Qi

    2013-04-05

    In this work, a one-step approach to facile preparation of organic-inorganic hybrid monoliths was successfully developed. After vinyl-end organic monomers and azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethoxysilane (TMOS) and 3-mercaptopropyltrimethoxysilane (MPTMS), the homogeneous mixture was introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the organic-silica hybrid monoliths. By employing this strategy, two types of organic-silica hybrid monoliths with positively charged quaternary ammonium and amide groups were prepared, respectively. The functional groups were successfully introduced onto the monoliths during the sol-gel process with "thiol-ene" click reaction, which was demonstrated by ζ-potential assessment, energy dispersive X-ray spectroscopy (EDX), and Fourier transform infrared (FT-IR) spectroscopy. The porous structure of the prepared monolithic columns was examined by scanning electron microscopy (SEM), nitrogen adsorption-desorption measurement, and mercury intrusion porosimetry. These results indicate the prepared organic-silica hybrid monoliths possess homogeneous column bed, large specific surface area, good mechanical stability, and excellent permeability. The prepared monolithic columns were then applied for anion-exchange/hydrophilic interaction liquid chromatography. Different types of analytes, including benzoic acids, inorganic ions, nucleosides, and nucleotides, were well separated with high column efficiency around 80,000-130,000 plates/m. Taken together, we present a facile and universal strategy to prepare organic-silica hybrid monoliths with a variety of organic monomers using one-step approach.

  17. Preparations for low-cost silica substrate of CIGS solar cell

    NASA Astrophysics Data System (ADS)

    Hsu, Ming-Seng; Chang, Chung Chih; Cheng, Hsiang Hshi; Ouyang, Yueh; Der Sheu, Shinn

    2008-08-01

    The production of CuInGaSe2 (CIGS) solar cell is based on vacuum processes, which requires a high manufacturing temperature and high cost. Our result show a simple method has been developed to prepare the silica substrates of CIGS solar cell. It's synthesized by sol-gel process from tetraethylorthosilicate (TEOS), methanol (CH3OH) and pure water (both ion-exchange and distillation) in the presence of ammonia as catalyst. The preparation procedure was elaborated as the flexible sequence to control chemical composition and properties of the particles in sol-gel-derived silica substrate. The morphology, particle size, and size distribution of CIGS substrate were characterized with dynamic light scattering (DLS) and atomic force microscopy (AFM). The results of AFM morphology and statistic evidence we find an easy way, non-vacuum and low temperature processes, to successfully prepare the CIGS solar cell substrates with surface roughness below 3 nm. It is powerful the advance study in low cost solar cell.

  18. Preparation of ultrafine silica from potash feldspar using sodium carbonate roasting technology

    NASA Astrophysics Data System (ADS)

    Liu, Jia-nan; Shen, Xiao-yi; Wu, Yan; Zhang, Jun; Zhai, Yu-chun

    2016-08-01

    A novel process was developed for the preparation of ultrafine silica from potash feldspar. In the first step, potash feldspar was roasted with Na2CO3 and was followed by leaching using NaOH solution to increase the levels of potassium, sodium, and aluminum in the solid residue. The leaching solution was then carbonated to yield ultrafine silica. The optimized reaction conditions in the roasting process were as follows: an Na2CO3-to-potash feldspar molar ratio of 1.1, a reaction temperature of 875°C, and a reaction time of 1.5 h. Under these conditions, the extraction rate of SiO2 was 98.13%. The optimized carbonation conditions included a final solution pH value of 9.0, a temperature of 40°C, a CO2 flow rate of 6 mL/min, a stirring intensity of 600 r/min, and an ethanol-to-water volume ratio of 1:9. The precipitation rate and granularity of the SiO2 particles were 99.63% and 200 nm, respectively. We confirmed the quality of the obtained ultrafine silica by comparing the recorded indexes with those specified in Chinese National Standard GB 25576―2010.

  19. Preparation of silica coated cobalt ferrite magnetic nanoparticles for the purification of histidine-tagged proteins

    NASA Astrophysics Data System (ADS)

    Aygar, Gülfem; Kaya, Murat; Özkan, Necati; Kocabıyık, Semra; Volkan, Mürvet

    2015-12-01

    Surface modified cobalt ferrite (CoFe2O4) nanoparticles containing Ni-NTA affinity group were synthesized and used for the separation of histidine tag proteins from the complex matrices through the use of imidazole side chains of histidine molecules. Firstly, CoFe2O4 nanoparticles with a narrow size distribution were prepared in an aqueous solution using the controlled co-precipitation method. In order to obtain small CoFe2O4 agglomerates, oleic acid and sodium chloride were used as dispersants. The CoFe2O4 particles were coated with silica and subsequently the surface of these silica coated particles (SiO2-CoFe2O4) was modified by amine (NH2) groups in order to add further functional groups on the silica shell. Then, carboxyl (-COOH) functional groups were added to the SiO2-CoFe2O4 magnetic nanoparticles through the NH2 groups. After that Nα,Nα-Bis(carboxymethyl)-L-lysine hydrate (NTA) was attached to carboxyl ends of the structure. Finally, the surface modified nanoparticles were labeled with nickel (Ni) (II) ions. Furthermore, the modified SiO2-CoFe2O4 magnetic nanoparticles were utilized as a new system that allows purification of the N-terminal His-tagged recombinant small heat shock protein, Tpv-sHSP 14.3.

  20. Preparation of aluminum-containing mesoporous silica with hierarchical macroporous architecture and its enhanced catalytic activities.

    PubMed

    Kamegawa, Takashi; Tanaka, Shota; Seto, Hiroki; Zhou, Dayang; Yamashita, Hiromi

    2013-08-28

    Aluminum-containing mesoporous silica with hierarchical macroporous architecture (Al-MMS) was successfully prepared using a solvent evaporation method through the combination of precursor solution for synthesis of Al-containing mesoporous silica (Al-MS) and poly(methyl methacrylate) (PMMA) colloidal crystals as a hard template. The porous structure and the state of aluminum were investigated using various characterization techniques. The construction of combined structure of Al-MMS, i.e., hierarchical macroporous architecture consisting of thin mesoporous silica frameworks, led to the formation of many mesopore entrances and the shortening of the mesoporous channels. In the tetrahydropyranylation of linear alcohols with dihydropyran (DHP), Al-MMS exhibited higher catalytic activities for the formation of corresponding tetrahydropyranyl ethers as compared to Al-MS. The advantageous structure of Al-MMS enables the efficient transport of reactants to the catalytically active sites, which realizes the significant enhancement of catalytic performances in the reaction of DHP with alcohols having longer alkyl chains.

  1. Preparation of bio-compatible boron nanoparticles and novel mesoporous silica nanoparticles for bio-applications

    NASA Astrophysics Data System (ADS)

    Gao, Zhe

    This dissertation presents the synthesis and characterization of several novel inorganic and hybrid nanoparticles, including the bio-compatible boron nanoparticles (BNPs) for boron neutron capture therapy (BNCT), tannic acid-templated mesoporous silica nanoparticles and degradable bridged silsesquioxane silica nanoparticles. Chapter 1 provides background information of BNCT and reviews the development of design and synthesizing silica nanoparticles and the study of silica material degradability. Chapter 2 describes the preparation and characterization of dopamine modified BNPs and the preliminary cell study of them. The BNPs were first produced via ball milling, with fatty acid on the surface to stabilize the combustible boron elements. This chapter will mainly focus on the ligand-exchange strategy, in which the fatty acids were replaced by non-toxic dopamines in a facile one-pot reaction. The dopamine-coated BNPs (DA-BNPs) revealed good water dispersibility and low cytotoxicity. Chapter 3 describes the synthesis of tannic acid template mesoporous silica nanoparticles (TA-TEOS SiNPs) and their application to immobilize proteins. The monodispersed TA SiNPs with uniform pore size up to approximately 13 nm were produced by utilizing tannic acid as a molecular template. We studied the influence of TA concentration and reaction time on the morphology and pore size of the particles. Furthermore, the TA-TEOS particles could subsequently be modified with amine groups allowing them to be capable of incorporating imaging ligands and other guest molecules. The ability of the TA-TEOS particles to store biomolecules was preliminarily assessed with three proteins of different charge characteristics and dimensions. The immobilization of malic dehydrogenase on TA-TEOS enhanced the stability of the enzyme at room temperature. Chapter 4 details the synthesis of several bridged silsesquioxanes and the preparation of degradable hybrid SiNPs via co-condensation of bridged

  2. Optically transparent polyelectrolyte-silica composite materials: Preparation, characterization, and application in optical chemical sensing

    SciTech Connect

    Shi, Yining; Seliskar, C.J.

    1997-03-01

    A series of polyelectrolyte-containing silica composite materials have been prepared by sol-gel processing. These optically transparent composites have been characterized by scanning electron microscopy and UV-visible spectrophotometry. These materials can be processed into monolithic disks and thin films. The thicknesses of spin-coated films of these materials on glass can be varied from 0.13 to 3.5 {mu}m as determined by an optical interferences method. These materials are ion exchangeable and less brittle than the parent silica glass due to the incorporation of the organic polyelectrolyte. These new composites retain the nanoscale porosity and optical transparency into the ultraviolet of the parent silica sol-gel glasses, making them attractive host matrixes for the immobilization of ionizable dye molecules and chemical reagents. An optical pH sensing platform (0.9 x 2.5 cm) based on the electrostatic immobilization of HPTS (8-hydroxy-1,3,6-pyrenetrisulfonic acid trisodium salt) in a PDMDAAC (poly(diallyldimethylammonium chloride))-silica composite film was fabricated and evaluated. The results clearly demonstrate that this platform is easy to construct with high batch reproducibility and can be regenerated by simple solution ion exchange. The platform is usable in both the modes of absorption and fluorescence, making it versatile. Having a fast response time (ca. {approximately}2 s to more than 2 units of pH change), the platform is also highly resistant to dye leaching and storage degradation over a period of months. 49 refs., 9 figs., 2 tabs.

  3. Enzyme encapsulation in silica gel prepared by polylysine and its catalytic activity

    NASA Astrophysics Data System (ADS)

    Kawachi, Yuki; Kugimiya, Shin-ichi; Nakamura, Hitomi; Kato, Katsuya

    2014-09-01

    Enzymes used in industrial applications are often immobilized onto different types of supports because they are sensitive to pH, temperature, and various other environmental conditions. However, many of the current immobilization approaches face problems such as the requirement of tedious multi-step procedures, loss of enzyme activity during immobilization, and poor reusability. In this study, we chose poly-L-lysine (Ki) as a catalyst for silica mineralization and attempted a one-step “leave to stand” synthesis method under mild conditions, so as to simultaneously maintain both high enzymatic activity and reusability. To examine the effect of Kx on the enzymatic reaction of lipase, we performed hydrolysis of 2-octylacetate without adding a silica precursor. Results indicate that Kx hardly exerts adverse influence on the enzymatic activity of lipase. The lipase encapsulated in the silica gel prepared by leave to stand (Gelstand) retained 70% of the activity compared to the free solution, which is two times higher than that obtained by mixing (Gelmix). However, the Km value was found to be similar to that of free enzymes. These results suggest that the leave to stand is a suitable procedure for immobilization, without any decrease in the mass transfer of substrate. The Gel-stand sample retained 100% activity even after the 5th cycle, and retained above 95% of its activity after 4 h of heat treatment at 65 °C. Using phenyltriethoxysilane as a silica precursor, tertiary structural stability of enzyme was obtained, and its Kcat value was improved when compared to a free solution.

  4. Dummy molecularly imprinted mesoporous silica prepared by hybrid imprinting method for solid-phase extraction of bisphenol A.

    PubMed

    Yu, Dan; Hu, Xiaolei; Wei, Shoutai; Wang, Qiang; He, Chiyang; Liu, Shaorong

    2015-05-29

    A novel hybrid dummy imprinting strategy was developed to prepare a mesoporous silica for the solid-phase extraction (SPE) of bisphenol A (BPA). A new covalent template-monomer complex (BPAF-Si) was first synthesized with 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BPAF) as the template. The imprinted silica was obtained through the gelation of BPAF-Si with tetraethoxysilane and the subsequent removal of template by thermal cleavage, and then it was characterized by FT-IR spectroscopy, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption-desorption isotherms. Results showed that the new silica had micron-level particle size and ordered mesoporous structure. The static binding test verified that the imprinted silica had much higher recognition ability for BPA than the non-imprinted silica. The imprinted silica also showed high extraction efficiencies and high enrichment factor for SPE of BPA. Using the imprinted silica, a SPE-HPLC-UV method was developed and successfully applied for detecting BPA in BPA-spiked tap water and lake water samples with a recovery of 99-105%, a RSD of 2.7-5.0% and a limit of detection (S/N=3) of 0.3ng/mL. The new imprinted silica avoided the interference of the residual template molecules and reduced the non-specific binding sites, and therefore it can be utilized as a good sorbent for SPE of BPA in environmental water samples.

  5. One-Pot Approach to Prepare Organo-silica Hybrid Capillary Monolithic Column with Intact Mesoporous Silica Nanoparticle as Building Block

    PubMed Central

    Liu, Shengju; Peng, Jiaxi; Liu, Zheyi; Liu, Zhongshan; Zhang, Hongyan; Wu, Ren’an

    2016-01-01

    A facile “one-pot” approach to prepare organo-silica hybrid capillary monolithic column with intact mesoporous silica nanoparticle (IMSN) as crosslinker and building block was described. An IMSN crosslinked octadecyl-silica hybrid capillary monolithic column (IMSN-C18 monolithic column) was successfully prepared, and the effects of fabrication conditions (e.g. concentration of intact mesoporous silica nanoparticle, polycondensation temperature, content of vinyltrimethoxysilane and stearyl methacrylate) on the structures of the IMSN-C18 monolithic column were studied in detail. The IMSN-C18 hybrid monolithic column possessed uniform morphology, good mechanical and pH stability (pH 1.1–11), which was applied to the separations of alkyl benzenes, polycyclic aromatic hydrocarbons (PAHs), as well as proteins. The minimum plate height of 10.5 μm (corresponding to 95000 N m−1) for butylbenzene and high reproducibility were achieved. The analysis of tryptic digest of bovine serum albumin (BSA) was carried out on the IMSN-C18 monolithic column by cLC coupled mass spectrometry (cLC-MS/MS), with the protein sequence coverage of 87.5% for BSA, demonstrating its potential application in proteomics. PMID:27698475

  6. Highly stabilized, polymer-lipid membranes prepared on silica microparticles as stationary phases for capillary chromatography

    PubMed Central

    Gallagher, Elyssia S.; Adem, Seid M.; Baker, Christopher A.; Ratnayaka, Saliya N.; Jones, Ian W.; Hall, Henry K.; Saavedra, S. Scott; Aspinwall, Craig A.

    2015-01-01

    The ability to rapidly screen complex libraries of pharmacological modulators is paramount to modern drug discovery efforts. This task is particularly challenging for agents that interact with lipid bilayers or membrane proteins due to the limited chemical, physical, and temporal stability of conventional lipid-based chromatographic stationary phases. Here, we describe the preparation and characterization of a novel stationary phase material composed of highly stable, polymeric-phospholipid bilayers self-assembled onto silica microparticles. Polymer lipid membranes were prepared by photochemical or redox initiated polymerization of 1,2-bis[10-(2′,4′-hexadieoyloxy)decanoyl]-sn-glycero-2-phosphocholine (bis-SorbPC), a synthetic, polymerizable lipid. The resulting polymerized bis-SorbPC (poly(bis-SorbPC)) stationary phases exhibited enhanced stability compared to particles coated with 1,2-dioleoyl-sn-glycero-phosphocholine (unpolymerized) phospholipid bilayers when exposed to chemical (50mM triton X-100 or 50% acetonitrile) and physical (15 min sonication) insults after 30 days of storage. Further, poly(bis-SorbPC)-coated particles survived slurry packing into fused silica capillaries, compared to unpolymerized lipid membranes, where the lipid bilayer was destroyed during packing. Frontal chromatographic analyses of the lipophilic small molecules acetylsalicylic acid, benzoic acid, and salicylic acid showed > 44% increase in retention times (P < 0.0001) for all analytes on poly(bis-SorbPC)-functionalized stationary phase compared to bare silica microspheres, suggesting a lipophilic retention mechanism. Phospholipid membrane-functionalized stationary phases that withstand the chemical and physical rigors of capillary LC conditions can substantially increase the efficacy of lipid membrane affinity chromatography, and represents a key advance towards the development of robust membrane protein-functionalized chromatographic stationary phases. PMID:25670414

  7. Highly stabilized, polymer-lipid membranes prepared on silica microparticles as stationary phases for capillary chromatography.

    PubMed

    Gallagher, Elyssia S; Adem, Seid M; Baker, Christopher A; Ratnayaka, Saliya N; Jones, Ian W; Hall, Henry K; Saavedra, S Scott; Aspinwall, Craig A

    2015-03-13

    The ability to rapidly screen complex libraries of pharmacological modulators is paramount to modern drug discovery efforts. This task is particularly challenging for agents that interact with lipid bilayers or membrane proteins due to the limited chemical, physical, and temporal stability of conventional lipid-based chromatographic stationary phases. Here, we describe the preparation and characterization of a novel stationary phase material composed of highly stable, polymeric-phospholipid bilayers self-assembled onto silica microparticles. Polymer-lipid membranes were prepared by photochemical or redox initiated polymerization of 1,2-bis[10-(2',4'-hexadieoyloxy)decanoyl]-sn-glycero-2-phosphocholine (bis-SorbPC), a synthetic, polymerizable lipid. The resulting polymerized bis-SorbPC (poly(bis-SorbPC)) stationary phases exhibited enhanced stability compared to particles coated with 1,2-dioleoyl-sn-glycero-phosphocholine (unpolymerized) phospholipid bilayers when exposed to chemical (50 mM triton X-100 or 50% acetonitrile) and physical (15 min sonication) insults after 30 days of storage. Further, poly(bis-SorbPC)-coated particles survived slurry packing into fused silica capillaries, compared to unpolymerized lipid membranes, where the lipid bilayer was destroyed during packing. Frontal chromatographic analyses of the lipophilic small molecules acetylsalicylic acid, benzoic acid, and salicylic acid showed >44% increase in retention times (P<0.0001) for all analytes on poly(bis-SorbPC)-functionalized stationary phase compared to bare silica microspheres, suggesting a lipophilic retention mechanism. Phospholipid membrane-functionalized stationary phases that withstand the chemical and physical rigors of capillary LC conditions can substantially increase the efficacy of lipid membrane affinity chromatography, and represents a key advance toward the development of robust membrane protein-functionalized chromatographic stationary phases.

  8. Impact of muffle furnace preparation on the results of crystalline silica analysis.

    PubMed

    Lee, R J; Van Orden, D R; Cox, L A; Arlauckas, S; Kautz, R J

    2016-10-01

    A prior report demonstrated an unacceptably low level of accuracy in silica analytical testing, with a general negative bias (i.e., underreporting) although other inaccuracies included false-positive results when analyzing blank filters. The possible bias may have been due to the loss of sample during shipping and or sample preparation. We report on a follow-up study that was designed to mimic the original study, but in which sources of variability were evaluated. We found no effect on silica recoveries due to shipping and confirmed the prior study results that the muffle furnace ashing process led to low overall recoveries (49-104%), depending on the adherence to the recommended preparation method. Plasma ashing recoveries ranged from 89 to 108%. Our results suggest that muffle-furnace ashing using a crucible should be restricted. More broadly, however, muffle-furnace ashing is only one source of analytical error that contributes to the relatively poor overall performance revealed by Cox et al. Whatever the case, OSHA should ensure that its proposed requirements to improve laboratory performance will actually lead to the discovery and correction of all major sources of error by participating laboratories. This is particularly important in light of OSHA's proposed reduction in the PEL and action level proposed by OSHA.

  9. Structural and optical properties of Cu:silica nanocomposite films prepared by co-sputtering deposition

    NASA Astrophysics Data System (ADS)

    Battaglin, G.; Cattaruzza, E.; Gonella, F.; Polloni, R.; Scremin, B. F.; Mattei, G.; Mazzoldi, P.; Sada, C.

    2004-03-01

    Copper-containing silica films were synthesized by radiofrequency (rf) co-sputtering deposition technique, and then heat-treated in different annealing atmospheres, i.e. either oxidizing or reducing, with the aim to develop suitable preparation methodologies for controlling the composite structure. Characterization of the samples along the various preparation steps was performed by Rutherford backscattering spectrometry (RBS), transmission electron microscopy and optical absorption spectroscopy. The nonlinear optical coefficient n2 of the nanocomposite films was estimated by the Z-scan technique. Experimental observations showed that copper migration and aggregation depend critically on the annealing conditions, giving rise to quite different stable structures. In particular, for samples heat-treated first in air and then in a H2-Ar gas mixture, the oxidizing atmosphere drives copper towards the surface while the reducing one promotes the subsequent clusterization in a well defined region.

  10. Poromechanics of microporous media

    NASA Astrophysics Data System (ADS)

    Brochard, L.; Vandamme, M.; Pellenq, R. J.-M.

    2012-04-01

    Microporous media, i.e., porous media made of pores with a nanometer size, are important for a variety of applications, for instance for sequestration of carbon dioxide in coal, or for storage of hydrogen in metal-organic frameworks. In a pore of nanometer size, fluid molecules are not in their bulk state anymore since they interact with the atoms of the solid: they are said to be in an adsorbed state. For such microporous media, conventional poromechanics breaks down. In this work we derive poroelastic constitutive equations which are valid for a generic porous medium, i.e., even for a porous medium with pores of nanometer size. The complete determination of the poromechanical behavior of a microporous medium requires knowing how the amount of fluid adsorbed depends on both the fluid bulk pressure and the strain of the medium. The derived constitutive equations are validated with the help of molecular simulations on one-dimensional microporous media. Even when a microporous medium behaves linearly in the absence of any fluid (i.e., its bulk modulus does not depend on strain), we show that fluid adsorption can induce non-linear behavior (i.e., its drained bulk modulus can then depend significantly on strain). We also show that adsorption can lead to an apparent Biot coefficient of the microporous medium greater than unity or smaller than zero. The poromechanical response of a microporous medium to adsorption significantly depends on the pore size distribution. Indeed, the commensurability (i.e., the ratio of the size of the pores to that of the fluid molecules) proves to play a major role. For a one-dimensional model of micropores with a variety of pore sizes, molecular simulations show that the amount of adsorbed fluid depends linearly on the strain of the medium. We derive linearized constitutive equations which are valid when such a linear dependence of the adsorbed amount of fluid on the strain is observed. As an application, the case of methane and coal is

  11. Preparation of the narrow size distribution USPIO in mesoporous silica for magnetic field guided drug delivery and release

    NASA Astrophysics Data System (ADS)

    Zapotoczny, B.; Guskos, N.; Kozioł, J. J.; Dudek, M. R.

    2015-01-01

    Ultra-small superparamagnetic iron oxides (USPIO) with an average diameter of 2 nm were synthesized in mesoporous silica using the method of co-precipitation of Fe2+ and Fe3+ ions in aqueous solution directly in the silica nanopores. Two types of the silica material, hexagonal phase MCM-41 and mesoporous silica spheres (MSS), were used. The resulting magnetically modified silica samples show high-quality superparamagnetic properties which persist also at low temperatures near 2 K. Their magnetization saturation in an applied external magnetic field exceeds 15 emu/g. The magnetically modified silica samples were studied with the help of the ferromagnetic resonance (FMR), SQUID-magnetometry, X-ray diffraction (XRD), dynamic light scattering (DLS) and TEM/EDX microscopy. The studies were complemented by confirming the possibility of drug release by the modified silica samples where the standard fluorescent dye was used as an example. The prepared material is suggested to be considered for magnetic field guided drug delivery and release.

  12. Preparation of double emulsions using hybrid polymer/silica particles: new pickering emulsifiers with adjustable surface wettability.

    PubMed

    Williams, Mark; Warren, Nicholas J; Fielding, Lee A; Armes, Steven P; Verstraete, Pierre; Smets, Johan

    2014-12-10

    A facile route for the preparation of water-in-oil-in-water (w/o/w) double emulsions is described for three model oils, namely, n-dodecane, isopropyl myristate, and isononyl isononanoate, using fumed silica particles coated with poly(ethylene imine) (PEI). The surface wettability of such hybrid PEI/silica particles can be systematically adjusted by (i) increasing the adsorbed amount of PEI and (ii) addition of 1-undecanal to the oil phase prior to homogenization. In the absence of this long-chain aldehyde, PEI/silica hybrid particles (PEI/silica mass ratio = 0.50) produce o/w Pickering emulsions in all cases. In the presence of 1-undecanal, this reagent reacts with the primary and secondary amine groups on the PEI chains via Schiff base chemistry, which can render the PEI/silica hybrid particles sufficiently hydrophobic to stabilize w/o Pickering emulsions at 20 °C. Gas chromatography, (1)H NMR and X-ray photoelectron spectroscopy provide compelling experimental evidence for this in situ surface reaction, while a significant increase in the water contact angle indicates markedly greater hydrophobic character for the PEI/silica hybrid particles. However, when PEI/silica hybrid particles are prepared using a relatively low adsorbed amount of PEI (PEI/silica mass ratio = 0.075) only o/w Pickering emulsions are obtained, since the extent of surface modification achieved using this Schiff base chemistry is insufficient. Fluorescence microscopy and laser diffraction studies confirm that highly stable w/o/w double emulsions can be achieved for all three model oils. This is achieved by first homogenizing the relatively hydrophobic PEI/silica hybrid particles (PEI/silica mass ratio = 0.50) with an oil containing 3% 1-undecanal to form an initial w/o emulsion, followed by further homogenization using an aqueous dispersion of relatively hydrophilic PEI/silica particles (PEI/silica mass ratio = 0.075). Dye release from the internal aqueous cores into the aqueous continuous

  13. Synthesis of silver nanoparticles deposited on silica by γ-irradiation and preparation of PE/Ag nano compound masterbatches

    NASA Astrophysics Data System (ADS)

    Nguyen, Thi Kim Lan; Trinh Nguyen, Thuy Ai; Phu Dang, Van; Duy Nguyen, Ngoc; Le, Anh Quoc; Hien Nguyen, Quoc

    2013-12-01

    Silver nanoparticles (AgNPs) deposited on silica were synthesized by gamma Co-60 irradiation of Ag+ dispersion in silica/ethanol/water mixture (9/80/20:w/v/v). The reduction of Ag+ is occurred by hydrated electron (e-aq) and hydrogen atom (H•) generated during radiolysis of ethanol/water. The conversion doses (Ag+ → Ag0) were determined by UV-Vis spectroscopy. The synthesized AgNPs/silica were characterized by transmission electron microscopy (TEM) and x-ray diffraction (XRD), which showed the size of AgNPs to be in the range of 5-40 nm for Ag+ concentrations from 5 to 20 mM. Masterbatches of PE/AgNPs/silica compound with silver content from 250 to 1000 mg kg-1 were also prepared. These masterbatches can be suitably used for various applications such as antimicrobial food containers and packing films, etc.

  14. Silica-tin nanotubes prepared from rice husk ash by sol-gel method: Characterization and its photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Adam, Farook; Appaturi, Jimmy Nelson; Thankappan, Radhika; Nawi, Mohd Asri Mohd

    2010-11-01

    Silica-tin material has been synthesized by simple sol-gel method using rice husk ash as the source of silica and cetyltrimethylammonium bromide as the surfactant at room temperature. Calcination of the material at 500 °C for 5 h gave nanotubes with external diameter of 2-4 nm and an internal diameter of 1-2 nm. The BET specific surface area was found to be 607 m 2 g -1. Nitrogen sorption analysis exhibits a type IV isotherm with H3 hysteresis loop. The powder X-ray diffraction pattern showed that the material is amorphous. The photocatalytic activity of the prepared material was studied towards degradation of methylene blue under UV-irradiation. According to the experimental results the silica-tin nanotubes exhibit high photocatalytic activity compared to pure rice husk silica.

  15. Optical Properties of Silica-Encapsulated ZnSe Nanocrystals Prepared with Water-in-Oil Microemulsions

    NASA Astrophysics Data System (ADS)

    Liu, Kang; Kim, Ji Hyeon; Park, Sang Joon

    2013-01-01

    Silica-encapsulated ZnSe nanocrystals (NCs) were prepared by a safe and simple synthesis method, utilizing a sodium bis (2-ethylhexyl) sulfosuccinate (AOT)/water/cyclohexane microemulsion system and characterized by UV-vis analysis, photoluminescence (PL) spectroscopy, and transmission electron microscopy (TEM). For the encapsulations, two reverse micellar solutions [one for tetraethyl orthosilicate (TEOS) and the other for ZnSe] containing different water volumes were employed. The size of silica particles containing ZnSe NCs could be controlled from 13-37 nm by varying the water content W (W=[H2O]/[AOT]). On the other hand, the size of encapsulated ZnSe NCs was almost unchanged (about 2.5 nm) even though the size of the silica particles was increased. At W = 7, the maximum PL efficiency of 6% was obtained and the photostability was increased markedly after ZnSe NCs were encapsulated by silica.

  16. Synthesis and electrical response of polyaniline/poly(styrene sulfonate)-coated silica spheres prepared by seed-coating method.

    PubMed

    Lee, Seungae; Hong, Jin-Yong; Jang, Jyongsik

    2013-05-15

    The polyaniline/poly(styrene sulfonate) (PANI/PSS)-coated silica spheres with three different sizes (50, 100, and 250 nm) are fabricated through seed-coating method and adopted as dispersing materials for electrorheological (ER) fluids to examine the influence of particle diameter on ER activity. Interestingly, the ER properties of PANI/PSS-coated silica spheres exhibit a dependence on their size. Performances of PANI/PSS-coated silica spheres-based ER fluids enhanced with decreasing the diameter of particle. It is believed that the size effect played a dominant role in enhancing the performance of ER fluid. Furthermore, the fibrillation phenomenon of prepared PANI/PSS-coated silica spheres-based ER fluid was observed via an optical microscope in the applied electric field. Sedimentation properties were also analyzed to provide additional insight into the size effect of ER fluids.

  17. Preparation of magnetite-loaded silica microspheres for solid-phase extraction of genomic DNA from soy-based foodstuffs.

    PubMed

    Shi, Ruobing; Wang, Yucong; Hu, Yunli; Chen, Lei; Wan, Qian-Hong

    2009-09-04

    Solid-phase extraction has been widely employed for the preparation of DNA templates for polymerase chain reaction (PCR)-based analytical methods. Among the variety of adsorbents studied, magnetically responsive silica particles are particularly attractive due to their potential to simplify, expedite, and automate the extraction process. Here we report a facile method for the preparation of such magnetic particles, which entails impregnation of porous silica microspheres with iron salts, followed by calcination and reduction treatments. The samples were characterized using powder X-ray diffractometry (XRD), scanning electron microscopy (SEM), nitrogen adsorption/desorption isotherms, and vibrating sample magnetometry (VSM). XRD data show that magnetite nanocrystals of about 27.2 nm are produced within the pore channels of the silica support after reduction. SEM images show that the as-synthesized particles exhibit spherical shape and uniform particle size of about 3 microm as determined by the silica support. Nitrogen sorption data confirm that the magnetite-loaded silica particles possess typical mesopore structure with BET surface area of about 183 m(2)/g. VSM data show that the particles display paramagnetic behavior with saturation magnetization of 11.37 emu/g. The magnetic silica microspheres coated with silica shells were tested as adsorbents for rapid extraction of genomic DNA from soybean-derived products. The purified DNA templates were amplified by PCR for screening of genetically modified organisms (GMOs). The preliminary results confirm that the DNA extraction protocols using magnetite-loaded silica microspheres are capable of producing DNA templates which are inhibitor-free and ready for downstream analysis.

  18. Unraveling the Mystery of Stöber Silica's Microporosity.

    PubMed

    Li, Shanshan; Wan, Quan; Qin, Zonghua; Fu, Yuhong; Gu, Yuantao

    2016-09-13

    Puzzling aspects of the microporous structure of Stöber silica, including inconsistencies in the BET specific surface area and the long measurement time required for N2 adsorption, hinder further research on and potential applications of this material. In this work, Stöber silica samples prepared using systematic and detailed post-treatment methods were characterized by N2 adsorption, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma optical emission spectrometry, elemental analysis, and Fourier transform infrared spectroscopy. We have found that the often overlooked sample preparation conditions may be the main causes that perplex the gas adsorption characterization results of Stöber silica samples. The pore-blocking processes associated with a variety of sample treatment methods are discussed in detail. Strong evidence for the particle growth model and pore-blocking mechanism involving ethoxyl groups, Si species, and condensation of silanols is provided. A remarkable result is that the measurement time is shortened from 1 month in our previous work to 2-3 days for samples with large specific surface areas. A suitable post-treatment condition is recommended to obtain microporous Stöber silica with a short measurement time, including water washing, low temperature drying without a vacuum, and a short storage time.

  19. Preparation and Properties of Ethylene Vinyl Acetate Copolymer/Silica Nanocomposites in Presence of EVA-g-Acrylic Acid.

    PubMed

    Tham, Do Quang; Tuan, Vu Manh; Thanh, Dinh Thi Mai; Chinh, Nguyen Thuy; Giang, Nguyen Vu; Trang, Nguyen Thi Thu; Hang, To Thi Xuan; Huong, Ho Thu; Dung, Nguyen Thi Kim; Hoang, Thai

    2015-04-01

    Here we report a facile approach to enhance the dispersibility of ethylene vinyl acetate copolymer (EVA)/silica nanocomposites (for the EVA/silica nanocomposites and interaction between silica nanoparticles (nanosilica) and EVA by adding EVA-g-acrylic acid (EVAgAA) as a compatibilizer, which was formed by grafting acrylic acid onto EVA chains with the aid of dicumyl peroxide). The above nanocomposites with and without EVAgAA were prepared by melt mixing in a Haake intermixer with different contents of silica and EVAgAA. Their structure and morphology were characterized by Fourier transform infra-red (FT-IR) spectroscopy, field emission scanning electron microscopy (FE-SEM), and the mechanical, rheological, dielectrical, and flammability properties of the nanocomposites were also investigated. The FT-IR spectra of the nanocomposites confirmed the formation of hydrogen bonds between the surface silanol groups of nanosilica and C=O groups of EVA and/or EVAgAA. The presence of EVAgAA remarkably increased the intensity of hydrogen bonding between nanosilica and EVA which not only enhanced the dispersion of nanosilica in EVA matrix but also increased the mechanical, viscosity and storage modulus of EVA/silica nanocomposites. In addition, the flammability of EVA/silica nanocomposites is also significantly reduced after the functionalization with EVAgAA. However, the mechanical properties of EVA/silica nanocomposites tended to level off when its content was above 1.5 wt.%. It has also been found that the dielectric constant value of the EVA/EVAgAA/silica nanocomposites is much lower than that of the EVA/silica nanocomposites, which is another evidence of the hydrogen bonding formation between EVAgAA and nanosilica.

  20. Preparation and characterization of PEG-coated silica nanoparticles for oral insulin delivery.

    PubMed

    Andreani, Tatiana; de Souza, Ana Luiza R; Kiill, Charlene P; Lorenzón, Esteban N; Fangueiro, Joana F; Calpena, Ana Cristina; Chaud, Marco V; Garcia, Maria L; Gremião, Maria Palmira D; Silva, Amélia M; Souto, Eliana B

    2014-10-01

    The present study reports the production and characterization of PEG-coated silica nanoparticles (SiNP-PEG) containing insulin for oral administration. High (PEG 20,000) and low (PEG 6000) PEG molecular weights were used in the preparations. SiNP were produced by sol-gel technology followed by PEG adsorption and characterized for in vitro release by Franz diffusion cells. In vitro permeation profile was assessed using everted rat intestine. HPLC method has been validated for the determination of insulin released and permeated. Insulin secondary structure was performed by circular dichroism (CD). Uncoated SiNP allowed slower insulin release in comparison to SiNP-PEG. The coating with high molecular weight PEG did not significantly (p> 0.05) alter insulin release. The slow insulin release is attributed to the affinity of insulin for silanol groups at silica surface. Drug release followed second order kinetics for uncoated and SiNP-PEG at pH 2.0. On the other hand, at pH 6.8, the best fitting was first-order for SiNP-PEG, except for SiNP which showed a Boltzmann behavior. Comparing the values of half-live, SiNP-PEG 20,000 showed a faster diffusion followed by Si-PEG 6000 and SiNP. CD studies showed no conformational changes occurring after protein release from the nanoparticles under gastrointestinal simulated conditions.

  1. Preparation of alumina nanoshell coated porous silica spheres for inorganic anions separation.

    PubMed

    Song, Zhihua; Wu, Dapeng; Ding, Kun; Guan, Yafeng

    2016-02-12

    It had been reported that alumina nanoshell coating could be obtained on the external surface of various substrates in one-nanometer precision in aqueous solution. In this work, alumina nanoshell coated mesoporous silica microbeads (nanoAl2O3/mesoSiO2) were prepared with the similar method, and were successfully applied to inorganic anions separation. As the mass transfer speed is largely constrained in the mesopore compared with that on the open surface, it was found that a complete alumina nanoshell coating could be obtained within the mesopore until the five-time coating was carried out. After characterization by BET, SEM and FTIR, it was found that the obtained nanoAl2O3/mesoSiO2 particles are smooth and well dispersed, and the mesopores are well reserved. In addition, the full coverage of nanoAl2O3 shell in mesopores was also confirmed by the binding capacity experiments with berberine. Finally, the nanoAl2O3/mesoSiO2 particles were packed in silica capillary for the separation of inorganic anions I(-), SCN(-), Br(-), NO2(-) and NO3(-) with ion chromatography (IC), and a column efficiency of 3.8 × 10(4) plates per meter was obtained for I(-).

  2. Nanocellulose Derivative/Silica Hybrid Core-Shell Chiral Stationary Phase: Preparation and Enantioseparation Performance.

    PubMed

    Zhang, Xiaoli; Wang, Litao; Dong, Shuqing; Zhang, Xia; Wu, Qi; Zhao, Liang; Shi, Yanping

    2016-05-04

    Core-shell silica microspheres with a nanocellulose derivative in the hybrid shell were successfully prepared as a chiral stationary phase by a layer-by-layer self-assembly method. The hybrid shell assembled on the silica core was formed using a surfactant as template by the copolymerization reaction of tetraethyl orthosilicate and the nanocellulose derivative bearing triethoxysilyl and 3,5-dimethylphenyl groups. The resulting nanocellulose hybrid core-shell chiral packing materials (CPMs) were characterized and packed into columns, and their enantioseparation performance was evaluated by high performance liquid chromatography. The results showed that CPMs exhibited uniform surface morphology and core-shell structures. Various types of chiral compounds were efficiently separated under normal and reversed phase mode. Moreover, chloroform and tetrahydrofuran as mobile phase additives could obviously improve the resolution during the chiral separation processes. CPMs still have good chiral separation property when eluted with solvent systems with a high content of tetrahydrofuran and chloroform, which proved the high solvent resistance of this new material.

  3. A simple approach to prepare monodisperse mesoporous silica nanospheres with adjustable sizes.

    PubMed

    Yu, Meihua; Zhou, Liang; Zhang, Jun; Yuan, Pei; Thorn, Peter; Gu, Wenyi; Yu, Chengzhong

    2012-06-15

    A new and facile approach has been developed to prepare monodisperse mesoporous silica nanospheres (MMSNs) with controlled particle sizes and pore structures. In our approach, MMSNs were synthesized simply in a sodium acetate solution without adding any other alkali or alcohol additives. MMSNs have a spherical shape and uniform particle sizes, which can be adjusted from 50 to 110 nm by increasing the reaction temperature from 40 to 80 °C. By performing a subsequent hydrothermal treatment (HT) under basic condition (pH=~11.5) at 130 °C, the mesoporous pore volume and surface area can be enhanced, while keeping the mono-dispersion characteristics and the mesopore size almost unchanged. The pore sizes of MMSNs can be adjusted from 2.8 to 4.0 nm under acidic solutions by changing the HT temperature from 100 to 130 °C. The formation process of MMSNs has been investigated by transmission electron microscopy (TEM) and attenuated total reflection Fourier transform infrared (ATR-FTIR) techniques. A spherical micelle templating mechanism is proposed to explain the formation of MMSNs in our system, which is different from that of traditional highly ordered mesoporous silica nanoparticles (MCM-41).

  4. Preparation, characterization and selective recognition for vanillic acid imprinted mesoporous silica polymers

    NASA Astrophysics Data System (ADS)

    Li, Hui; Xu, Miaomiao; Wang, Susu; Lu, Cuimei; Li, Zhiping

    2015-02-01

    A vanillic acid imprinted mesoporous silica polymer (MIPs) was prepared by copolymerizing a modified mesoporous silica molecular sieve with template molecule, functional monomer and cross-linker in present work. Interaction between the template and functional monomer was investigated by ultraviolet/visible spectrophotometry. These MIPs were characterized by Fourier transmission infrared spectrometry (FTIR) and scanning electron microscopy (SEM). Adsorption dynamics and thermodynamic behavior of MIPs was explored and the selective recognition capability evaluated. Also, the applicability for the MIPs as solid phase extraction media was tested. Results indicated the 1:1 (mole ratio) complex of vanillic acid-4-vinylpyridine might predominate in the pre-polymerization mixture and the MIPs obtained possessed rapid binding dynamics and higher affinity toward template molecules, reaching adsorption equilibrium within 230 min with the highest adsorption amount of 50.7 mg g-1. Freundlich model was shown best to describe isotherm adsorption for the MIPs. The MIPs could selectively bind template molecule with selectivity coefficients of 1.36-1.50. In addition, a higher enrichment capability when using it for gathering target compound from methanol extract of Artemisia stelleriana and a good reusability during adsorption-desorption recycling use could be observed.

  5. Preparation and complex characterization of silica holmium sol-gel monoliths.

    PubMed

    Cacaina, D; Areva, S; Laaksonen, H; Simon, S; Ylänen, H

    2011-01-01

    Amorphous, sol-gel derived SiO(2) are known to biocompatible and bioresorbable materials. Biodegradable and inert materials containing radioactive isotopes have potential application as delivery vehicles of the beta radiation to the cancer tumors inside the body. Incorporation of holmium in the sol-gel derived SiO(2) could lead to the formation of a biodegradable material which could be used as carrier biomaterial for the radiation of radioactive holmium to the various cancer sites. The homogeneity of the prepared sol-gel silica holmium monoliths was investigated by Back Scattered Electron Imaging of Scanning Electron Microscope equipped with Energy Dispersive X-ray Analysis, X-ray Induced Photoelectron Spectroscopy and Nuclear Magnetic Resonance Spectroscopy. The biodegradation of the monoliths was investigated in Simulated Body Fluid and TRIS (Trizma pre-set Crystals) solution. The results show that by suitable tailoring of the sol-gel processing parameters holmium can be homogeneously incorporated in the silica matrix with a controlled biodegradation rate.

  6. Facile preparation and characterization of modified magnetic silica nanocomposite particles for oil absorption

    NASA Astrophysics Data System (ADS)

    Yu, Liuhua; Hao, Gazi; Liang, Qianqian; Zhou, Shuai; Zhang, Ning; Jiang, Wei

    2015-12-01

    In this study, a novel environmental-friendly and superhydrophobic oil absorbent was fabricated by modifying magnetic silica nanocomposites. It was demonstrated that the modified rough magnetic silica nanocomposite particles possessed a number of superior features such as superhydrophobicity, superoleophilicity, and high oil-water separation efficiency etc. Moreover, the as-obtained material could be used as excellent absorbents for high density oils such as toluene and many organic liquids including viscous oils e.g. lubricating oil. The lubricating oil intake capacity for the nanocomposites was 7.15 times of its own weight. Importantly, the oil-absorption process of the nanocomposites was selective, fast and efficient when they were used in the purification of oil-contaminated water. Notably, the oil-absorbed nanocomposites could be renewed after suitable absolute ethanol washing and natural drying. In addition, the renewed nanocomposites still remained high oil-absorption capacity after the 20th cycle. These inspiring results show that the oil-absorbent material has good prospects for selection removal of oils and organic solvents on water surface. It is believed that the present work may have provided a novel and facile way for preparing environmental-friendly materials with ideal properties.

  7. Preparation of glycerol carbonate esters by using hybrid Nafion-silica catalyst.

    PubMed

    Climent, María J; Corma, Avelino; Iborra, Sara; Martínez-Silvestre, Sergio; Velty, Alexandra

    2013-07-01

    Glycerol carbonate esters (GCEs), which are valuable biomass-derivative compounds, have been prepared through the direct esterification of glycerol carbonate and long organic acids with different chain lengths, in the absence of solvent, and with heterogeneous catalysts, including acidic-organic resins, zeolites, and hybrid organic-inorganic acids. The best results, in terms of activity and selectivity towards GCEs, were obtained using a Nafion-silica composite. A full reaction scheme has been established, and it has been demonstrated that an undesired competing reaction results in the generation of glycerol and esters derived from a secondary hydrolysis of the endocyclic ester group, which is attributed to water formed during the esterification reaction. The influence of temperature, substrate ratio, catalyst-to-substrate ratio, and the use of solvent has been studied and, under optimized reaction conditions and with the adequate catalyst, it was possible to achieve 95% selectivity for the desired product at 98% conversion. It was demonstrated that the reaction rate decreased as the number of carbon atoms in the linear alkyl chain of the carboxylic acid increased for both p-toluenesulfonic acid and Nafion-silica nanocomposite (Nafion SAC-13) catalysts. After fitting the experimental data to a mechanistically based kinetic model, the reaction kinetic parameters for Nafion SAC-13 catalysis were determined and compared for reactions involving different carboxylic acids. A kinetic study showed that the reduced reactivity of carboxylic acids with increasing chain lengths could be explained by inductive as well as steric effects.

  8. Sonochemical preparation of silica nanorods for gene delivery using single-walled carbon nanotubes as templates.

    PubMed

    Lee, Kyoung G; Min, Jung Sun; Wi, Rinbok; Kim, Jin Chul; Ahn, Jeong Keun; Kim, Do Hyun

    2011-01-01

    Silica nanorods were fabricated with single-walled carbon nanotubes (SWCNTs) via ultrasound. The diameter of the resulting SWCNT-silica particles ranged from 60 to 70 nm. The morphology of this composite material was investigated via scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The individual SWCNTs are uniformly coated with silica and formed a unique nanocomposite material. The important role of ultrasound and the mechanism of silica layer formation on SWCNTs were explained via the hydrolysis of the silica source and the adsorption of the siloxane groups on the SWCNT surfaces under ultrasound irradiation. The amino-functionalized silica nanorods were demonstrated as non-viral vectors for gene delivery.

  9. Preparation, characterization and photocatalytic activity of manganese doped TiO(2) immobilized on silica gel.

    PubMed

    Xu, Yuehua; Lei, Bo; Guo, Laiqiu; Zhou, Wuyi; Liu, Youqin

    2008-12-15

    A series of Mn-TiO(2)/SiO(2) (silica gel loaded with manganese doped TiO(2)) photocatalysts have been prepared by sol-gel method, and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). Photocatalytic activities were enhanced in photocatalytic degradation of methyl orange over Mn-TiO(2)/SiO(2). XPS analysis shows that a Ti-O-Si or Ti-O-Mn bond is formed on the surface of photocatalyst. Mn is doped as a mixture of Mn(2+) and Mn(3+) on the surface of 1.0mol% Mn-TiO(2)/SiO(2). Mn(3+) appears to trap electrons and prohibit the electron-hole recombination. The electrons trapped in Mn(3+) site are subsequently transferred to the adsorbed O(2). As a result, the combination of the electron-hole pair was reduced.

  10. Titanized silica-based stationary phases prepared with thermally and microwave-immobilized poly(methyloctylsiloxane).

    PubMed

    Fonseca, Dania A; Collins, Kenneth E; Collins, Carol H

    2004-03-19

    Silica supports having their surface modified with titanium oxide were prepared and coated with poly(methyloctylsiloxane) (PMOS). Subsequently, immobilization of the polysiloxane was induced by thermal treatment or microwave radiation. The thermal treatment was carried out for different times (4, 8, 16 and 24 h) at temperatures ranging between 100 and 220 degrees C. For PMOS immobilization by microwave radiation, 452, 520 and 586 W power levels and exposure times of 5, 15 and 30 min were used. After extraction of non-immobilized polymer, the chromatographic properties of the phases were evaluated. The phase immobilized at 120 degrees C for 8 h presented the best chromatographic parameters, suggesting that the quantity of acidic hydroxyl groups on the support surface was reduced, resulting in fewer undesirable interactions of a basic solute with the silanols not removed or covered on the support surface.

  11. N-doped mesoporous carbons supported palladium catalysts prepared from chitosan/silica/palladium gel beads.

    PubMed

    Zeng, Minfeng; Wang, Yudong; Liu, Qi; Yuan, Xia; Feng, Ruokun; Yang, Zhen; Qi, Chenze

    2016-08-01

    In this study, a heterogeneous catalyst including palladium nanoparticles supported on nitrogen-doped mesoporous carbon (Pd@N-C) is synthesized from palladium salts as palladium precursor, colloidal silica as template, and chitosan as carbon source. N2 sorption isotherm results show that the prepared Pd@N-C had a high BET surface area (640m(2)g(-1)) with large porosity. The prepared Pd@N-C is high nitrogen-rich as characterized with element analysis. X-ray photoelectron spectroscopy (XPS), high-resolution transmission electron microscopy (HR-TEM), and Raman spectroscopy characterization of the catalyst shows that the palladium species with different chemical states are well dispersed on the nitrogen-containing mesoporous carbon. The Pd@N-C is high active and shows excellent stability as applied in Heck coupling reactions. This work supplies a successful method to prepare Pd heterogeneous catalysts with high performance from bulk biopolymer/Pd to high porous nitrogen-doped carbon supported palladium catalytic materials.

  12. Preparation and characterization of phosphorylated Zr-doped hybrid silica/PSF composite membrane.

    PubMed

    Zhang, Yuqing; Jin, Zhenhua; Shan, Xing; Sunarso, Jaka; Cui, Ping

    2011-02-15

    Polysulfone (PSF) membranes are broadly applied in many fields owing to good physicochemical stability, resistance to oxidation and chlorine. But when treated with wastewater containing oil, PSF membranes are easy to be contaminated for its hydrophobicity, which can result in the declining of flux and lifespan of the membrane and limit their application in large scale. To enhance the capability of PSF membrane in the above circumstances, phosphorylated Zr-doped hybrid silica particles (SZP particles) were firstly prepared. SZP particles have various point defects inside their structure and lots of hydroxide radicals on their surface. SZP particles were added to the porous matrix of PSF to prepare a novel composite membrane (SZP/PSF) through a phase inversion process. Finally, the optimum preparation conditions of SZP/PSF composite membranes were determined. The optimum conditions are: the mass ratio of PSF, PEG400 and SZP is 12:10:10; ultrasound 10 min inside each 30 min; the pre-evaporating time is 10s. Optimized SZP/PSF composite membrane was characterized by scanning electron microscope (SEM) and ultrafiltration experiment. The results indicate that SZP particles can be uniformly dispersed in SZP/PSF composite membranes with excellent hydrophilic property, antifouling capability and tensile strength. Therefore, it can be concluded that the optimized SZP/PSF composite membrane is desirable in the treatment of wastewater containing oil and wastewater.

  13. Preparation of mesoporous silica thin films by photocalcination method and their adsorption abilities for various proteins.

    PubMed

    Kato, Katsuya; Nakamura, Hitomi; Yamauchi, Yoshihiro; Nakanishi, Kazuma; Tomita, Masahiro

    2014-07-01

    Mesoporous silica (MPS) thin film biosensor platforms were established. MPS thin films were prepared from tetraethoxysilane (TEOS) via using sol-gel and spin-coating methods using a poly-(ethylene oxide)-block-poly-(propylene oxide)-block-poly-(ethylene oxide) triblock polymer, such as P123 ((EO)20(PO)70(EO)20) or F127 ((EO)106(PO)70(EO)106), as the structure-directing agent. The MPS thin film prepared using P123 as the mesoporous template and treated via vacuum ultraviolet (VUV) irradiation to remove the triblock copolymer had a more uniform pore array than that of the corresponding film prepared via thermal treatment. Protein adsorption and enzyme-linked immunosorbent assay (ELISA) on the synthesized MPS thin films were also investigated. VUV-irradiated MPS thin films adsorbed a smaller quantity of protein A than the thermally treated films; however, the human immunoglobulin G (IgG) binding efficiency was higher on the former. In addition, protein A-IgG specific binding on MPS thin films was achieved without using a blocking reagent; i.e., nonspecific adsorption was inhibited by the uniform pore arrays of the films. Furthermore, VUV-irradiated MPS thin films exhibited high sensitivity for ELISA testing, and cytochrome c adsorbed on the MPS thin films exhibited high catalytic activity and recyclability. These results suggest that MPS thin films are attractive platforms for the development of novel biosensors.

  14. Preparation of nanoscale Bacillus thuringiensis chitinases using silica nanoparticles for nematicide delivery.

    PubMed

    Qin, Xu; Xiang, Xuemei; Sun, Xiaowen; Ni, Hong; Li, Lin

    2016-01-01

    A series of amino, carboxylic, and aldehydic surface-grafted silica nanoparticles (SNPs) was prepared based on SiO2 NYSi40 nanoparticles to develop an efficient, biocompatible, and cost-effective biopesticide delivery system. Bacillus thuringiensis chitinase (Chi9602) was immobilized onto SNP surface to prepare nanoscale chitinases (SNPCs) through electrostatic adsorption and covalent binding. The specimens were characterized by Fourier transform infrared, scanning electron microscopy, and zeta-potential analyses. The delivery capacity of the SNPs in Caenorhabditis elegans N2 was observed by immunofluorescence. Results demonstrated that amino-grafted SiO2 nanoparticles with Chi9602 electrostatically adsorbed onto their surface (SNPC2) exhibited a relatively high enzyme immobilization rate (80.2%) and the highest (94.1%) residual enzyme activity among all SNPCs. SNPC2 also showed wider pH tolerance and relatively higher thermostability and ultraviolet radiation resistance capacity than Chi9602. Bioassays further showed that SNPC2 synergistically enhanced the nematicidal effect of B. thuringiensis YBT-020 preparation against C. elegans, with a reduced LC50 of 8.35mg/mL and a shortened LT50 of 12.04h. Immunofluorescence assays showed that SNPC2 had considerable delivery capacity to carry a large protein into C. elegans. Therefore, SNP2 can serve as an efficient nanocarrier for the delivery of macromolecular proteic biopesticides or drugs, indicating potential agricultural or biotechnological applications.

  15. Preparation of 4-butylaniline-bonded silica gel for the solid-phase extraction of flavone glycosides.

    PubMed

    Chu, Ganghui; Cai, Wensheng; Shao, Xueguang

    2015-04-01

    To extract flavone glycosides efficiently, a new extraction material based on 4-butylaniline-bonded silica gel was prepared using a two-step grafting method including a ring-opening reaction and synchronous hydrolysis. Preparation of the silica-based material was easily achieved under mild conditions, and the material was characterized by Fourier transform infrared spectroscopy, elemental analysis, and scanning electron microscopy. The material was used in solid-phase extraction, and the extraction can be performed in neutral conditions without regard to ionic strength. Selectivity tests of 14 compounds on the extraction cartridge showed that the material has a high affinity to flavone glycosides in contrast to octadecyl silica, and the extraction yields for four flavone glycosides were found to be >93%. Selectivity tests further reveal that the adsorption on its surface is likely attributed to multiple interactions, including hydrophobic interactions, π-π interactions, and hydrogen bonding. To explore the applicability of 4-butylaniline-bonded silica gel, naringin and hesperidin from Simotang oral liquid were extracted, and the extraction yields were >90%, which is distinguished from <28% on octadecyl silica cartridge.

  16. Preparation of silica thin films by novel wet process and study of their optical properties.

    PubMed

    Im, Sang-Hyeok; Kim, Nam-Jin; Kim, Dong-Hwan; Hwang, Cha-Won; Yoon, Duck-Ki; Ryu, Bong-Ki

    2012-02-01

    Silicon dioxide (SiO2) thin films have gained considerable attention because of their various industrial applications. For example, SiO2 thin films are used in superhydrophilic self-cleaning surface glass, UV protection films, anti-reflection coatings, and insulating materials. Recently, many processes such as vacuum evaporation, sputtering, chemical vapor deposition, and spin coating have been widely applied to prepare thin films of functionally graded materials. However, these processes suffer from several engineering problems. For example, a special apparatus is required for the deposition of films, and conventional wet processes are not suitable for coating the surfaces of substrates with a large surface area and complex morphology. In this study, we investigated the film morphology and optical properties of SiO2 films prepared by a novel technique, namely, liquid phase deposition (LPD). Images of the SiO2 films were obtained by scanning electron microscopy (SEM) and atomic force microscopy (AFM) in order to study the surface morphology of these films: these images indicate that films deposited with different reaction times were uniform and dense and were composed of pure silica. Optical properties such as refractive index and transmittance were estimated by UV-vis spectroscopy and ellipsometry. SiO2 films with porous structures at the nanometer scale (100-250 nm) were successfully produced by LPD. The deposited film had excellent transmittance in the visible wavelength region.

  17. Preparation of Silica/Reduced Graphene Oxide Nanosheet Composites for Removal of Organic Contaminants from Water.

    PubMed

    Li, Wen; Liu, Wei; Wang, Haifei; Lu, Wensheng

    2016-06-01

    Graphene-based composites open up new opportunities as effective adsorbents for the removal of organic contaminants from water. In this article, we report a novel and facile process to synthesize well-dispersed silica/reduced graphene oxide (SiO2/RGO) nanosheet composites. The SiO2/RGO nanosheet composites are prepared through a modified sol-gel process with in situ hydrolysis of tetraethoxysilane (TEOS) on graphene oxide (GO) nanosheet, followed by reduction of GO to graphene. In comparison with the RGO nanosheets, the as-prepared SiO2/RGO nanosheet composites have a larger surface area and good aqueous disperse ability. In addition, the application of SiO2/RGO nanosheet composites was demonstrated on removing organic dyes from water. The SiO2/RGO nanosheet composites show rapid and stable adsorption performance on removal of Methylene Blue (MB) and thionine (TH) from water. It is indicated that the resulting SiO2/RGO composites can be utilized as efficient adsorbents for the removal of organic contaminants from water.

  18. Preparation of micropatterns with profile heights up to 30 microns from silica sols

    NASA Astrophysics Data System (ADS)

    Mennig, Martin; Gier, A.; Krug, Herbert; Schmidt, Helmut K.

    1997-10-01

    A new synthesis and processing route for SiO2 glass like micropatterns with heights up to 30 micrometer by gel embossing and thermal densification has been developed. For this reason an organically modified nanoparticulate sol prepared by acid catalysis of methyl- and phenyl- triethoxysilane and tetraethyl orthosilicate in combination with colloidal silica sol was used. Sol coatings with thicknesses up to 15 micrometer are obtained by dipping of float glass substrates. After a predrying step of about 60 s micropatterns are obtained using a pressure of only 2.5 mN/mm2. Due to this low pressure, flexible and low cost silicon rubber stampers can be used. The gelation time of the sol can be extended from 5 d to 16 days and the working time for embossing can be extended from 60 s up to 100 s by a partial replacement of methyl silane by phenyl silane from 0 to 20 mole %. After embossing and drying at 50 degrees Celsius the patterned layer was densified at temperatures up to 500 degrees Celsius to 95% density as indicated by refractive index measurements. It is assumed that the densification process is strongly promoted by the used colloidal silica nano particles. The linear shrinkage of the micropatterns is limited to about 25% due to the high solid content of the sol and the high green density of the layers. Since the structures are densified at temperatures far below Tg sharp edged patterns can be obtained as shown by high resolution secondary electron microscopy. The capability of this technique is demonstrated by the fabrication of light trapping structures with pyramides of 7 micrometer in height and 10 micrometer in width on an area of 20 multiplied by 20 mm2 and micro lens arrays of lenses with 30 micrometer in height and 600 micrometer in diameter on an area of 20 multiplied by 30 mm2.

  19. Preparation of porous TiO{sub 2}/silica composites without any surfactants

    SciTech Connect

    Ren Suxia; Zhao Xu; Zhao Lina; Yuan Meirong; Yu Yang; Guo Yupeng Wang Zichen

    2009-02-15

    TiO{sub 2}-SiO{sub 2} composites, with high specific surface area (up to 308 m{sup 2}/g), large pore volume, and narrow distribution with average pore sizes of 3.2 nm, have been synthesized from wollastonite and titanium sulfate in the absence of any surfactants. Calcium sulfate, a microsolubility salt, plays an important role in the formation of pores in this porous TiO{sub 2}/silica composite. The microstructure and chemical composition of composite were characterized by X-ray diffractometry (XRD), transmission electron microscopy (TEM) equipped with energy-dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectrometer (XPS) and N{sub 2} adsorption and desorption analysis. The as-prepared porous titanium dioxide-silicon dioxide composites with high specific surface area and well-crystallized anatase contents were used as an efficient photocatalyst. - Graphical abstract: TiO{sub 2}-SiO{sub 2} composites have been synthesized from wollastonite and titanium sulfate in the absence of any surfactants. In acid Ti(SO{sub 4}){sub 2} solution, Ca and Si ions in chain-like wollastonite could dissolve into the bulk solution and slightly soluble CaSO{sub 4} crystal phase and silicic acid formed. The concentration of the titanium species in the reaction solution is expected to increase with the hydrolysis process, nucleation starts. After the start of the nucleation, a very small amount of TiO{sub 2}, silicate and CaSO{sub 4} particle deposited together and formed composites. Some cavities formed during the washing step through the dissolution of CaSO{sub 4} crystal phase. The bulk of the material is then transformed from wollastonite into TiO{sub 2}/silica composites.

  20. Preparation of magnetic mesoporous silica nanoparticles as a multifunctional platform for potential drug delivery and hyperthermia

    PubMed Central

    Yu, Xia; Zhu, Yufang

    2016-01-01

    Abstract We report the preparation of magnetic mesoporous silica (MMS) nanoparticles with the potential multifunctionality of drug delivery and magnetic hyperthermia. Carbon-encapsulated magnetic colloidal nanoparticles (MCN@C) were used to coat mesoporous silica shells for the formation of the core-shell structured MMS nanoparticles (MCN@C/mSiO2), and the rattle-type structured MMS nanoparticles (MCN/mSiO2) were obtained after the removal of the carbon layers from MCN@C/mSiO2 nanoparticles. The morphology, structure, magnetic hyperthermia ability, drug release behavior, in vitro cytotoxicity and cellular uptake of MMS nanoparticles were investigated. The results revealed that the MCN@C/mSiO2 and MCN/mSiO2 nanoparticles had spherical morphology and average particle sizes of 390 and 320 nm, respectively. The MCN@C/mSiO2 nanoparticles exhibited higher magnetic hyperthermia ability compared to the MCN/mSiO2 nanoparticles, but the MCN/mSiO2 nanoparticles had higher drug loading capacity. Both MCN@C/mSiO2 and MCN/mSiO2 nanoparticles had similar drug release behavior with pH-controlled release and temperature-accelerated release. Furthermore, the MCN@C/mSiO2 and MCN/mSiO2 nanoparticles showed low cytotoxicity and could be internalized into HeLa cells. Therefore, the MCN@C/mSiO2 and MCN/mSiO2 nanoparticles would be promising for the combination of drug delivery and magnetic hyperthermia treatment in cancer therapy. PMID:27877873

  1. Preparation of composite with silica-coated nanoparticles of iron oxide spinels for applications based on magnetically induced hyperthermia

    NASA Astrophysics Data System (ADS)

    Andrade, Angela L.; Fabris, José D.; Pereira, Márcio C.; Domingues, Rosana Z.; Ardisson, José D.

    2013-04-01

    It is reported a novel method to prepare magnetic core (iron oxide spinels)-shell (silica) composites containing well-dispersed magnetic nanoparticles in aqueous solution. The synthetic process consists of two steps. In a first step, iron oxide nanoparticles obtained through co-precipitation are dispersed in an aqueous solution containing tetramethylammonium hydroxide; in a second step, particles of this sample are coated with silica, through hydrolyzation of tetraethyl orthosilicate. The intrinsic atomic structure and essential properties of the core-shell system were assessed with powder X-ray diffraction, Fourier transform infrared spectrometry, Mössbauer spectroscopy and transmission electron microscopy. The heat released by this ferrofluid under an AC-generated magnetic field was evaluated by following the temperature evolution under increasing magnetic field strengths. Results strongly indicate that this ferrofluid based on silica-coated iron oxide spinels is technologically a very promising material to be used in medical practices, in oncology.

  2. High-throughput preparation of hexagonally ordered mesoporous silica and gadolinosilicate nanoparticles for use as MRI contrast agents.

    PubMed

    Tse, Nicholas M K; Kennedy, Danielle F; Moffat, Bradford A; Kirby, Nigel; Caruso, Rachel A; Drummond, Calum J

    2012-08-13

    The development of biomedical nanoparticulate materials for use in diagnostics is a delicate balance between performance, particle size, shape, and stability. To identify materials that satisfy all of the criteria it is useful to employ automated high-throughput (HT) techniques for the study of these materials. The structure and performance of surfactant templated mesoporous silica is very sensitive to a wide number of variables. Variables, such as the concentration of the structure-directing agent, the cosolvent and dopant ions and also the temperature and concentration of quenching all have an influence on the structure, surface chemistry, and therefore, the performance of the mesoporous silica nanoparticles generated. Using an automated robotic synthetic platform, a technique has been developed for the high-throughput preparation of mesoporous silica and gadolinium-doped silicate (gadoliniosilicate) nanoparticulate MRI contrast agents. Twelve identical repeats of both the mesoporous silica and gadolinosilicate were synthesized to investigate the reproducibility of the HT technique. Very good reproducibility in the production of the mesoporous silica and the gadolinosilcate materials was obtained using the developed method. The performance of the gadolinosilicate materials was comparable as a T(1) agent to the commercial MRI contrast agents. This HT methodology is highly reproducible and an effective tool that can be translated to the discovery of any sol-gel derived nanomaterial.

  3. Silica-supported Au@hollow-SiO2 particles with outstanding catalytic activity prepared via block copolymer template approach.

    PubMed

    Shajkumar, Aruni; Nandan, Bhanu; Sanwaria, Sunita; Albrecht, Victoria; Libera, Marcin; Lee, Myong-Hoon; Auffermann, Gudrun; Stamm, Manfred; Horechyy, Andriy

    2017-04-01

    Catalytically active Au@hollow-SiO2 particles embedded in porous silica support (Au@hollow-SiO2@PSS) were prepared by using spherical micelles from poly(styrene)-block-poly(4-vinyl pyridine) block copolymer as a sacrificial template. Drastic increase of the shell porosity was observed after pyrolytic removal of polymeric template because the stretched poly(4-vinyl pyridine) chains interpenetrating with silica shell acted as an effective porogen. The embedding of Au@hollow-SiO2 particles in porous silica support prevented their fusion during pyrolysis. The catalytic activity of Au@hollow-SiO2@PSS was investigated using a model reaction of catalytic reduction of 4-nitrophenol and reductive degradation of Congo red azo-dye. Significantly, to the best of our knowledge, Au@hollow-SiO2@PSS catalyst shows the highest activity among analogous systems reported till now in literature. Such high activity was attributed to the presence of multiple pores within silica shell of Au@hollow-SiO2 particles and easy accessibility of reagents to the catalytically active sites of the ligand-free gold surface through the porous silica support.

  4. Preparation of silica stabilized biological templates for the production of metal and layered nanoparticles

    SciTech Connect

    Culver, James N; Royston, Elizabeth; Brown, Adam; Harris, Michael

    2013-02-26

    The present invention relates to a system and method providing for increased silica growth on a bio-template, wherein the bio-template is pretreated with aniline to produce a uniform silica attractive surface and yielding a significant silica layers of at least 10 nm, and more preferably at least 20 nm in thickness, thereby providing for a high degree of stability to the bio-template.

  5. Preparation and in vitro characterisation of bioactive mesoporous silica microparticles for drug delivery applications.

    PubMed

    Prokopowicz, Magdalena; Czarnobaj, Katarzyna; Szewczyk, Adrian; Sawicki, Wiesław

    2016-03-01

    The aim of this study was to evaluate the surface mineralization activity and in vitro drug behaviour potential of new mesoporous silica microparticles (MSM). The unmodified MSM (MSM-0%Ca) and calcium-modified MSM (MSM-5%Ca, MSM-15%Ca, MSM-25%Ca) were prepared using the self-assembling method. Calcium diethoxide was used as a calcium precursor. Doxorubicin hydrochloride (DOX), used as an anticancer model drug, was selected to the drug loading and release studies. The DOX loading into the microparticles was performed by liquid adsorption process. The self-formation of carbonate hydroxyapatite (C-Hap) on the MSM surface was examined under in vitro biomimetic conditions. The samples were characterised by means of scanning-transmission electron microscopy (STEM) and energy dispersive X-ray spectrometry, powder X-ray diffraction, Fourier transform infrared spectroscopy, and nitrogen adsorption-desorption measurements. The results indicated an inverse relationship--while increasing the total amount of calcium in the MSM composition the surface area and pore volume decrease with a simultaneous increase in the pore size. This was correlated with a progressive increase in the surface mineralization ability--especially its initial promotion, and in the decrease in MSM drug loading efficiency. The release rate of the DOX can be effectively tailored by varying the amount of calcium, where the elution rate of DOX increases with an increasing amount of the Ca precursor.

  6. Silica cross-linked micelles loading with silicon nanoparticles: preparation and characterization.

    PubMed

    Pan, Guo-Hui; Barras, Alexandre; Boussekey, Luc; Boukherroub, Rabah

    2013-08-14

    A new family of luminescent and stable silicon-based nanoparticles (NPs), silica cross-linked pluronic F127 (PF127) micelles loaded with decyl capped silicon nanoparticles (decyl-SiNPs), were synthesized in aqueous media. The decyl-SiNPs were prepared by first liberating hydride terminated SiNPs (H-SiNPs) from a porous silicon matrix followed by their functionalization via hydrosilylation with 1-decene under photochemical activation. The silicon-based NPs exhibit bright photoluminescence (PL) with a quantum yield of ∼3.8% and peaking at ∼2.0 eV, which lies within the transmission window that is useful for biological imaging. They display a hydrodynamic size of ∼25 nm with exterior polyethylene oxide (PEO) blocks stretching out in aqueous media. Chloroform was found to quench the excitation at energy above 4.9 eV by shielding the incident light or relaxing the charge carriers, which highlights that caution against solvent interference should be taken when performing the studies on PL origin and luminescence efficiency of SiNPs. For PF127, the blocks of hydrophilic PEO participate in the PL quenching, while poly(propylene oxide) (PPO) does not. The colloidal solution displays excellent PL stability against salt (NaCl) and temperature but is susceptible to basic solution at pH above 9.

  7. Yb³⁺-doped large core silica fiber for fiber laser prepared by glass phase-separation technology.

    PubMed

    Chu, Yingbo; Ma, Yunxiu; Yang, Yu; Liao, Lei; Wang, Yibo; Hu, Xiongwei; Peng, Jinggang; Li, Haiqing; Dai, Nengli; Li, Jinyan; Yang, Luyun

    2016-03-15

    We report on the preparation and optical characteristics of an Yb(3+)-doped large core silica fiber with the active core prepared from nanoporous silica rod by the glass phase-separation technology. The measurements show that the fiber has an Yb(3+) concentration of 9811 ppm by weight, a low background attenuation of 0.02 dB/m, and absorption from Yb(3+) about 5.5 dB/m at 976 nm. The laser performance presents a high slope efficiency of 72.8% for laser emission at 1071 nm and a low laser threshold of 3 W within only 2.3 m fiber length. It is suggested that the glass phase-separation technology shows great potential for realizing active fibers with larger core and complex fiber designs.

  8. Preparation of silica stabilized Tobacco mosaic virus templates for the production of metal and layered nanoparticles.

    PubMed

    Royston, Elizabeth S; Brown, Adam D; Harris, Michael T; Culver, James N

    2009-04-15

    The use of biological molecules as templates for the production of metal nanoparticles and wires is often limited by the stability of the bio-template and its affinity for nucleating metal deposition. In this study, Tobacco mosaic virus (TMV) was used as a model bio-template to investigate the use of silica coatings as a means to both enhance template stability and increase its affinity for metal ions. Results indicate that the unmodified TMV particle can function as a template for the growth of thin (<1 nm) silica layers. However, this thin silica shell did not enhance the stability of the template during metal deposition. To increase silica growth on the TMV template, a pretreatment with aniline was used to produce a uniform silica attractive surface. Aniline pretreated templates yielded significant silica layers of >20 nm in thickness. These silica shells conferred a high degree of stability to the TMV particle and promoted the deposition of various metal nanoparticles through conventional silica mineralization chemistries. This process provides a simple and robust method for the layering of inorganics onto a biological template.

  9. Supported microporous ceramic membranes

    DOEpatents

    Webster, E.; Anderson, M.

    1993-12-14

    A method for the formation of microporous ceramic membranes onto a porous support includes placing a colloidal suspension of metal or metal oxide particles on one side of the porous support and exposing the other side of the porous support to a drying stream of gas or a reactive gas stream so that the particles are deposited on the drying side of the support as a gel. The gel so deposited can be sintered to form a supported ceramic membrane useful for ultrafiltration, reverse osmosis, or molecular sieving having mean pore sizes less than 100 Angstroms. 4 figures.

  10. Supported microporous ceramic membranes

    DOEpatents

    Webster, Elizabeth; Anderson, Marc

    1993-01-01

    A method for permformation of microporous ceramic membranes onto a porous support includes placing a colloidal suspension of metal or metal oxide particles on one side of the porous support and exposing the other side of the porous support to a drying stream of gas or a reactive gas stream so that the particles are deposited on the drying side of the support as a gel. The gel so deposited can be sintered to form a supported ceramic membrane useful for ultrafiltration, reverse osmosis, or molecular sieving having mean pore sizes less than 100 Angstroms.

  11. Influence of roasting-quenching pretreatment on the rice husk silica prepared by calcination method

    NASA Astrophysics Data System (ADS)

    Maksum, Ahmad; Rustandi, Andi; Permana, Sulaksana; Soedarsono, Johny Wahyuadi

    2017-03-01

    Calcination is a simple method to produce silica from rice husk (RH). One of the key to obtain higher purity silica from rice husk by calcination method is the effectiveness of impurities removal, especially potassium, from RH surface before calcination process. So, in the present study, an attempt has been made to produce high purity silica powder by using calcination method with the combination of roasting-quenching and acid leaching as a pretreatment to eliminate metal impurities, especially potassium, detected by using inductively coupled plasma mass spectrometry (ICP-MS). Finally, the high purity silica, 99.928% was obtained by roasting and calcination temperature of 300°C and 650°C, respectively. However, by considering less energy usage and silica purity achievement, the combination of 300°C roasting-quenching, 1M hydrochloric acid leaching, and calcination at the temperature of 600°C was the best route.

  12. Preparation of frustule-like 1,2-ethylene-silica nanospheres through a chiral amphiphile/organic solvent dual-templating approach

    SciTech Connect

    Zhao, Yanwei; Huang, Zhibin; Yan, Zhuojun; Wang, Sibing; Li, Baozong; Li, Yi; Yang, Yonggang

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Frustule-like 1,2-ethylene-silicas were prepared through a dual-templating approach. ► The morphologies and pore architectures of the 1,2-ethylene-silicas are tunable. ► Mesoporous 1,2-ethylene-silica nanotubes were also prepared. -- Abstract: Hollow silica nanospheres with mesopores in the walls have been widely studied because of their potential applications in catalysis and drug release. Hollow organosilica nanospheres also attracted much attention because of their tunable wall backbones and wider applications. Herein, frustule-like 1,2-ethylene-silicas were obtained using a chiral amphiphile, CHCl{sub 3}, and a dual-templating approach. The morphologies and pore architectures of the 1,2-ethylene-silicas are tunable by changing the amount of CHCl{sub 3} in the reaction mixture. With the addition of CHCl{sub 3} in the reaction mixtures, hollow 1,2-ethylene-silica nanospheres with opened mesopores in the walls were feasible. Moreover, 1,2-ethylene-silicas with mesopores on the surfaces and coiled pore channels within the walls were obtained using the chiral amphiphile in a single-templating approach. These 1,2-ethylene-silicas were characterized using field-emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction and N{sub 2} sorptions.

  13. Ordered mesoporous silica prepared by quiescent interfacial growth method - effects of reaction chemistry

    PubMed Central

    2013-01-01

    Acidic interfacial growth can provide a number of industrially important mesoporous silica morphologies including fibers, spheres, and other rich shapes. Studying the reaction chemistry under quiescent (no mixing) conditions is important for understanding and for the production of the desired shapes. The focus of this work is to understand the effect of a number of previously untested conditions: acid type (HCl, HNO3, and H2SO4), acid content, silica precursor type (TBOS and TEOS), and surfactant type (CTAB, Tween 20, and Tween 80) on the shape and structure of products formed under quiescent two-phase interfacial configuration. Results show that the quiescent growth is typically slow due to the absence of mixing. The whole process of product formation and pore structuring becomes limited by the slow interfacial diffusion of silica source. TBOS-CTAB-HCl was the typical combination to produce fibers with high order in the interfacial region. The use of other acids (HNO3 and H2SO4), a less hydrophobic silica source (TEOS), and/or a neutral surfactant (Tweens) facilitate diffusion and homogenous supply of silica source into the bulk phase and give spheres and gyroids with low mesoporous order. The results suggest two distinct regions for silica growth (interfacial region and bulk region) in which the rate of solvent evaporation and local concentration affect the speed and dimension of growth. A combined mechanism for the interfacial bulk growth of mesoporous silica under quiescent conditions is proposed. PMID:24237719

  14. Ordered mesoporous silica prepared by quiescent interfacial growth method - effects of reaction chemistry

    NASA Astrophysics Data System (ADS)

    Alsyouri, Hatem M.; Abu-Daabes, Malyuba A.; Alassali, Ayah; Lin, Jerry YS

    2013-11-01

    Acidic interfacial growth can provide a number of industrially important mesoporous silica morphologies including fibers, spheres, and other rich shapes. Studying the reaction chemistry under quiescent (no mixing) conditions is important for understanding and for the production of the desired shapes. The focus of this work is to understand the effect of a number of previously untested conditions: acid type (HCl, HNO3, and H2SO4), acid content, silica precursor type (TBOS and TEOS), and surfactant type (CTAB, Tween 20, and Tween 80) on the shape and structure of products formed under quiescent two-phase interfacial configuration. Results show that the quiescent growth is typically slow due to the absence of mixing. The whole process of product formation and pore structuring becomes limited by the slow interfacial diffusion of silica source. TBOS-CTAB-HCl was the typical combination to produce fibers with high order in the interfacial region. The use of other acids (HNO3 and H2SO4), a less hydrophobic silica source (TEOS), and/or a neutral surfactant (Tweens) facilitate diffusion and homogenous supply of silica source into the bulk phase and give spheres and gyroids with low mesoporous order. The results suggest two distinct regions for silica growth (interfacial region and bulk region) in which the rate of solvent evaporation and local concentration affect the speed and dimension of growth. A combined mechanism for the interfacial bulk growth of mesoporous silica under quiescent conditions is proposed.

  15. Facile preparation of transparent and dense CdS-silica gel glass nanocomposites for optical limiting applications

    NASA Astrophysics Data System (ADS)

    Feng, Miao; Zhan, Hongbing

    2014-03-01

    To realize their practical and operable applications as a potential optical limiting (OL) material, quantum dots (QDs) need to have good processability by incorporating them into optical-quality matrices. This work reports a facile route for the room-temperature preparation of large, stable transparent monolithic CdS nanocomposites which can be easily extended to allow the introduction of acid-sensitive functional molecules/nanoparticles into a silica network by sol-gel chemistry. Our strategy involves a two-step sol-gel process (acid-catalyst hydrolysis and basic-catalyst condensation) and the co-condensation of the resulting alkoxysilane-capped CdS QDs with other alkoxysilanes, which allows the CdS QDs to become part of the silica covalent network. The degradation and agglomeration of CdS QDs were thereby effectively restrained, and large monolithic transparent CdS-silica gel glass was obtained. Using Z-scan theory and the resulting open-aperture Z-scan curves, the nonlinear extinction coefficient of the CdS-silica nanocomposite gel glass was calculated to be 1.02 × 10-14 cm W-1, comparable to that of the parent CdS QD dispersion, indicating their promise for OL applications.

  16. Facile preparation of transparent and dense CdS-silica gel glass nanocomposites for optical limiting applications.

    PubMed

    Feng, Miao; Zhan, Hongbing

    2014-04-21

    To realize their practical and operable applications as a potential optical limiting (OL) material, quantum dots (QDs) need to have good processability by incorporating them into optical-quality matrices. This work reports a facile route for the room-temperature preparation of large, stable transparent monolithic CdS nanocomposites which can be easily extended to allow the introduction of acid-sensitive functional molecules/nanoparticles into a silica network by sol-gel chemistry. Our strategy involves a two-step sol-gel process (acid-catalyst hydrolysis and basic-catalyst condensation) and the co-condensation of the resulting alkoxysilane-capped CdS QDs with other alkoxysilanes, which allows the CdS QDs to become part of the silica covalent network. The degradation and agglomeration of CdS QDs were thereby effectively restrained, and large monolithic transparent CdS-silica gel glass was obtained. Using Z-scan theory and the resulting open-aperture Z-scan curves, the nonlinear extinction coefficient of the CdS-silica nanocomposite gel glass was calculated to be 1.02 × 10(-14) cm W(-1), comparable to that of the parent CdS QD dispersion, indicating their promise for OL applications.

  17. Preparation of Silica Nanoparticles Loaded with Nootropics and Their In Vivo Permeation through Blood-Brain Barrier

    PubMed Central

    Zaruba, Kamil; Kunes, Martin; Ulbrich, Pavel; Brezaniova, Ingrid; Triska, Jan; Suchy, Pavel

    2015-01-01

    The blood-brain barrier prevents the passage of many drugs that target the central nervous system. This paper presents the preparation and characterization of silica-based nanocarriers loaded with piracetam, pentoxifylline, and pyridoxine (drugs from the class of nootropics), which are designed to enhance the permeation of the drugs from the circulatory system through the blood-brain barrier. Their permeation was compared with non-nanoparticle drug substances (bulk materials) by means of an in vivo model of rat brain perfusion. The size and morphology of the nanoparticles were characterized by transmission electron microscopy. The content of the drug substances in silica-based nanocarriers was analysed by elemental analysis and UV spectrometry. Microscopic analysis of visualized silica nanocarriers in the perfused brain tissue was performed. The concentration of the drug substances in the tissue was determined by means of UHPLC-DAD/HRMS LTQ Orbitrap XL. It was found that the drug substances in silica-based nanocarriers permeated through the blood brain barrier to the brain tissue, whereas bulk materials were not detected in the brain. PMID:26075264

  18. Preparation of silica nanoparticles loaded with nootropics and their in vivo permeation through blood-brain barrier.

    PubMed

    Jampilek, Josef; Zaruba, Kamil; Oravec, Michal; Kunes, Martin; Babula, Petr; Ulbrich, Pavel; Brezaniova, Ingrid; Opatrilova, Radka; Triska, Jan; Suchy, Pavel

    2015-01-01

    The blood-brain barrier prevents the passage of many drugs that target the central nervous system. This paper presents the preparation and characterization of silica-based nanocarriers loaded with piracetam, pentoxifylline, and pyridoxine (drugs from the class of nootropics), which are designed to enhance the permeation of the drugs from the circulatory system through the blood-brain barrier. Their permeation was compared with non-nanoparticle drug substances (bulk materials) by means of an in vivo model of rat brain perfusion. The size and morphology of the nanoparticles were characterized by transmission electron microscopy. The content of the drug substances in silica-based nanocarriers was analysed by elemental analysis and UV spectrometry. Microscopic analysis of visualized silica nanocarriers in the perfused brain tissue was performed. The concentration of the drug substances in the tissue was determined by means of UHPLC-DAD/HRMS LTQ Orbitrap XL. It was found that the drug substances in silica-based nanocarriers permeated through the blood brain barrier to the brain tissue, whereas bulk materials were not detected in the brain.

  19. Preparation and characterization of monodisperse large-porous silica microspheres as the matrix for protein separation.

    PubMed

    Xia, Hongjun; Wan, Guangping; Zhao, Junlong; Liu, Jiawei; Bai, Quan

    2016-11-04

    High performance liquid chromatography (HPLC) is a kind of efficient separation technology and has been used widely in many fields. Micro-sized porous silica microspheres as the most popular matrix have been used for fast separation and analysis in HPLC. In this paper, the monodisperse large-porous silica microspheres with controllable size and structure were successfully synthesized with polymer microspheres as the templates and characterized. First, the poly(glycidyl methacrylate-co-ethyleneglycol dimethacrylate) microspheres (PGMA-EDMA) were functionalized with tetraethylenepentamine (TEPA) to generate amino groups which act as a catalyst in hydrolysis of tetraethyl orthosilicate (TEOS) to form Si-containing low molecular weight species. Then the low molecular weight species diffused into the functionalized PGMA-EDMA microspheres by induction force of the amino groups to form polymer/silica hybrid microspheres. Finally, the organic polymer templates were removed by calcination, and the large-porous silica microspheres were obtained. The compositions, morphology, size distribution, specific surface area and pore size distribution of the porous silica microspheres were characterized by infrared analyzer, scanning-electron microscopy, dynamic laser scattering, the mercury intrusion method and thermal gravimetric analysis, respectively. The results show that the agglomeration of the hybrid microspheres can be overcome when the templates were functionalized with TEPA as amination reagent, and the yield of 95.7% of the monodisperse large-porous silica microspheres can be achieved with high concentration of polymer templates. The resulting large-porous silica microspheres were modified with octadecyltrichlorosilane (ODS) and the chromatographic evaluation was performed by separating the proteins and the digest of BSA. The baseline separation of seven kinds of protein standards was achieved, and the column delivered a better performance when separating BSA digests

  20. Silica-based nanocomposites via reverse microemulsions: classifications, preparations, and applications

    NASA Astrophysics Data System (ADS)

    Wang, Jiasheng; Shah, Zameer Hussain; Zhang, Shufen; Lu, Rongwen

    2014-04-01

    Silica-based nanocomposites with amorphous silica as the matrix or carrier along with a functional component have been extensively investigated. These nanocomposites combine the advantages of both silica and the functional components, demonstrating great potential for various applications. To synthesize such composites, one of the most frequently used methods is reverse microemulsion due to its convenient control over the size, shape, and structures. The structures of the composites have a decisive significance for their properties and applications. In this review, we tried to categorize the silica-based nanocomposites via reverse microemulsions based on their structures, discussed the syntheses individually for each structure, summarized their applications, and made some perspectives based on the current progress of this field.Silica-based nanocomposites with amorphous silica as the matrix or carrier along with a functional component have been extensively investigated. These nanocomposites combine the advantages of both silica and the functional components, demonstrating great potential for various applications. To synthesize such composites, one of the most frequently used methods is reverse microemulsion due to its convenient control over the size, shape, and structures. The structures of the composites have a decisive significance for their properties and applications. In this review, we tried to categorize the silica-based nanocomposites via reverse microemulsions based on their structures, discussed the syntheses individually for each structure, summarized their applications, and made some perspectives based on the current progress of this field. Electronic supplementary information (ESI) available: The structures of all the surfactants included in this review are listed. See DOI: 10.1039/c3nr06025j

  1. Zeolite materials prepared using silicate waste from template synthesis of ordered mesoporous carbon.

    PubMed

    Kim, Yun Kyung; Rajesh, Kizhakke Palleeri; Yu, Jong-Sung

    2013-09-15

    Significant amount of silica waste is generated in the preparation of porous carbon materials using template synthesis. Industrial production of such porous carbon not only creates waste chemicals, but also poses significant environmental concerns and high waste treatment cost. Recycling is proposed as the best solution for tackling such chemical wastes. In this study, etched silica waste released from template synthesis of mesoporous carbon is recycled to produce precious functional microporous zeolite materials. The solid silica template is etched out with NaOH solution to produce silica-free mesoporous carbon. The collected silica waste is recycled to generate zeolites such as LTA and MFI type silica materials. The formation of zeolites is confirmed by FT-IR, XRD, (29)Si NMR, (27)Al NMR, and SEM. This straight forward green chemistry route not only recycles the waste chemicals, but also decreases environmental pollution for better improvement of our living.

  2. Effect of Sintering Temperature on the Properties of Fused Silica Ceramics Prepared by Gelcasting

    NASA Astrophysics Data System (ADS)

    Wan, Wei; Huang, Chun-e.; Yang, Jian; Zeng, Jinzhen; Qiu, Tai

    2014-07-01

    Fused silica ceramics were fabricated by gelcasting, by use of a low-toxicity N' N-dimethylacrylamide gel system, and had excellent properties compared with those obtained by use of the low-toxicity 2-hydroxyethyl methacrylate and toxic acrylamide systems. The effect of sintering temperature on the microstructure, mechanical and dielectric properties, and thermal shock resistance of the fused silica ceramics was investigated. The results showed that sintering temperature has a critical effect. Use of an appropriate sintering temperature will promote densification and improve the strength, thermal shock resistance, and dielectric properties of fused silica ceramics. However, excessively high sintering temperature will greatly facilitate crystallization of amorphous silica and result in more cristobalite in the sample, which will cause deterioration of these properties. Fused silica ceramics sintered at 1275°C have the maximum flexural strength, as high as 81.32 MPa, but, simultaneously, a high coefficient of linear expansion (2.56 × 10-6/K at 800°C) and dramatically reduced residual flexural strength after thermal shock (600°C). Fused silica ceramics sintered at 1250°C have excellent properties, relatively high and similar flexural strength before (67.43 MPa) and after thermal shock (65.45 MPa), a dielectric constant of 3.34, and the lowest dielectric loss of 1.20 × 10-3 (at 1 MHz).

  3. The situ preparation of silica nanoparticles on the surface of functionalized graphene nanoplatelets

    NASA Astrophysics Data System (ADS)

    Li, Jiani; Yu, Kejing; Qian, Kun; Cao, Haijian; Lu, Xuefeng; Sun, Jie

    2014-04-01

    A method for situ preparing a hybrid material consisting of silica nanoparticles (SiO2) attached onto the surface of functionalized graphene nanoplatelets (f-GNPs) is proposed. Firstly, polyacrylic acid (PAA) was grafted to the surface of f-GNPs to increase reacting sites, and then 3-aminopropyltriethoxysilane (APTES) KH550 reacted with abovementioned product PAA-GNPs to obtain siloxane-GNPs, thus providing reaction sites for the growth of SiO2 on the surface of GNPs. Finally, the SiO2/graphene nanoplatelets (SiO2/GNPs) hybrid material is obtained through introducing siloxane-GNPs into a solution of tetraethyl orthosilicate, ammonia and ethanol for hours' reaction. The results from Fourier transform infrared spectroscopy (FTIR) showed that SiO2 particles have situ grown on the surface of GNPs through chemical bonds as Si-O-Si. And the nanostructure of hybrid materials was characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). All the images indicated that SiO2 particles with similar sizes were grafted on the surface of graphene nanoplatelets successfully. And TEM images also showed the whole growth process of SiO2 particles on the surface of graphene as time grows. Moreover, TGA traces suggested the SiO2/GNPs hybrid material had stable thermal stability. And at 900°C, the residual weight fraction of polymer on siloxane-GNPs was about 94.2% and that of SiO2 particles on hybrid materials was about 75.0%. However, the result of Raman spectroscopy showed that carbon atoms of graphene nanoplatelets became much more disordered, due to the destroyed carbon domains during the process of chemical drafting. Through orthogonal experiments, hybrid materials with various sizes of SiO2 particles were prepared, thus achieving the particle sizes controllable. And the factors' level of significance is as follows: the quantity of ammonia > the quantity of tetraethyl orthosilicate (TEOS) > the reaction time.

  4. In-column preparation of a brush-type chiral stationary phase using click chemistry and a silica monolith

    PubMed Central

    Slater, Michael D.; Fréchet, Jean M.J.; Svec, Frantisek

    2009-01-01

    Brush-type chiral stationary phases have been prepared both from a silica monolith and, separately, from 10 μm porous silica beads via a process of in-column modification including attachment of the chiral selector via copper catalyzed azide-alkyne cycloaddition. Azide functionalities were first introduced on the pore surface of each type of support by reaction with 3-(azidopropyl)trimethoxysilane, followed by immobilization of a proline-derived chiral selector containing an alkyne moiety. This functionalization reaction was carried out in dimethylformamide in the presence of catalytic amounts of copper(I) iodide. The separation performance of these triazole linked stationary phases was demonstrated in enantioseparations of four model analytes, which afforded separation factors as high as 11.4. PMID:19051194

  5. New opportunities in the preparation of nanocomposites for biomedical applications: revised mechanosynthesis of magnetite–silica nanocomposites

    NASA Astrophysics Data System (ADS)

    Scano, Alessandra; Cabras, Valentina; Marongiu, Francesca; Peddis, Davide; Pilloni, Martina; Ennas, Guido

    2017-02-01

    Environmentally friendly preparation of functionalized magnetite-silica (Fe3O4/SiO2) nanocomposites (NCs) with different SiO2 content (6, 20 and 50 wt%) using revised mechanosynthesis is reported. High-energy ball milling of α-Fe2O3, Si and SiO2 mixtures was followed by hydrolysis and condensation of 3-aminopropyl-triethoxysilane. X-ray powder diffraction and transmission electron microscopy showed the formation of almost spherical Fe3O4 nanocrystals with a narrow size distribution (4–6 nm) uniformly dispersed in the amorphous 100–200 nm SiO2 agglomerates. Scanning electron microscopy and energy dispersive spectroscopy were used to study the elemental distribution in the sample. Fourier transform infrared spectroscopy confirmed the NC surface functionalization with amino groups. Magnetic properties were also explored, indicating a homogeneous distribution of magnetic nanoparticles in the silica matrix.

  6. Thermo-optic characterization of neodymium/nickel doped silica glasses prepared via sol-gel route.

    PubMed

    Manuel, Ancy; Kumar, B Rajesh; Basheer, N Shemeena; Kumari, B Syamala; Paulose, P I; Kurian, Achamma; George, Sajan D

    2012-12-01

    Intrinsic as well as rare earth (Neodymium) doped silica glasses with various molar ratio of dopant and a metallic (Nickel) co-dopant is prepared via sol-gel route. The structural characterization of the sample is carried out using X-ray diffraction and Fourier Transform Infrared Spectroscopy. The influence of dopant and doping concentration on the optical properties of silica matrix is investigated via UV-VIS absorption spectroscopy. Effect of dopant on thermal effusivity value of the host matrix is carried out by laser induced open cell photoacoustic technique. Analysis of the results showed that doping affect the thermal effusivity value and results are interpreted in terms of structural modification of the lattice and phonon assisted heat transport mechanism.

  7. Preparation and characterization of a BisGMA-resin dental restorative composites with glass, silica and titania fillers.

    PubMed

    Thorat, Sanjay; Patra, Niranjan; Ruffilli, Roberta; Diaspro, Alberto; Salerno, Marco

    2012-01-01

    A photo-polymerizable Bisphenol-A diglycidylether methacrylate resin was characterized by Fourier transform infrared spectroscopy after its irradiation under different conditions to identify the best curing. Bonding-agent free composites with particles of ball-milled glass, silica and titania at loading of 10 and 50%wt were prepared, and their viscoelastic properties investigated by dynamic mechanical analysis, in experimental conditions close to the working environment in the mouth. All composites showed good stability at the considered conditions. The stiffest composite was the silica one, which was based on the smallest primary particles. The storage moduli close to room temperature (25°C) and mastication frequency (1 Hz) were extracted as reference bending moduli for the materials, and compared to static compressive moduli measured by nanoindentation performed by atomic force microscopy.Nanoindentation showed qualitative results in agreement with dynamic mechanical analysis as to the ranking of different materials, while resulting in approximately two-fold elastic modulus.

  8. Mesoporous Silica Films with Long-Range Order Prepared from Strongly Segregated Block Copolymer/Homopolymer Blend Templates

    SciTech Connect

    Tirumala, Vijay R.; Pai, Rajaram A.; Agarwal, Sumit; Testa, Jason J.; Bhatnagar, Gaurav; Romang, Alvin H.; Chandler, Curran; Gorman, Brian P.; Jones, Ronald L.; Lin, Eric K.; Watkins, James J.

    2008-06-30

    Well-ordered mesoporous silica films were prepared by infusion and selective condensation of Si alkoxides within preorganized block copolymer/homopolymer blend templates using supercritical CO{sub 2} as the delivery medium. The morphologies of the mesoporous silica films reflect significant improvements in the strength of segregation and long-range order of template blends of poly(ethylene oxide-b-propylene oxide-b-ethylene oxide) triblock copolymers with selectively associating homopolymers such as poly(acrylic acid) or poly(4-hydroxystyrene) prior as compared to templates comprised of the neat copolymer. Control over film porosity, pore ordering, and morphology of the films is achieved through simple variations in the homopolymer concentration. The films were characterized using X-ray reflectivity, small-angle X-ray scattering, and transmission electron microscopy.

  9. Preparation of silane-functionalized silica films via two-step dip coating sol-gel and evaluation of their superhydrophobic properties

    NASA Astrophysics Data System (ADS)

    Ramezani, Maedeh; Vaezi, Mohammad Reza; Kazemzadeh, Asghar

    2014-10-01

    In this paper, we study the two-step dip coating via a sol-gel process to prepare superhydrophobic silica films on the glass substrate. The water repellency of the silica films was controlled by surface silylation method using isooctyltrimethoxysilane (iso-OTMS) as a surface modifying agent. Silica alcosol was synthesized by keeping the molar ratio of ethyltriethoxysilane (ETES) precursor, ethanol (EtOH) solvent, water (H2O) was kept constant at 1:36:6.6 respectively, with 6 M NH4OH throughout the experiment and the percentages of hydrophobic agent in hexane bath was varied from 0 to 15 vol.%. The static water contact angle values of the silica films increased from 108° to 160° with an increase in the vol.% of iso-OTMS. At 15 vol%. of iso-OTMS, the silica film shows static water contact angle as high as 160°. The superhydrophobic silica films are thermally stable up to 440 °C and above this temperature, the silica films lose superhydrophobicity. By controlling the primer particle size of SiO2 about 26 nm, leading to decrease the final size of silica nanoparticles after modification of nanoparticles by isooctyltrimethoxysilane about 42 nm. The films are transparent and have uniform size on the surface. The silica films have been characterized by atomic force microscopy (AFM), fourier transform infrared spectroscopy (FT-IR), transparency, contact angle measurement (CA), Zeta-potential, Thermal stability by TG-DTA analysis.

  10. Mesoporous silica/polyacrylamide composite: Preparation by UV-graft photopolymerization, characterization and use as Hg(II) adsorbent

    NASA Astrophysics Data System (ADS)

    Saad, Ali; Bakas, Idriss; Piquemal, Jean-Yves; Nowak, Sophie; Abderrabba, Manef; Chehimi, Mohamed M.

    2016-03-01

    MCM-41 ordered mesoporous silica was prepared, aminosilanized and grafted with polyacrylamide (PAAM) through in situ radical photopolymerization process. The resulting composite, denoted PAAM-NH2-MCM-41, the calcined and silanized reference MCM-41s were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and N2 physisorption at 77 K. These complementary techniques brought strong supporting evidence for the silanization process followed by PAAM grafting. The surface composition was found to be PAAM-rich as judged by XPS. The composite was then employed for the uptake of Hg(II) from aqueous solutions. Adsorption was monitored versus pH, time, and temperature. The maximum adsorption capacity at 25 °C and pH 5.2 was 177 mg g-1. Kinetically, the equilibrium was reached within 60 min for a 100 mg L-1 mercury solution. The adsorption of Hg(II) on PAAM-NH2-MCM-41 composites followed second order kinetics. Thermodynamic parameters suggested that the favorable adsorption process is exothermic in nature and the adsorption is ascribed to a decrease in the degree of freedom of adsorbed ions which results in the entropy change. This work conclusively shows that mesoporous silica-polymer hybrid metal ion adsorbents (with robust silica-polymer interface) can be prepared in a simple way by in situ radical photopolymerization in the presence of aminosilanized silica acting as a support and a macro-hydrogen donor simultaneously.

  11. Preparation of a mercaptopropyl bonded silica intermediate in supercritical carbon dioxide: synthesis, characterisation and chromatography of a quinine based chiral stationary phase.

    PubMed

    Scully, Norma M; O'Sullivan, Gerard P; Healy, Liam O; Glennon, Jeremy D; Dietrich, Benjamin; Albert, Klaus

    2007-07-13

    This research examines the preparation of a mercaptopropyl bonded silica intermediate in supercritical carbon dioxide (sc-CO(2)) and the subsequent conversion in sc-CO(2) to a quinine derived chiral stationary phase (CSP). The effects of reaction temperature, pressure and time on the surface coverage of the silica intermediate were investigated when porous silica particles (Exsil-Avanti, 3microm) were reacted with 3-trimethoxymercaptopropylsilane in sc-CO(2). We present results which demonstrate that a stable mercaptopropyl bonded silica intermediate can be successfully prepared under supercritical conditions of 40 degrees C, 483bar, in a substantially reduced reaction time of 1h with superior surface coverages compared to organic solvent based methods. The further utility of this supercritical fluid technology was demonstrated by the free radical addition of a quinine derived chiral selector onto a mercaptopropyl bonded silica intermediate in sc-CO(2). This supercritical fluid generated chiral stationary phase (CSP) was utilised for the direct LC enantioseparation of a series of 3,5-dinitrobenzoyl (DNB) amino acids. Bonded silica samples were characterised using elemental analysis, diffuse reflectance infrared fourier transform (DRIFT) spectroscopy, solid state (13)C and (29)Si CP-MAS NMR spectroscopy, and thermogravimetric analysis (TGA). This supercritical fluid functionalisation approach offers an efficient and cleaner alternative to existing organic solvent based approaches for the preparation of bonded silica phases.

  12. Core-shell-structured silica/polyacrylate particles prepared by Pickering emulsion: influence of the nucleation model on particle interfacial organization and emulsion stability.

    PubMed

    Ji, Jing; Shu, Shi; Wang, Feng; Li, Zhilin; Liu, Jingjun; Song, Ye; Jia, Yi

    2014-01-01

    This work reports a new evidence of the versatility of silica sol as a stabilizer for Pickering emulsions. The organization of silica particles at the oil-water interface is a function of the nucleation model. The present results show that nucleation model, together with monomer hydrophobicity, can be used as a trigger to modify the packing density of silica particles at the oil-water interface: Less hydrophobic methylmethacrylate, more wettable with silica particles, favors the formation of core-shell-structured composite when the composite particles are prepared by miniemulsion polymerization in which monomers are fed in batch (droplet nucleation). By contrast, hydrophobic butylacrylate promotes the encapsulating efficiency of silica when monomers are fed dropwise (homogeneous nucleation). The morphologies of polyacrylate-nano-SiO2 composites prepared from different feed ratio of methylmethacrylate/butylacrylate (with different hydrophobicity) and by different feed processes are characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM) techniques. The results from SEM and TEM show that the morphologies of the as-prepared polyacrylate/nano-SiO2 composite can be a core-shell structure or a bare acrylic sphere. The stability of resulting emulsions composed of these composite particles is strongly dependent on the surface coverage of silica particles. The emulsion stability is improved by densely silica-packed composite particles.

  13. Preparation of bi-functional silica particles for antibacterial and self cleaning surfaces.

    PubMed

    Hebalkar, Neha Y; Acharya, Snigdhatanu; Rao, Tata N

    2011-12-01

    Synthesis of bi-functional silica particles by a simple wet chemical method is described where the mixture of ultra fine nanoparticles (1-3 nm) of titania and silver were attached on the silica particle surface in a controlled way to form a core-shell structure. The silica surface showed efficient bi-functional activity of photo-catalytically self cleaning and antibacterial activity due to nanotitania and nanosilver mutually benefiting each other's function. The optimum silver concentration was found where extremely small silver nanoparticles are formed and the total composite particle remains white in color. This is an important property in view of certain applications such as antibacterial textiles where the original fabric color has to be retained even after applying the nanosilver on it. The particles were characterized at each step of the synthesis by X-ray photoelectron spectroscopy, UV-visible spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy and electron energy loss spectroscopy. Bi-functional silica particles showed accelerated photocatalytic degradation of methylene blue as well as enhanced antibacterial property when tested as such particles and textiles coated with these bi-functional silica particles even at lower silver concentration.

  14. Facile preparation of silver nanoparticles homogeneously immobilized in hierarchically monolithic silica using ethylene glycol as reductant.

    PubMed

    Yu, Huan; Zhu, Yang; Yang, Hui; Nakanishi, Kazuki; Kanamori, Kazuyoshi; Guo, Xingzhong

    2014-09-07

    A facile and "green" method was proposed to introduce Ag nanoparticles (Ag NPs) into the hierarchically monolithic silica uniformly in the presence of (3-aminopropyl)-triethoxysilane (APTES) and ethylene glycol. APTES is used to modify the monolith by incorporating amino groups onto the surface of meso-macroporous skeletons, while ethylene glycol is employed as the productive reductant. Ag NPs are homogeneously immobilized in hierarchically monolithic silica after reduction and drying at 40 °C for different duration times, and the embedded amount of Ag NPs can reach 15.44 wt% when treated once. The embedment of Ag NPs increases with the repeat treatment and the APTES amount, without uncontrollable crystalline growth. The surface areas of Ag NPs embedded in silica monoliths after heat treatment at 300 and 400 °C are higher than those before heat treatment. The modification via APTES and the embedment of Ag NPs does not spoil the morphology of monolithic silica, while changing the pore structures of the monolith. A tentative formation process and a reduction mechanism are proposed for the modification, reduction and embedment. Ag NPs embedded in monolithic silica is promising for wide applications such as catalysis and separation.

  15. Synthesis and adsorption properties of chitosan-silica nanocomposite prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Budnyak, Tetyana M.; Pylypchuk, Ievgen V.; Tertykh, Valentin A.; Yanovska, Elina S.; Kolodynska, Dorota

    2015-02-01

    A hybrid nanocomposite material has been obtained by in situ formation of an inorganic network in the presence of a preformed organic polymer. Chitosan biopolymer and tetraethoxysilane (TEOS), which is the most common silica precursor, were used for the sol-gel reaction. The obtained composite chitosan-silica material has been characterized by physicochemical methods such as differential thermal analyses (DTA); carbon, hydrogen, and nitrogen (CHN) elemental analysis; nitrogen adsorption/desorption isotherms, scanning electron microscopy (SEM); and Fourier transform infrared (FTIR) spectroscopy to determine possible interactions between silica and chitosan macromolecules. Adsorption of microquantities of V(V), Mo(VI), and Cr(VI) oxoanions from the aqueous solutions by the obtained composite has been studied in comparison with the chitosan beads, previously crosslinked with glutaraldehyde. The adsorption capacity and kinetic sorption characteristics of the composite material were estimated.

  16. A sustainable route for the preparation of activated carbon and silica from rice husk ash.

    PubMed

    Liu, Yan; Guo, Yupeng; Zhu, Yanchao; An, Dongmin; Gao, Wei; Wang, Zhuo; Ma, Yuejia; Wang, Zichen

    2011-02-28

    An environmentally friendly and economically effective process to produce silica and activated carbon form rice husk ask simultaneously has been developed in this study. An extraction yield of silica of 72-98% was obtained and the particle size was 40-50 nm. The microstructures of the as-obtained silica powders were characterized by X-ray diffraction (XRD) and infrared spectra (IR). The surface area, iodine number and capacitance value of activated carbon could achieve 570 m(2)/g, 1708 mg/g, 180 F/g, respectively. In the whole synthetic procedure, the wastewater and the carbon dioxide were collected and reutilized. The recovery rate of sodium carbonate was achieved 92.25%. The process is inexpensive, sustainable, environmentally friendly and suitable for large-scale production.

  17. Preparation of efficient quercetin delivery system on Zn-modified mesoporous SBA-15 silica carrier.

    PubMed

    Trendafilova, Ivalina; Szegedi, Agnes; Mihály, Judith; Momekov, Georgi; Lihareva, Nadejda; Popova, Margarita

    2017-04-01

    Mesoporous silica material type SBA-15 was modified with different amounts of Zn (2 and 4wt.%) by incipient wetness impregnation method in ethanol. The parent, Zn-modified and quercetin loaded samples, were characterized by XRD, N2 physisorption, TEM, thermal gravimetric analysis, UV-vis and FT-IR spectroscopies and in vitro release of quercetin at pH5.5 which is typical of dermal formulations. By this loading method anhydrous quercetin was formed on the silica carrier It was found that the different hydrate forms of quercetin (dihydrate, monohydrate, anhydrite) significantly influence the physico-chemical properties of the delivery system. It was found that hydrate forms of quercetin can be differentiated by XRD and by FT-IR spectroscopic methods. Thus, by evaluating the interaction of the drug with the silica carrier the changes due to its hydration state always have to be taken into account. Formation of Zn-quercetin complex was evidenced on zinc modified SBA-15 silica by FT-IR spectroscopy. High quercetin loading capacity (over 40wt.%) could be achieved on the parent and Zn-containing SBA-15 samples. The in-vitro release process at pH=5.5 showed slower quercetin release from Zn-modified SBA-15 samples compared to the parent one. Additionally, the comparative cytotoxic experiments evidenced that quercetin encapsulated in Zn-modified silica carriers has superior antineoplastic potential against HUT-29 cells compared to free drug. Zn-modified SBA-15 silica particles could be promising carriers for dermal delivery of quercetin.

  18. Particle-filled microporous materials

    DOEpatents

    McAllister, Jerome W.; Kinzer, Kevin E.; Mrozinski, James S.; Johnson, Eric J.

    1992-07-14

    A microporous particulate-filled thermoplastic polymeric article is provided. The article can be in the form of a film, a fiber, or a tube. The article has a thermoplastic polymeric structure having a plurality of interconnected passageways to provide a network of communicating pores. The microporous structure contains discrete submicron or low micron-sized particulate filler, the particulate filler being substantially non-agglomerated.

  19. Particle-filled microporous materials

    DOEpatents

    McAllister, Jerome W.; Kinzer, Kevin E.; Mrozinski, James S.; Johnson, Eric J.; Dyrud, James F.

    1990-01-01

    A microporous particulate-filled thermoplastic polymeric article is provided. The article can be in the form of a film, a fiber, or a tube. The article has a thermoplastic polymeric structure having a plurality of interconnected passageways to provide a network of communicating pores. The microporous structure contains discrete submicron or low micron-sized particulate filler, the particulate filler being substantially non-agglomerated.

  20. Particle-filled microporous materials

    DOEpatents

    McAllister, J.W.; Kinzer, K.E.; Mrozinski, J.S.; Johnson, E.J.; Dyrud, J.F.

    1990-09-18

    A microporous particulate-filled thermoplastic polymeric article is provided. The article can be in the form of a film, a fiber, or a tube. The article has a thermoplastic polymeric structure having a plurality of interconnected passageways to provide a network of communicating pores. The microporous structure contains discrete submicron or low micron-sized particulate filler, the particulate filler being substantially non-agglomerated. 3 figs.

  1. Preparation of Mesoporous Silica Templated Metal Nanowire Films on Foamed Nickel Substrates

    SciTech Connect

    Campbell, Roger; Kenik, Edward A; Bakker, Martin; Havrilla, George; Montoya, Velma; Shamsuzzoha, Mohammed

    2006-01-01

    A method has been developed for the formation of high surface area nanowire films on planar and three-dimensional metal electrodes. These nanowire films are formed via electrodeposition into a mesoporous silica film. The mesoporous silica films are formed by a sol-gel process using Pluronic tri-block copolymers to template mesopore formation on both planar and three-dimensional metal electrodes. Surface area increases of up to 120-fold have been observed in electrodes containing a templated film when compared to the same types of electrodes without the templated film.

  2. On-machine precision preparation and dressing of ball-headed diamond wheel for the grinding of fused silica

    NASA Astrophysics Data System (ADS)

    Chen, Mingjun; Li, Ziang; Yu, Bo; Peng, Hui; Fang, Zhen

    2013-09-01

    In the grinding of high quality fused silica parts with complex surface or structure using ball-headed metal bonded diamond wheel with small diameter, the existing dressing methods are not suitable to dress the ball-headed diamond wheel precisely due to that they are either on-line in process dressing which may causes collision problem or without consideration for the effects of the tool setting error and electrode wear. An on-machine precision preparation and dressing method is proposed for ball-headed diamond wheel based on electrical discharge machining. By using this method the cylindrical diamond wheel with small diameter is manufactured to hemispherical-headed form. The obtained ball-headed diamond wheel is dressed after several grinding passes to recover geometrical accuracy and sharpness which is lost due to the wheel wear. A tool setting method based on high precision optical system is presented to reduce the wheel center setting error and dimension error. The effect of electrode tool wear is investigated by electrical dressing experiments, and the electrode tool wear compensation model is established based on the experimental results which show that the value of wear ratio coefficient K' tends to be constant with the increasing of the feed length of electrode and the mean value of K' is 0.156. Grinding experiments of fused silica are carried out on a test bench to evaluate the performance of the preparation and dressing method. The experimental results show that the surface roughness of the finished workpiece is 0.03 μm. The effect of the grinding parameter and dressing frequency on the surface roughness is investigated based on the measurement results of the surface roughness. This research provides an on-machine preparation and dressing method for ball-headed metal bonded diamond wheel used in the grinding of fused silica, which provides a solution to the tool setting method and the effect of electrode tool wear.

  3. Preparation and In-vitro Evaluation of Rifampin-loaded Mesoporous Silica Nanoaggregates by an Experimental Design

    PubMed Central

    Mohseni, Meysam; Gilani, Kambiz; Bahrami, Zohreh; Bolourchian, Noushin; Mortazavi, Seyed Alireza

    2015-01-01

    The goal of this research is preparation, optimization and in-vitro evaluation of rifampin-loaded silica nanoparticles in order to use in the pulmonary drug delivery. Nanoparticles are exhaled because of their small size. Preparation of nanoaggregates in a micron-size scale and re-dispersion of them after deposition in the lung is an approach to overcome this problem. We used this approach in our research. Rifampin was selected as a model lipophilic molecule since it was a well-documented and much used anti tuberculosis drug. A half factorial design was used to identify significant parameters of the spray drying process. The results showed that feed concentration, feed pH and the interaction between feed flow rate and gas atomizer flow rate had statistically significant effects on the particle size of nanoaggregates. The Box-Behnken design was employed to optimize the spray drying process. Finally, a quadratic equation which explains the relation between independent variables and aerodynamic diameter of nanoaggregates was obtained. Rifampin-loaded silica nanoaggregates underwent different in-vitro tests including: SEM, Aerosol performance and drug release. The in-vitro drug release was investigated with buffer phosphate (pH=7.4). Regarding the drug release study, a triphasic pattern of release was observed. The rifampin-loaded silica nanoaggregates were capable of releasing 90% drug content after 24 h in combination patterns of release. The prepared rifampin-loaded nanoaggregates seem to have a potential to be used in a pulmonary drug delivery. PMID:25901143

  4. Preparation and retention mechanism exploration of mesostructured cellular foam silica as stationary phase for high performance liquid chromatography.

    PubMed

    Sun, Shaoai; Zhang, Xiaoqiong; Han, Qiang; Wan, Wei; Ding, Mingyu

    2016-01-01

    Siliceous mesostructured cellular foam (MCF) with highly interconnected porous structure, ultralarge pore size and relatively uniform particle size (3-5μm) was prepared to achieve the mixed-mode and efficient separation of intact proteins. And molecular sieving effect for the first time played an important role in protein separation using mesoporous silica materials as HPLC stationary phase. The spherical silica particles were synthesized via hydrothermal method and the pore size was easily regulated by adding NH4F as well as altering the aging time. After aminopropyl derivatization, the chromatographic performance of functionalized mesoporous silica particles was investigated in comparison with those without modification and commercial NH2 column, and their mixed-mode retention mechanisms were investigated in detail. The superior separation performance for the retention of proteins was obtained on our home-made column in comparison with commercial NH2 column. The influences of aminopropyl derivatization and mobile phase composition on the column property were also investigated. Moreover, the home-made column showed similar performance for separation of polar anilines and neutral PAHs with the commercial column, owing to mixed-mode retention mechanisms including p-π stacking, electron interaction, hydrophobic effect, π-π EDA interaction and hydrogen bonding. All these results indicated that the aminopropyl modified MCF would be promising in the mixed-mode and efficient separation of biomolecules in addition with small molecules.

  5. A study on the consecutive preparation of d-xylose and pure superfine silica from rice husk.

    PubMed

    Zhang, Hongxi; Zhao, Xu; Ding, Xuefeng; Lei, Hong; Chen, Xue; An, Dongmin; Li, Yunling; Wang, Zichen

    2010-02-01

    Rice husk is an abundant agricultural byproduct. In the present paper, research on consecutive preparation of d-xylose and superfine silica from rice husk is carried out. The optimum hydrolysis conditions of xylan in rice husk to d-xylose are as follows: the concentration of H(2)SO(4) is 4% (wt.%), the temperature is 130 degrees C, the ratio of rice husk mass (g) to H(2)SO(4) solution volume (ml) is 1:4 and the time is 2 h. The hydrolysis degree of xylan reaches 96.22% (wt.%). High purity (98.5%, wt.%) d-xylose is obtained from acid hydrolysis solution with the purification yield of 71.63% (wt.%). At the same time, the metal oxides in rice husk are efficiently dissolved by H(2)SO(4). Residuals from H(2)SO(4) pre-treatment are incinerated under 750 degrees C in stationary air for 15 min. Silica is obtained with the purity of 99.87% (wt.%). The superfine silica powder is obtained after ground and ultrasonic dispersion, with the diameter of 30-200 nm and specific surface 287.86 m(2)/g.

  6. Microwave-induced degradation of atrazine sorbed in mineral micropores.

    PubMed

    Hu, Erdan; Cheng, Hefa; Hu, Yuanan

    2012-05-01

    The herbicide atrazine is a common pollutant in reservoirs and other sources of drinking water worldwide. The adsorption of atrazine from water onto zeolites CBV-720 and 4A, mesoporous silica MCM-41, quartz sand, and diatomite, and its microwave-induced degradation when sorbed on these minerals, were studied. Dealuminated HY zeolite CBV-720 exhibited the highest atrazine sorption capacity among the mineral sorbents because of its high micropore volume, suitable pore sizes, and surface hydrophobicity. Atrazine sorbed on the minerals degraded under microwave irradiation due to interfacial selective heating by the microwave, while atrazine in aqueous solution and associated with PTFE powder was not affected. Atrazine degraded rapidly in the micropores of CBV-720 under microwave irradiation and its degradation intermediates also decomposed with further irradiation, suggesting atrazine could be fully mineralized. Two new degradation intermediates of atrazine, 3,5-diamino-1,2,4-triazole and guanidine, were first identified in this study. The evolution of degradation intermediates and changes in infrared spectra of CBV-720 after microwave irradiation consistently indicate the creation of microscale hot spots in the micropores and the degradation of atrazine following a pyrolysis mechanism. These results indicate that microporous mineral sorption coupled with microwave-induced degradation could serve as an efficient treatment technology for removing atrazine from drinking water.

  7. Preparation, characterization and application in deep catalytic ODS of the mesoporous silica pillared clay incorporated with phosphotungstic acid.

    PubMed

    Li, Baoshan; Liu, Zhenxing; Liu, Jianjun; Zhou, Zhiyuan; Gao, Xiaohui; Pang, Xinmei; Sheng, Huiting

    2011-10-15

    Mesoporous silica pillared clay (SPC) materials with different contents of H(3)PW(12)O(40) (HPW) heteropoly acid were synthesized by introducing HPW into clay interlayer template in an acidic suspension using sol-gel method. Samples with similar HPW loadings were also prepared by impregnation method using SPC as the support. The results of the characterizations showed that HPW was dispersed more homogeneously in the encapsulated samples than in the impregnated samples. The encapsulated materials exhibited better catalytic performance than the impregnated samples in oxidative desulfurization of dibenzothiophene-containing model oil. The sulfur removal reached up to 98.6% for the model oil under the experiential conditions.

  8. Preparation and optical properties of silica Ag-Cu alloy core-shell composite colloids

    SciTech Connect

    Zhang Jianhui Liu Huaiyong; Wang Zhenlin; Ming Naiben

    2007-04-15

    The silica Ag-Cu alloy core-shell composite colloids have been successfully synthesized by an electroless plating approach to explore the possibility of modifying the plasmon resonance at the nanoshell surface by varying the metal nanoshell composition for the first time. The surface plasmon resonance of the composite colloids increases in intensity and shifts towards longer, then shorter wavelengths as the Cu/Ag ratio in the alloy shell is increased. The variations in intensity of the surface plasmon resonance with the Cu/Ag ratio obviously affect the Raman bands of the silica colloid core. The report here may supply a new technique to effectively modify the surface plasmon resonance. - Graphical abstract: The silica Ag-Cu alloy core-shell colloids have been successfully synthesized to explore the possibility of modifying the surface plasmon resonance (SPR) by varying the metal nanoshell composition for the first time. Varying the Cu/Ag ratio of the alloy nanoshell has obvious influences on the SPR of the composite colloids and the Raman bands of the amorphous silica core.

  9. Development of novel biocompatible hybrid nanocomposites based on polyurethane-silica prepared by sol gel process.

    PubMed

    Rashti, Ali; Yahyaei, Hossein; Firoozi, Saman; Ramezani, Sara; Rahiminejad, Ali; Karimi, Roya; Farzaneh, Khadijeh; Mohseni, Mohsen; Ghanbari, Hossein

    2016-12-01

    Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants.

  10. Dry plant extracts loaded on fumed silica for direct compression: preparation and preformulation.

    PubMed

    Palma, S D; Manzo, R H; Allemandi, D A

    1999-01-01

    This paper describes the development of a method to load fumed silica with vegetal material (solid residue) from a liquid extract to obtain a solid loaded silica product (LSP) with satisfactory flow properties and compressibility to be processed by direct-compression technology. Extracts of Melissa officinalis L. (M.o.), Cardus marianus L. (C.m.), and Peumus boldus L. (P.b.) were used to load silica support. The release of boldine from LSP (P.b.) reached 100% in HCl 0.1 N solution and only approximately 70% in water. Some physical-mechanical properties of LSP (M.o. and C.m.) alone and LSP-excipient mixtures were determined. The densities (bulk and tap) of LSP were higher than those of fumed silica alone. Consequently, good flow properties of LSP products were observed. On the other hand, flowability, densities, and compactibility of directly compressible excipients (lactose, dicalcium phosphate dihydrate, and microcrystalline cellulose) were not adversely affected when mixed with LSP.

  11. Preparation of Self-Activated Fluorescence Mesoporous Silica Hollow Nanoellipsoids for Theranostics.

    PubMed

    Singh, Rajendra Kumar; Kim, Tae-Hyun; Mahapatra, Chinmaya; Patel, Kapil Dev; Kim, Hae-Won

    2015-10-20

    The newly developed multifunctional (self-activated fluorescent, mesoporous, and biocompatible) hollow mesoporous silica nanoellipsoids (f-hMS) are potentially useful as a delivery system of drugs for therapeutics and imaging purposes. For the synthesis of f-hMS, self-activated fluorescence hydroxyapatite (fHA) was used as a core template. A mesoporous silica shell was obtained by silica formation and subsequent removal of the fHA core, which resulted in a hollow-cored f-hMS. Although the silica shell provided a highly mesoporous structure, enabling an effective loading of drug molecules, the fluorescent property of fHA was also well-preserved in the f-hMS. Cytochrome c and doxorubicin, used as a model protein and anticancer drug, respectively, were shown to be effectively loaded onto f-hMS and were then released in a sustainable and controllable manner. The f-hMS was effectively taken up by the cells and exhibited fluorescent labeling while preserving excellent cell viability. Overall, the f-hMS nanoreservoir may be useful as a multifunctional carrier system for drug delivery and cell imaging.

  12. Facile and scalable preparation of highly wear-resistance superhydrophobic surface on wood substrates using silica nanoparticles modified by VTES

    NASA Astrophysics Data System (ADS)

    Jia, Shanshan; Liu, Ming; Wu, Yiqiang; Luo, Sha; Qing, Yan; Chen, Haibo

    2016-11-01

    In this study, an efficient, facile method has been developed for fabricating superhydrophobic surfaces on wood substrates using silica nanoparticles modified by VTES. The as-prepared superhydrophobic wood surface had a water contact angle of 154° and water slide angle close to 0°. Simultaneously, this superhydrophobic wood showed highly durable and robust wear resistance when having undergone a long period of sandpaper abrasion or being scratched by a knife. Even under extreme conditions of boiling water, the superhydrophobicity of the as-prepared wood composite was preserved. Characterizations by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy showed that a typical and tough hierarchical micro/nanostructure was created on the wood substrate and vinyltriethoxysilane contributed to preventing the agglomeration of silica nanoparticles and serving as low-surface-free-energy substances. This superhydrophobic wood was easy to fabricate, mechanically resistant and exhibited long-term stability. Therefore, it is considered to be of significant importance in the industrial production of functional wood, especially for outdoor applications.

  13. Preparation of Mn-Zn ferrite nanoparticles and their silica-coated clusters: Magnetic properties and transverse relaxivity

    NASA Astrophysics Data System (ADS)

    Kaman, Ondřej; Kuličková, Jarmila; Herynek, Vít; Koktan, Jakub; Maryško, Miroslav; Dědourková, Tereza; Knížek, Karel; Jirák, Zdeněk

    2017-04-01

    Hydrothermal synthesis of Mn1-xZnxFe2O4 nanoparticles followed by direct encapsulation of the as-grown material into silica is demonstrated as a fast and facile method for preparation of efficient negative contrast agents based on clusters of ferrite crystallites. At first, the hydrothermal procedure is optimized to achieve strictly single-phase magnetic nanoparticles of Mn-Zn ferrites in the compositional range of x≈0.2-0.6 and with the mean size of crystallites ≈10 nm. The products are characterized by powder X-ray diffraction, X-ray fluorescence spectroscopy, and SQUID magnetometry, and the composition close to x=0.4 is selected for the preparation of silica-coated clusters with the mean diameter of magnetic cores ≈25 nm. Their composite structure is studied by means of transmission electron microscopy combined with detailed image analysis and magnetic measurements in DC fields. The relaxometric studies, performed in the magnetic field of B0=0.5 T, reveal high transverse relaxivity (r2(20 °C)=450 s-1 mmol(Me3O4)-1 L) with a pronounced temperature dependence, which correlates with the observed temperature dependence of magnetization and is ascribed to a mechanism of transverse relaxation similar to the motional averaging regime.

  14. Aptamer-based organic-silica hybrid affinity monolith prepared via "thiol-ene" click reaction for extraction of thrombin.

    PubMed

    Wang, Zheng; Zhao, Jin-cheng; Lian, Hong-zhen; Chen, Hong-yuan

    2015-06-01

    A novel strategy for preparing aptamer-based organic-silica hybrid monolithic column was developed via "thiol-ene" click chemistry. Due to the large specific surface area of the hybrid matrix and the simplicity, rapidness and high efficiency of "thiol-ene" click reaction, the average coverage density of aptamer on the organic-silica hybrid monolith reached 420 pmol μL(-1). Human α-thrombin can be captured on the prepared affinity monolithic column with high specificity and eluted by NaClO4 solution. N-p-tosyl-Gly-Pro-Arg p-nitroanilide acetate was used as the sensitive chromogenic substrate of thrombin. The thrombin enriched by this affinity column was detected with a detection of limit of 0.01 μM by spectrophotometry. Furthermore, the extraction recovery of thrombin at 0.15 μM in human serum was 91.8% with a relative standard deviation of 4.0%. These results indicated that "thiol-ene" click chemistry provided a promising technique to immobilize aptamer on organic-inorganic hybrid monolith and the easily-assembled affinity monolithic material could be used to realize highly selective recognition of trace proteins.

  15. One-pot preparation of glutathione-silica hybrid monolith for mixed-mode capillary liquid chromatography based on "thiol-ene" click chemistry.

    PubMed

    Lin, Zian; Tan, Xiaoqing; Yu, Ruifang; Lin, Jiashi; Yin, Xiaofei; Zhang, Lan; Yang, Huanghao

    2014-08-15

    A novel glutathione (GSH)-silica hybrid monolithic column synthesized via a combination of thiol-ene click reaction and one-pot process was described, where thiol-end GSH organic monomer and 2,2-azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethyloxysilane (TMOS) and γ-methacryloxypropyltrimethoxysilane (γ-MAPS) and then introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the GSH-silica hybrid monolith. The effects of the molar ratio of TMOS/γ-MAPS, the amount of GSH, and the volume of porogen on the morphology, permeability and pore properties of the prepared GSH-silica hybrid monoliths were studied in detail. A uniform monolithic network with high porosity was obtained. A series of test compounds including alkylbenzenes, amides, and anilines were used to evaluate the retention behaviors of the GSH-silica hybrid monolithic column. The results demonstrated that the prepared GSH-silica hybrid monolith exhibited multiple interactions including hydrophobicity, hydrophilicity, as well as cation exchange interaction. The run-to-run, column-to-column and batch-to-batch reproducibilities of the GSH-silica hybrid monolith for phenols' retention were satisfactory with the relative standard deviations (RSDs) less than 1.3% (n=5), 2.6% (n=3) and 3.2% (n=3), respectively, indicating the effectiveness and practicability of the proposed method. In addition, the GSH-silica hybrid monolith was applied to the separation of nucleotides, peptides and protein tryptic digests, respectively. The successful applications suggested the potential of the GSH-silica hybrid monolith in complex sample analysis.

  16. Preparation of nanoporous systems for the study of the mechanical properties of silica aerogels by Molecular Dynamics simulations

    NASA Astrophysics Data System (ADS)

    Rivas Murillo, John S.; Bachlechner, Martina E.; Barbero, Ever J.

    2009-03-01

    This presentation focuses on the application of the Molecular Dynamics technique to study the mechanical properties of silica aerogels through the simulation of a tension test. It covers multiple areas, including aspects related to the preparation of a well-relaxed nanoporous system from the expansion of an amorphous bulk sample and the influence of the initial configuration of the system on the final results of the simulated tension test. The results presented here will help to develop a more complete procedure to prepare a proper sample for the study of the mechanical properties of a nanoporous system by using Molecular Dynamics. Comparison of the simulation results and previously published experimental data is provided

  17. Capillary electrochromatography with monolithic silica column: I. Preparation of silica monoliths having surface-bound octadecyl moieties and their chromatographic characterization and applications to the separation of neutral and charged species.

    PubMed

    Allen, Darin; El Rassi, Ziad

    2003-01-01

    Monolithic silica columns with surface-bound octadecyl (C18) moieties have been prepared by a sol-gel process in 100 microm ID fused-silica capillaries for reversed-phase capillary electrochromatography of neutral and charged species. The reaction conditions for the preparation of the C18-silica monoliths were optimized for maximum surface coverage with octadecyl moieties in order to maximize retention and selectivity toward neutral and charged solutes with a sufficiently strong electroosmotic flow (> 2 mm/s) to yield rapid analysis time. Furthermore, the effect of the pore-tailoring process on the silica monoliths was performed over a wide range of treatment time with 0.010 M ammonium hydroxide solution in order to determine the optimum time and conditions that yield mesopores of narrow pore size distribution that result in high separation efficiency. Under optimum column fabrication conditions and optimum mobile phase composition and flow velocity, the average separation efficiency reached 160 000 plates/m, a value comparable to that obtained on columns packed with 3 microm C18-silica particles with the advantages of high permeability and virtually no bubble formation. The optimized monolithic C18-silica columns were evaluated for their retention properties toward neutral and charged analytes over a wide range of mobile phase compositions. A series of dimensionless retention parameters were evaluated and correlated to solute polarity and electromigration property. A dimensionless mobility modulus was introduced to describe charged solute migration and interaction behavior with the monolithic C18-silica in a counterflow regime during capillary electrochromatography (CEC )separations. The mobility moduli correlated well with the solute hydrophobic character and its charge-to-mass ratio.

  18. Preparation of single-site catalyst inside the functionalized nanopore of silica and its ethylene polymerization.

    PubMed

    Lee, Sang Yun; Ko, Young Soo

    2013-06-01

    Amorphous silica have been functionalized with organo-silane, and (n-BuCp)2ZrCI2 and methylaluminoxane (MAO) were subsequently immobilized on the functionalized silica for the further evaluation as a catalyst of ethylene polymerization. Four organo-silanes such as 3-aminopropyltrimethoxysilane (1NS), N-[(3-trimethoxysilyl)propyl]ethylenediamine (2NS), N1-[3-(trimethoxysilyl)propyl]diethylenetriamine (3NS), and 4-(triethoxysilyl)butyronitrile (1NCy), were employed for this study. The Zr content and polymerization activity of the supported catalysts were strongly dependent on the kind and structure of organo-silane. 2NS showed the highest Zr content with higher activity, indicating the more Zr could be captured due to a stronger interaction between (n-BuCp)2ZrCl2 and amine group.

  19. Preparation and characterization of silica aerogels from diatomite via ambient pressure drying

    NASA Astrophysics Data System (ADS)

    Wang, Baomin; Ma, Hainan; Song, Kai

    2014-07-01

    The silica aerogels were successfully fabricated under ambient pressure from diatomite. The influence of different dilution ratios of diatomite filtrate on physical properties of aerogels were studied. The microstructure, surface functional groups, thermal stability, morphology and mechanical properties of silica aerogels based on diatomite were investigated by BET adsorption, FT-IR, DTA-TG, FESEM, TEM, and nanoindentation methods. The results indicate that the filtrate diluted with distilled water in a proportion of 1: 2 could give silica aerogels in the largest size with highest transparency. The obtained aerogels with density of 0.122-0.203 g/m3 and specific surface area of 655.5-790.7 m2/g are crack free amorphous solids and exhibited a sponge-like structure. Moreover, the peak pore size resided at 9 nm. The initial aerogels were hydrophobic, when being heat-treated around 400°C, the aerogels were transformed into hydrophilic ones. The obtained aerogel has good mechanical properties.

  20. Preparation and characterization of antibacterial Senegalia (Acacia) senegal/iron-silica bio-nanocomposites

    NASA Astrophysics Data System (ADS)

    Şişmanoğlu, Tuba; Karakuş, Selcan; Birer, Özgür; Soylu, Gülin Selda Pozan; Kolan, Ayşen; Tan, Ezgi; Ürk, Öykü; Akdut, Gizem; Kilislioglu, Ayben

    2015-11-01

    Many studies that research bio-nanocomposites utilize techniques that involve the dispersion of strengthening components like silica, metal and metal oxides through a host biopolymer matrix. The biggest success factor for the bio-nanocomposite is having a smooth integration of organic and inorganic phases. This interattraction between the surfaces of inorganic particles and organic molecules are vital for good dispersion. In this study, a novel biodegradable antibacterial material was developed using gum arabic from Senegalia senegal (stabilizer), silica (structure reinforcer) and zero valent iron particles. Silica particles work to not only strengthen the mechanical properties of the Senegalia senegal but also prevent the accumulation of ZVI nanoparticles due to attraction between hydroxyl groups and FeO. The gum arabic/Fe-SiO2 bio-nanocomposite showed effective antibacterial property against the Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli. Using Scanning electron microscopy, homogeneous dispersion and uniform particle size was viewed in the biopolymer. X-ray diffraction studies of iron particles organization in Senegalia senegal also showed that the main portion of iron was crystalline and in the form of FeO and Fe0. X-ray photoelectron spectroscopy was used to evaluate the chemical composition of the surface but no appreciable peak was measured for the iron before Ar etching. These results suggest that the surface of iron nanoparticles consist mainly of a layer of iron oxides in the form of FeO. Thermal gravimetric analysis was used to determine the thermal stability and absorbed moisture content.

  1. Preparation and in vitro/in vivo Evaluation of Lacidipine by Adsorption onto Fumed Silica Using Supercritical Carbon Dioxide.

    PubMed

    Geng, Yajie; Fu, Qiang; Guo, Bei; Li, Yun; Zhang, Xiangrong; Wang, Xianglin; Zhang, Tianhong

    2016-01-01

    The aim of this study was to design a silica-supported solid dispersion of lacidipine (LCDP) to enhance the dissolution rate and oral absorption using supercritical CO2 (scCO2) as a solvent. The formulation was characterized using differential scanning calorimetry, powder X-ray diffraction, scanning electron microscopy and fourier transformed infrared spectroscopy. In the dissolution test, LCDP-scCO2 formulation showed a significantly enhanced dissolution compared with LCDPsilica physical mixture and a faster dissolution rate than Lacipil® under different dissolution conditions. In an in vivo test, the area under concentration-time curve and Cmax of LCDP-scCO2 formulation was 9.23 and 23.78 fold greater than LCDP-silica physical mixture (1:15, w/w), respectively, whereas the corresponding values were 1.92 and 2.80 fold greater than Lacipil®, respectively. Our results showed that the solid dispersion prepared by supercritical fluids technology is a feasible method to enhance the oral bioavailability of LCDP.

  2. Preparation and evaluation of a lysine-bonded silica monolith as polar stationary phase for hydrophilic interaction pressurized capillary electrochromatography.

    PubMed

    Huang, Guihua; Lian, Qiuyan; Zeng, Wencan; Xie, Zenghong

    2008-09-01

    A silica-based monolith as polar stationary phase was described for hydrophilic interaction pressurized capillary electrochromatography (HI-pCEC). The polar monolithic column was prepared by on-column reaction of lysine with epoxy groups on a gamma-glycidoxypropyltrimethosysilane-modified silica monolith. The stationary phase yielded strong hydrophilic interaction due to the slightly polar hydroxyl groups, and the strong polar lysine ligand with amino groups and carboxylic groups contained on the surface of the monolith. In order to evaluate the hydrophilic character of lysine ligand, the chromatographic behaviors of epoxy monolith (before lysine bonded) and diol monolith (hydroxyl groups contained) were also investigated. Two groups of comparative experiment were developed in terms of the separation of typical neutral non-polar and polar compounds performed in a mobile phase of aqueous-acetonitrile solution. Results showed that the lysine monolith was much more hydrophilic than the diol monolith, which presented less hydrophobic than the epoxy monolith. For further study on its hydrophilic character, the lysine monolith was demonstrated in the HI-pCEC mode for the separations of various polar compounds such as phenols, nucleic acid bases and nucleosides.

  3. Structural, Optical and Magnetic Properties of Nickel-Silica Nanocomposite Prepared by a Sol-Gel Route

    NASA Astrophysics Data System (ADS)

    Saha, Mrinal; Soumya Mukherjee; Gayen, Arup; Siddhartha Mukherjee

    2015-10-01

    Nickel-silica nanocomposites have been synthesized by a sol-gel method using dextrose (C6H12O6) as the reducing agent. The dried gel is heat treated at 850 and 900 °C for 30 min in an inert atmosphere by N2 purging to obtain the composite material. The samples have been characterized by powder X-ray diffraction, field emission scanning electron microscopy, atomic force microscopy, transmission electron microscopy and selected area electron diffraction. Pure polycrystalline nickel granular particle has been found to form with face-centered cubic structure and is entrapped in amorphous silica matrix with particle sizes in between 10 and 30 nm and is almost spherical in shape. The strong ferromagnetic nature of Ni-SiO2 composite became evident from the M-H curve which is quite different from the bulk nickel. The band gap of the synthesized Ni-SiO2 nanocomposite is found to be 2.35 eV. The reported sol-gel technique is a convenient and effective method to prepare high purity nanopowders with uniform size distribution.

  4. Preparation of iron boride-silica core-shell nanoparticles with soft ferromagnetic properties.

    PubMed

    Saiyasombat, C; Petchsang, N; Tang, I M; Hodak, J H

    2008-02-27

    A one-pot aqueous chemical synthesis for silica-passivated ferromagnetic nanoparticles is presented. The average size of these particles is 84 ± 20 nm. The x-ray and electron diffraction experiments revealed that the nanoparticles are mainly composed of polycrystalline iron boride. The broad x-ray diffraction peak leads to an average crystallite size of 1.8 nm, which is much smaller than the overall size of the particles, and is consistent with the polycrystalline nature of the samples. Mössbauer spectroscopy and magnetization experiments were used to establish the room temperature magnetic properties as well as the chemical nature of the particles. Fe(2)B dominates the composition of the nanoparticles, having a hyperfine field broadly distributed in the 10-33 T range. Alpha iron, the second ferromagnetic material identified in the particles, amounts to 4.6% of the composition. Finally, a paramagnetic phase accounting for approximately 14.6% of the material of the particles was also detected. These nanoparticles contain a core with soft ferromagnetic properties surrounded by a passivating silica layer, and are suitable for magnetically targeted drug delivery and electromagnetic induction heating applications.

  5. Preparation of porous hollow silica spheres via a layer-by-layer process and the chromatographic performance

    NASA Astrophysics Data System (ADS)

    Wei, Xiaobing; Gong, Cairong; Chen, Xujuan; Fan, Guoliang; Xu, Xinhua

    2017-01-01

    Hollow silica spheres possessing excellent mechanical properties were successfully prepared through a layer-by-layer process using uniform polystyrene (PS) latex fabricated by dispersion polymerization as template. The formation of hollow SiO2 micro-spheres, structures and properties were observed in detail by zeta potential, SEM, TEM, FTIR, TGA and nitrogen sorption porosimetry. The results indicated that the hollow spheres were uniform with particle diameter of 1.6 μm and shell thickness of 150 nm. The surface area was 511 m2/g and the pore diameter was 8.36 nm. A new stationary phase for HPLC was obtained by using C18-derivatized hollow SiO2 micro-spheres as packing materials and the chromatographic properties were evaluated for the separation of some regular small molecules. The packed column showed low column pressure, high values of efficiency (up to about 43 000 plates/m) and appropriate asymmetry factors.

  6. Preparation of Fe3O4 encapsulated-silica sulfonic acid nanoparticles and study of their in vitro antimicrobial activity.

    PubMed

    Naeimi, Hossein; Nazifi, Zahra Sadat; Amininezhad, Seyedeh Matin

    2015-08-01

    A simple and efficient method for the functionalization of silica-coated Fe3O4 magnetic nanoparticles (Fe3O4@SiO2) using chlorosulfonic acid is described. The prepared compounds were screened for antibacterial activity against Escherichia coli (E. coli ATCC 25922) and Staphylococcus aureus (S. aureus ATCC 25923) under UV-light and dark conditions. It was found that the Fe3O4@SiO2-SO3H was significantly indicated the higher photocatalytic inactivation than both Fe3O4 and Fe3O4@SiO2 against E. coli in compared with S. aureus. Furthermore, the inactivation efficiency against both organisms under light conditions has been higher than this efficiency under dark conditions.

  7. Preparation of porous hollow silica spheres via a layer-by-layer process and the chromatographic performance

    NASA Astrophysics Data System (ADS)

    Wei, Xiaobing; Gong, Cairong; Chen, Xujuan; Fan, Guoliang; Xu, Xinhua

    2017-03-01

    Hollow silica spheres possessing excellent mechanical properties were successfully prepared through a layer-by-layer process using uniform polystyrene (PS) latex fabricated by dispersion polymerization as template. The formation of hollow SiO2 micro-spheres, structures and properties were observed in detail by zeta potential, SEM, TEM, FTIR, TGA and nitrogen sorption porosimetry. The results indicated that the hollow spheres were uniform with particle diameter of 1.6 μm and shell thickness of 150 nm. The surface area was 511 m2/g and the pore diameter was 8.36 nm. A new stationary phase for HPLC was obtained by using C18-derivatized hollow SiO2 micro-spheres as packing materials and the chromatographic properties were evaluated for the separation of some regular small molecules. The packed column showed low column pressure, high values of efficiency (up to about 43 000 plates/m) and appropriate asymmetry factors.

  8. Microporous biodegradable polyurethane membranes for tissue engineering.

    PubMed

    Tsui, Yuen Kee; Gogolewski, Sylwester

    2009-08-01

    Microporous membranes with controlled pore size and structure were produced from biodegradable polyurethane based on aliphatic diisocyanate, poly(epsilon-caprolactone) diol and isosorbide chain extender using the modified phase-inversion technique. The following parameters affecting the process of membrane formation were investigated: the type of solvent, solvent-nonsolvent ratio, polymer concentration in solution, polymer solidification time, and the thickness of the polymer solution layer cast on a substrate. The experimental systems evaluated were polymer-N,N-dimethylformamide-water, polymer-N,N-dimethylacetamide-water and polymer-dimethylsulfoxide-water. From all three systems evaluated the best results were obtained for the system polymer-N,N-dimethylformamide-water. The optimal conditions for the preparation of microporous polyurethane membranes were: polymer concentration in solution 5% (w/v), the amount of nonsolvent 10% (v/v), the cast temperature 23 degrees C, and polymer solidification time in the range of 24-48 h depending on the thickness of the cast polymer solution layer. Membranes obtained under these conditions had interconnected pores, well defined pore size and structure, good water permeability and satisfactory mechanical properties to allow for suturing. Potential applications of these membranes are skin wound cover and, in combination with autogenous chondrocytes, as an "artificial periosteum" in the treatment of articular cartilage defects.

  9. Preparation and characterization of pure and mixed monolayers of poly(ethylene glycol) brushes chemically adsorbed to silica surfaces.

    PubMed

    McNamee, Cathy E; Yamamoto, Shinpei; Higashitani, Ko

    2007-04-10

    We prepared pure and mixed monolayers of methoxy-terminated poly(ethylene glycol)s (m-PEG's) chemically attached to silica surfaces by using m-PEG silane coupling agents of three different molecular weights. These films were subsequently characterized in water by atomic force microscopy (AFM). Images of pure m-PEG monolayers showed the formation of polymer brushes on silica. Force curves between two modified surfaces suggested that an increase in the number of oxyethylene (OE) groups from 6 (PEG6 surface) to 43 (PEG43 surface) to 113 (PEG113 surface) decreased the flexibility of the m-PEG chains in the m-PEG brushes. Frictional force measurements also showed that the friction increased in the order PEG6 < PEG43 prepared using various fractions of PEG6 and PEG113. Images of mixed PEG6 and PEG113 monolayers showed that the size of the PEG113 islands in the film decreased as the fraction of PEG113 decreased. The force curves between two modified surfaces suggested that the flexibility of the mixed monolayers decreased as the fraction of PEG113 increased. Frictional force measurements also showed that the friction decreased as the fraction of PEG6 in the PEG6-PEG113 mixed film increased. Entanglements were therefore thought to decrease as the fraction of PEG113 in the mixed monolayer decreased.

  10. Controlling surface energy of glass substrates to prepare superhydrophobic and transparent films from silica nanoparticle suspensions.

    PubMed

    Ogihara, Hitoshi; Xie, Jing; Saji, Tetsuo

    2015-01-01

    We fabricated superhydrophobic and transparent silica nanoparticle (SNP) films on glass plates via spray-coating technique. When suspensions containing 1-propanol and hydrophobic SNPs were sprayed over glass plates that were modified with dodecyl groups, superhydrophobic and transparent SNP films were formed on the substrates. Surface energy of the glass plates had a significant role to obtain superhydrophobic and transparent SNP films. SNP films did not show superhydrophobicity when bare glass plates were used as substrates, because water droplets tend to adhere the exposed part of the hydrophilic glass plate. Glass plates having extreme low surface energy were not also suitable because suspension solution was repelled from the substrates, which resulted in forming non-uniform SNP films.

  11. [Preparation and stability of β-carotene loaded using mesoporous silica nanoparticles as carriers system].

    PubMed

    Liu, Jing; Ren, Zhi-hui; Wang, Hai-yuan; Jin, Xing-hua

    2015-09-01

    1,3,5-Trimethylbenzene (1,3,5-TMB) was used as the pore-enlarging modifier to expand the pore size of MCM-41 (mobil company of matter) mesoporous silica nanoparticles. The solvent impregnation method was adopted to assemble non-water-soluble β-carotene into the pore channel of MCM-41. The MCM-41 and drug assemblies were characterized by TEM, FT-IR, elemental analysis and N2 adsorption-desorption. The results showed that MCM-41 has good sphericity and regular pore structure. The research also investigated the optimal loading time, the drug loading and the vitro stability of the β-carotene. As a drug carrier, the modified MCM-41 showing a shorter drug loading time, the drug loading as high as 85.58% and the stability of β-carotene in drug assemblies has improved. The study of this new formulation provides a new way for β-carotene application.

  12. Preparation of MTMS based transparent superhydrophobic silica films by sol-gel method.

    PubMed

    Venkateswara Rao, A; Latthe, Sanjay S; Nadargi, Digambar Y; Hirashima, H; Ganesan, V

    2009-04-15

    Superhydrophobic surfaces with water contact angle higher than 150 degrees generated a lot of interest both in academia and in industry because of the self-cleaning properties. Optically transparent superhydrophobic silica films were synthesized at room temperature (27 degrees C) using sol-gel process by a simple dip coating technique. The molar ratio of MTMS:MeOH:H(2)O (5 M NH(4)OH) was kept constant at 1:10.56:4.16, respectively. Emphasis is given to the effect of the surface modifying agents on the hydrophobic behavior of the films. Methyl groups were introduced in the silica film by post-synthesis grafting from two solutions using trimethylchlorosilane (TMCS) and hexamethyldisilazane (HMDZ) silylating agents in hexane solvent, individually. The percentage of silylating agents and silylation period was varied from 2.5 to 7.5% and 1 to 3 h, respectively. The TMCS modified films exhibited a very high water contact angle (166+/-2 degrees) in comparison to the HMDZ (138+/-2 degrees) modified films, indicating the water repellent behavior of the surface. When the TMCS and HMDZ modified films were heated at temperatures higher than 350 degrees C and 335 degrees C, respectively, the films became superhydrophilic; the contact angle for water on the films was smaller than 5 degrees. Further, the humidity study was carried out at a relative humidity of 85% at 30 degrees C temperature over 30 days. The films have been characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FT-IR), % optical transmission, humidity tests and contact angle (CA) measurements.

  13. Development of a simple method for the preparation of novel egg-shell type Pt catalysts using hollow silica nanostructures as supporting precursors

    SciTech Connect

    Wang Jiexin; Chen Jianfeng

    2008-04-01

    A simple method for the preparation of novel egg-shell type platinum catalysts was developed and achieved by utilizing unique hollow silica nanostructures, i.e., hollow silica nanospheres and nanotubes, as supports. The observation by transmission electron microscopy indicated that the well-dispersed hollow silica supported Pt catalysts with a Pt particle diameter of 8-14 nm can be successfully prepared by wet impregnation process and heat treatment. The Pt-loaded hollow silica nanostructures were also characterized by inductively coupled plasma, X-ray diffraction, specific surface area, Fourier transformation infrared spectroscopy, X-ray photoelectron spectroscopy and energy dispersive spectroscopy. It was thus demonstrated that a higher Pt loading amount (0.392%) could be obtained under the same conditions except the addition of ammonia, which was found to be more effective than that (0.061%) with the addition of HCl in the immobilization of Pt. In addition, the effect of soaking time, Pt precursor concentration and calcination temperature on the loading of Pt in hollow silica nanostructures were investigated as well.

  14. Slow Desorption of Phenanthrene from Silica Particles: Influence of Pore Size, Pore Water, and Aging Time

    SciTech Connect

    Huesemann, Michael H.; Fortman, Timothy J.; Riley, Robert G.; Thompson, Christopher J.; Wang, Zheming; Truex, Michael J.; Peyton, Brent M.

    2006-01-16

    When micro-porous and meso-porous silica particles were exposed to aqueous phenanthrene solutions for various durations it was observed that sorbed-phase phenanthrene concentrations increased with aging time only for meso-porous but not micro-porous silicas. Desorption equilibrium was reached almost instantaneously for the micro-porous particles while both the rate and extent of desorption decreased with increasing aging time for the meso-porous silicas. These findings indicate that phenanthrene can be sequestered within the internal pore-space of meso-porous silicas while the internal surfaces of micro-porous silicas are not accessible to phenanthrene sorption, possibly due to the presence of physi- or chemi-sorbed water that may sterically hinder the diffusion of phenanthrene inside water-filled micro-pores. By contrast, the internal surfaces of these micro-porous silicas are accessible to phenanthrene when aging methods are employed which assure that pores are devoid of physi-sorbed water. Consequently, when phenanthrene was incorporated into these particles using either supercritical CO2 or via solvent soaking, the aqueous desorption kinetics were extremely slow indicating effective sequestration of phenanthrene inside micro-porous particles. Finally, a two-compartment conceptual model is used to interpret the experimental findings.

  15. Methods for synthesizing microporous crystals and microporous crystal membranes

    DOEpatents

    Dutta, Prabir; Severance, Michael; Sun, Chenhu

    2017-02-07

    A method of making a microporous crystal material, comprising: a. forming a mixture comprising NaOH, water, and one or more of an aluminum source, a silicon source, and a phosphate source, whereupon the mixture forms a gel; b. heating the gel for a first time period, whereupon a first volume of water is removed from the gel and micoroporous crystal nuclei form, the nuclei having a framework; and c.(if a membrane is to be formed) applying the gel to a solid support seeded with microporous crystals having a framework that is the same as the framework of the nuclei; d. heating the gel for a second time period. during which a second volume of water is added to the gel; wherein the rate of addition of the second volume of water is between about 0.5 and about 2.0 fold the rate of removal of the first volume of water.

  16. Preparation of TiO2/MCM-41 photocatalyst using rice husk ash as silica source

    NASA Astrophysics Data System (ADS)

    Fatimah, Is; Sopia, Lusi

    2017-03-01

    This work aimed to prepare TiO2/MCM-41 from rice husk ash (RHA) agricultural waste and its application as photocatalyst in dye degradation. The preparation was conducted by two main steps; preparation of MCM-41 and titanium immobilization onto MCM-41. Sol gel method using CTMABr as templating agent was applied in MCM-41 synthesis and as TiO2 precursor, titanium isopropoxide was utilized. The study of physicochemical character change was performed by by X-ray diffraction, IR spectroscopy, BET method and thermogravimetric analysis (TGA). Photocatalytic activity of material was tested in methylene blue photodegradation system. According to the results, it is found that TiO2/MCM-41 has been successfully prepared and shows photocatalytic activity. Kinetic study of the reaction is discussed in this paper.

  17. Preparation and characterization of new photoluminescent nano-powder based on Eu3+:La2Ti2O7 and dispersed into silica matrix for latent fingerprint detection

    NASA Astrophysics Data System (ADS)

    Saif, M.; Alsayed, N.; Mbarek, A.; El-Kemary, M.; Abdel-Mottaleb, M. S. A.

    2016-12-01

    Pure lanthanum titanate doped with europium metal ions (La2Ti2O7:Eu3+) and dispersed in silica matrix phosphor powder was prepared by sol-gel process followed by thermal treatment. The prepared nanophosphors were characterized by powder X-ray Diffraction (XRD), Fourier Transform Infrared (FT-IR), Transmission Electron Microscope (TEM), Energy Dispersive Spectroscopy (EDX), and Photoluminescence Spectroscopy (PL). The effects of silica, thermal treatment, Eu3+ ion, and surfactant (CTAB) concentrations on the crystal, morphology, and photoluminescence properties were investigated. The present work found that dispersion of La2Ti2O7:Eu3+ into silica matrix significantly altered the morphology of La2Ti2O7:Eu3+ from high crystalline micro-plate like shape into amorphous aggregated Nano-spherical shape. The high separated spherical shape with intense red PL emission and long lifetime was obtained from 10 mol% Eu3+:La2Ti2O7:Eu3+, dispersed into silica matrix, and prepared in the presence of CTAB. The high PL Nano-phosphor has been successfully used in developing latent fingerprint from various forensic relevant materials.

  18. One Polymorph and Various Morphologies of Phenytoin at a Silica Surface Due to Preparation Kinetics

    PubMed Central

    2014-01-01

    The preparation of solid crystalline films at surfaces is of great interest in a variety of fields. Within this work the preparation of pharmaceutically relevant thin films containing the active pharmaceutical ingredient phenytoin is demonstrated. The preparation techniques applied include drop casting, spin coating, and vacuum deposition. For the solution processed samples a decisive impact of the solution concentration and the applied film fabrication technique is observed; particular films form for all samples but with their extensions along different crystallographic directions strongly altered. Vacuum deposition of phenytoin reveals amorphous films, which over time crystallize into needle-like or particular-type structures whereby a nominal thickness of 50 nm is required to achieve a fully closed layer. Independent of all preparation techniques, the resulting polymorph is the same for each sample as confirmed by specular X-ray diffraction scans. Thus, morphologies observed via optical and atomic force microscope techniques are therefore a result of the preparation technique. This shows that the different time scales for which crystallization is obtained is the driving force for the various morphologies in phenytoin thin films rather than the presence of another polymorph forming. PMID:25593545

  19. Preparation and adsorption behavior of berberine hydrochloride imprinted polymers by using silica gel as sacrificed support material

    NASA Astrophysics Data System (ADS)

    Li, Hui; Li, Yuzhuo; Li, Zhiping; Peng, Xiyang; Li, Yanan; Li, Gui; Tan, Xianzhou; Chen, Gongxi

    2012-03-01

    Preparation of berberine hydrochloride (B-Cl) imprinted polymers (MIPs) based on surface imprinting technique with silica gel as sacrificial support material was performed successfully by using B-Cl as template, methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) as functional monomer and cross-linker, respectively. The prepared polymers were characterized by Fourier transmission infrared spectrometry (FTIR) and scanning electron microscopy (SEM). Adsorption behavior of the MIPs for the template and its structural analogues was investigated. Sites distribution on the surface of MIPs was explored by using different isotherm adsorption models and thermodynamic parameters for the adsorption of B-Cl on the MIPs determined. Sample application and reusability for the MIPs was also evaluated. Results indicated the strong adsorption and high selectivity of the MIPs for B-Cl. Saturated adsorption capacity reached 27.2 μmol g-1 and the selectivity coefficient of the MIPs for B-Cl relative to jatrorrhizine hydrochloride (J-Cl) and palmatine palmatus hydrochloride (P-Cl) are 3.70 and 6.03, respectively. In addition, the MIPs were shown with good reusability and selectively retention ability in sample application.

  20. The hybrid photocatalyst of TiO2-SiO2 thin film prepared from rice husk silica

    NASA Astrophysics Data System (ADS)

    Klankaw, P.; Chawengkijwanich, C.; Grisdanurak, N.; Chiarakorn, Siriluk

    2012-03-01

    The TiO2-SiO2 thin film was prepared by self-assembly method by mixing SiO2 precursor with titanium precursor solution and aged to obtain a co-precipitation of silica and titanium crystals. Dip coating method was applied for thin film preparation on glass slide. The X-ray diffraction (XRD) of the self-assembly thin film had no characteristic property of SiO2 and even anatase TiO2 but indicated new crystal structure which was determined from the Fourier Transform Infrared Spectrophotometer (FTIR) as a hybridized Ti-O-Si bonding. The surface area and surface volume of the self-assembly sample were increased when SiO2 was incorporated into the film. The self-assembly TiO2-SiO2 thin film exhibited the enhanced photocatalytic decolorization of methylene blue (MB) dye. The advantages of SiO2 are; (1) to increase the adsorbability of the film and (2) to provide the hydroxyl radical to promote the photocatalytic reaction. The self-assembly thin film with the optimum molar ratio (SiO2:TiO2) as 20:80 gave the best performance for photocatalytic decolorization of MB dye with the overall efficiency of 81%.

  1. Tuning of the vinyl groups' spacing at surface of modified silica in preparation of high density imprinted layer-coated silica nanoparticles: a dispersive solid-phase extraction materials for chlorpyrifos.

    PubMed

    Lu, Qing; Chen, Xuemei; Nie, Li; Luo, Jing; Jiang, Huijun; Chen, Lina; Hu, Qin; Du, Shuhu; Zhang, Zhongping

    2010-05-15

    This paper reports the preparation of high density imprinted layer-coated silica nanoparticles toward selective recognition and fast enrichment of chlorpyrifos (CP) from complicated matrices. The molecularly imprinted polymers (MIPs) were successfully coated at the surface of modified silica through using the chemical immovable vinyl groups at the nanoparticles' surface, followed by the graft copolymerization of methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) in the presence of templates CP. It has been demonstrated that the space of end vinyl groups at the surface of silica can be controlled by changing the condition of chemical modification, regulating the thickness of imprinted shells and the density of efficient imprinted sites. After removal of templates by solvent extraction, the recognition sites of CP were created in the polymer coating layer. The CP-imprinted nanoparticles exhibited high recognition selectivity and binding affinity to CP analyte. When the CP-imprinted nanoparticles were used as dispersive solid-phase extraction (dSPE) materials, the high recovery yields of 76.1-93.5% from various spiked samples with only 1microg/mL analyte were achieved by one-step extraction. These results reported herein provide the possibility for the separation and enrichment of CP from complicated matrices by the molecular imprinting modification at the surface of common silica nanoparticles.

  2. Preparation and evaluation of 2-methylimidazolium-functionalized silica as a mixed-mode stationary phase for hydrophilic interaction and anion-exchange chromatography.

    PubMed

    Yang, Beibei; Liu, Houmei; Chen, Jia; Guan, Ming; Qiu, Hongdeng

    2016-10-14

    In this paper, a novel 2-methylimidazolium-functionalized silica stationary phase was prepared and further used for hydrophilic interaction and anion-exchange mixed-mode chromatography. The stationary phase was characterized by elemental analysis and Fourier transform infrared spectrometry. The chromatographic properties of this stationary phase were investigated by hydrophilic chromatography for the separation of nucleosides, nucleobases, water soluble vitamins, sulfonamides and saccharides, and ion chromatography for the separation of inorganic anions. The effect of acetonitrile content, salt concentration and pH values of the mobile phase on the retention of the stationary phases was also investigated. Compared with 1-methylimidazolium-functionalized silica stationary phase, this new stationary phase demonstrated similar or better separation selectivity. This new column demonstrated good performance and separation selectivity even better than a commercial hydrophilic column. Besides, 2-methylimidazolium-functionalized silica is possible to be modified again and used as a precursor to derivate some new stationary phases from the 3-position nitrogen.

  3. Preparation of amino-Fe(III) functionalized mesoporous silica for synergistic adsorption of tetracycline and copper.

    PubMed

    Zhang, Ziyang; Liu, Huijuan; Wu, Liyuan; Lan, Huachun; Qu, Jiuhui

    2015-11-01

    Finding effective methods for simultaneous removal of antibiotics and heavy metals has attracted increasing concern since both of them are frequently detected in aquatic environments. In this study, a novel mesoporous silica adsorbent (Fe-N,N-SBA15) contained dual-functional groups was synthesized by first grafting di-amino groups on SBA15, and then coordinating Fe(III) onto the adsorbent. The adsorbent was then used in the synchronous elimination of tetracycline (TC) and Cu(II) from water, which was deeply studied by solution pH, kinetics, equilibriums in sole and binary systems. It was found that the adsorbent had high affinity for both TC and Cu(II) and synergistic effects on the adsorption were found. The solution pH remarkably affected the adsorption due to pH-dependent speciation of TC, Cu(II), TC-Cu(II) complex and the surface properties of the adsorbent. Increasing adsorption amount of TC and Cu(II) on the adsorbent could be attributed to the formation of complex TC-Cu(II) bridging or the stronger affinity of the adsorbent for the TC-Cu(II) complex than that for TC or Cu(II) separately. FT-IR and XPS studies revealed that Fe(III) and amino groups on the adsorbent were complexed with the amide of TC and Cu(II), respectively. The recyclabilities of the adsorbent were also evaluated and the Fe-N,N-SBA15 exhibited good reusability for TC and Cu(II) removal. This study shows guidelines and offers an innovative, effective method for the synergistic removal of antibiotics and heavy metals from aquatic environments.

  4. White light emission from transparent SiO2 glass prepared from nanometer-sized silica particles

    NASA Astrophysics Data System (ADS)

    Uchino, Takashi; Yamada, Tomoko

    2004-08-01

    We report that nanometer-sized silicon-dioxide particles are sintered to optical transparency at temperatures even below 1000°C, forming nonporous bulk silica glass. The resultant silica glass exhibits visible emission, which appears white to the naked eye, in the wavelength range from ˜400to˜700nm at room temperature under ultraviolet excitation. The observed emission is quite stable after prolonged exposure to the atmosphere and shows no appreciable light-induced degradation. The present photoluminescence characteristics are found to be basically different from those reported previously for silica nanoparticles and silica-based porous materials.

  5. Composites of Eu(3+)-doped calcium apatite nanoparticles and silica particles: comparative study of two preparation methods.

    PubMed

    Isobe, Ayumu; Takeshita, Satoru; Isobe, Tetsuhiko

    2015-02-10

    We synthesized composites of Eu(3+)-doped calcium apatite (CaAp:Eu(3+)) nanoparticles and silica particles via two methods: (i) in situ synthesis of CaAp:Eu(3+) in the presence of silica particles and (ii) electrostatic adsorption of CaAp:Eu(3+) nanoparticles on silica particle surfaces. In both methods, submicrometer spherical silica particles were covered with CaAp:Eu(3+) nanoparticles without forming any impurity phases, as confirmed by X-ray diffractometry, Fourier-transform infrared spectroscopy, and scanning electron microscopy. In method i, part of the silica surface acted as a nucleation site for apatite crystals and silica particles were inhomogeneously covered with CaAp:Eu(3+) nanoparticles. In method ii, positively charged CaAp:Eu(3+) nanoparticles were homogeneously adsorbed on the negatively charged silica surface through electrostatic interactions. The bonds between the silica surface and CaAp:Eu(3+) nanoparticles are strong enough not to break under ultrasonic irradiation, irrespective of the synthetic method used. The composite particles showed red photoluminescence corresponding to 4f → 4f transitions of Eu(3+) under near-UV irradiation. Although the absorption coefficient of the forbidden 4f → 4f transitions of Eu(3+) was small, the red emission was detectable with a commercial fluorescence microscope because the CaAp:Eu(3+) nanoparticles accumulated on the silica particle surfaces.

  6. Facile and fast preparation of low-cost silica-supported graphitic carbon nitride for solid-phase extraction of fluoroquinolone drugs from environmental waters.

    PubMed

    Speltini, Andrea; Maraschi, Federica; Govoni, Roberta; Milanese, Chiara; Profumo, Antonella; Malavasi, Lorenzo; Sturini, Michela

    2017-03-17

    The analytical application of silica-supported graphitic carbon nitride (g-C3N4@silica) for solid-phase extraction (SPE) of fluoroquinolone (FQ) pollutants from water is presented for the first time. g-C3N4@silica was easily and quickly prepared by one-pot thermal condensation of dicyandiamide and characterized by powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy and surface area measurements. The novel composite was applied as sorbent for SPE of FQs from water prior high-performance liquid chromatography with fluorescence detection. The extraction efficiency of g-C3N4 was tested in tap and surface waters at actual concentrations (10-100ngL(-1)). Quantitative adsorption was achieved using 100mg sorbent (20wt% g-C3N4) for pre-concentration of 50-500mL sample, at the native pH (∼7.5-8). Elution was performed with 25mM H3PO4 aqueous solution-acetonitrile (80:20), obtaining recoveries in the range 70-114%, enrichment factors up to 500 and inter-day RSDs≤12%. The batch-to-batch reproducibility was assessed on three independently synthesized g-C3N4@silica preparations (RSD 6-12%). g-C3N4 supported on silica microparticles proved to be of easy preparation, inexpensive, reusable for at least 4 extractions of raw surface waters, and suitable for determination in real matrices.

  7. Preparation and evaluation of micro and meso porous silica monoliths with embedded carbon nanoparticles for the extraction of non-polar compounds from waters.

    PubMed

    Fresco-Cala, Beatriz; Cárdenas, Soledad; Valcárcel, Miguel

    2016-10-14

    A novel hybrid micro and meso porous silica monolith with embedded carbon nanoparticles (Si-CNPs monolith) was prepared inside a fused silica capillary (3cm in length) and used as a sorbent for solid-phase microextraction. The hybrid monolithic capillary was synthetized by hydrolysis and polycondensation of a mixture of tetraethoxysilane (TEOS), ethanol, and three different carbon nanoparticles such as carboxylated single-walled carbon nanotubes (c-SWCNTs), carboxylated multi-walled carbon nanotubes (c-MWCNTs), and oxidized single-walled carbon nanohorns (o-SWNHs) via a two-step catalytic sol-gel process. Compared with silica monolith without carbon nanoparticles, the developed monolithic capillary column exhibited a higher extraction efficiency towards the analytes which can be ascribed to the presence of the carbon nanoparticles. In this regard, the best performance was achieved for silica monolith with embedded c-MWCNTs. The resulted monolithic capillaries were also characterized by scanning electron microscopy (SEM), elemental analysis and nitrogen intrusion porosimetry. Variables affecting to the preparation of the sorbent phase including three different carbon nanoparticles and extraction parameters were studied in depth using polycyclic aromatic hydrocarbons (PAHs) as target analytes. Gas chromatography-mass spectrometry was selected as instrumental technique. Detection limits range from 0.1 to 0.3μgL(-1), and the inter-extraction units precision (expressed as relative standard deviation) is between 5.9 and 14.4%.

  8. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    PubMed

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples.

  9. Fabrication of colloidal crystals composed of pore-expanded mesoporous silica nanoparticles prepared by a controlled growth method.

    PubMed

    Yamamoto, Eisuke; Mori, Seiya; Shimojima, Atsushi; Wada, Hiroaki; Kuroda, Kazuyuki

    2017-02-16

    Colloidal crystals composed of mesoporous silica nanoparticles (MSNs) are expected to have various applications because of their unique hierarchical structures and tunable functions. The expansion of the mesopore size is important for introducing guest species which cannot be accommodated by using conventional colloidal crystals of MSNs; however, the preparation of MSNs with a controllable pore size, suitable for the fabrication of colloidal crystals, still remains a challenge. In this study, we fabricated colloidal crystals composed of pore-expanded MSNs using a sophisticated particle growth method to control the pore size of colloidal MSNs while retaining their monodispersity high enough to form colloidal crystals. By adding triisopropylbenzene (TIPB) only during the growth process with the stepwise addition of tetrapropoxysilane (TPOS), the particle size can be tuned from 60 nm to 100 nm, while the pore size can be tuned from 3 nm to ten plus several nm which is the largest size among the previous MSNs capable of forming colloidal crystals. These novel colloidal crystals should contribute to the expansion of nanomaterials science.

  10. Preparation of a boronate affinity silica stationary phase with enhanced binding properties towards cis-diol compounds.

    PubMed

    Li, Hengye; Zhang, Xuemeng; Zhang, Lin; Wang, Xiaojin; Kong, Fenying; Fan, Dahe; Li, Lei; Wang, Wei

    2016-11-18

    In this study, a boronate affinity silica stationary phase with enhanced binding properties towards cis-diol compounds was prepared through the combination of surface-initiated atom transfer radical polymerization (SI-ATRP) with a Wulff-type boronate as affinity ligand. The stationary phase showed good hydrophilicity and improved binding strength toward adenosine, with binding constant to be as low as 2.38×10(-4)M. The column exhibited excellent binding specificity, low binding pH (≥5.5) and high binding capacities (80.1μmol adenosine g(-1) at pH 7.0 and 45.2μmol adenosine g(-1) at pH 5.5, respectively). The stationary phase was applied as adsorbent for the selective extraction of nucleosides in human urine with excellent specificity and high enrichment efficiency. These results demonstrated that this stationary phase could be favorably applied for selective capture and enrichment of cis-diol compounds in complex samples.

  11. Preparation and characterization of 1-naphthylacetic acid-silica conjugated nanospheres for enhancement of controlled-release performance

    NASA Astrophysics Data System (ADS)

    Ao, Mingming; Zhu, Yuncong; He, Shun; Li, Deguang; Li, Pingliang; Li, Jianqiang; Cao, Yongsong

    2013-01-01

    Chemical pesticides have been widely used to increase the yield and quality of agricultural products as they are efficient, effective, and easy to apply. However, the rapid degradation and low utilization ratio of conventional pesticides has led to environmental pollution and resource waste. Nano-sized controlled-release formulations (CRFs) can provide better penetration through the plant cuticle and deliver the active ingredients efficiently to the targeted tissue. In this paper we reported novel conjugated nanospheres derived from 1-naphthylacetic acid (NNA), 3-aminopropyltriethoxysilane (APTES) and tetraethyl orthosilicate and their application as a controlled-release plant growth regulator. The NNA and APTES conjugate was prepared through a covalent cross-linking reaction and subsequent hydrolyzation and polycondensation to synthesize NNA-silica nanospheres. The release data indicated that the release of NNA was by non-Fickian transport and increased as particle size decreased. It was also found that the acidity-alkalinity was enhanced and as the temperature increased, the release of the active ingredient was faster. The nanoconjugate displayed a better efficacy in promoting root formation than NNA technical. The present study provides a novel synthesis route for CRFs comprising a pesticide, with long-duration sustained-release performance and good environmental compatibility. This method may be extended to other pesticides that possess a carboxyl group.

  12. TiO{sub 2} supported on rod-like mesoporous silica SBA-15: Preparation, characterization and photocatalytic behaviour

    SciTech Connect

    Li, Yanjuan; Li, Nan; Tu, Jinchun; Li, Xiaotian; Wang, Beibei; Chi, Yue; Liu, Darui; Yang, Dianfan

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer Rod-like SBA-15 and normal SBA-15 were used to prepare TiO{sub 2}/SBA-15 composites. Black-Right-Pointing-Pointer TiO{sub 2}/SBA-15 composites were studied as catalysts for methyl orange photodegradation. Black-Right-Pointing-Pointer TiO{sub 2}/Rod-SBA-15 exhibited higher photocatalytic activity than TiO{sub 2}/Nor-SBA-15. Black-Right-Pointing-Pointer The higher catalytic activity was a result of the controlled morphology of SBA-15. -- Abstract: TiO{sub 2} nanoparticles have been successfully incorporated in the pores of mesoporous silica SBA-15 with different morphologies by a wet impregnation method. The composites were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), inductively coupled plasma (ICP) emission spectroscopy, transmission electron microscopy (TEM), N{sub 2}-sorption and UV-Vis diffuse reflectance spectroscopy. The photodegradation of methyl orange (MO) was used to study their photocatalytic property. It is indicated that the morphology of SBA-15 had a great influence on the photocatalytic activity of the composites. When TiO{sub 2}/SBA-15 composite was prepared by loading TiO{sub 2} nanoparticles on uniform rod-like SBA-15 of 1 {mu}m length, it showed higher photocatalytic degradation rate than that on less regular but much larger SBA-15 support. This difference was rationalized in terms of the homogeneously distributed and shorter channels of rod-like SBA-15, which favored mass transport and improved the efficient utilization of the pore surface.

  13. Photoluminescence from terbium doped silica-titania prepared by a sol-gel method

    SciTech Connect

    Ismail, Adel Ali; Abboudi, Mostafa . E-mail: abboudi14@hotmail.com; Holloway, Paul; El-Shall, Hassan

    2007-01-18

    Terbium doped (0.5 at.%) TiO{sub 2}-SiO{sub 2} (30%/70%) was prepared by a sol-gel method. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the powder calcined at two different temperatures. At a low temperature of 550 deg. C an amorphous phase was obtained, but at a higher temperature of 1000 deg. C, the anatase TiO{sub 2} phase was crystallized in the amorphous SiO{sub 2} phase. Green photoluminescence from ultraviolet excitation was detected after heating to either temperature, but the amorphous sample heated to 550 deg. C exhibited a higher intensity. X-ray diffraction and photoluminescence excitation data are discussed to explain these observations.

  14. Preparation and antifrictional properties of surface modified hybrid fluorine-containing silica particles

    NASA Astrophysics Data System (ADS)

    Gorbunova, T. I.; Zapevalov, A. Ya.; Beketov, I. V.; Demina, T. M.; Timoshenkova, O. R.; Murzakaev, A. M.; Gaviko, V. S.; Safronov, A. P.; Saloutin, V. I.

    2015-01-01

    Modified SiO2 particles were successfully prepared via [(perfluorobutyl)methyl]oxirane and [(perfluorobutyl)methyl]thiirane in sol-gel conditions using basic catalysis. As a result of acid catalysis non-modified nano-sized SiO2 particles were formed. Chemically modified SiO2 particles were characterized by means of FT-IR, BET, TEM, XRD- and XPS-analyses. Friction coefficients were determined at steel surface for base oil with modified SiO2 additives (5, 10 and 15 wt.%) at 10, 20, 30 and 60 N loads. Friction was reduced most strongly in the oil mix with the lowest content of the additive. A possible mechanism of antifrictional improvement is the formation of boundary lubrication layers containing iron salts.

  15. Characteristics of organic-inorganic hybrid sols prepared from colloidal silica and multifunctional organoalkoxysilanes

    NASA Astrophysics Data System (ADS)

    Lee, Hyeon Hwa; Park, Hoy Yul; Kang, Dong Jun

    2015-01-01

    The characteristics of organic-inorganic hybrid coatings that were prepared well from surfacemodified silicate sols were studied. The surface-modified silicate sols were fabricated in a two-step sol-gel process involving nano-silicates and silanes by varying the type of silane and the reaction time. The synthesized oraganosilane-treated silicate hybrid sols were confirmed using Fouriertransform infrared (FT-IR) spectroscopy. The viscosity of the sols increased with increasing number of alkoxy functional groups in the organoalkoxysilane and the transmittance of the sol solutions decreased with increasing reaction time. The thermal stability of the hybrid coatings increased with increasing amount of inorganic components. The surface roughness of the coatings depended highly on the homogeneity of the sol solutions. In addition, the contact angle of the hybrid coatings increased as the length of the alkyl chain decreased. Importantly, stabilized hybrid sols and coatings with well-controlled surface and thermal propreties were successfully fabricated by controlling the organoalkoxysilanes and the reaction time.

  16. Yeast-based microporous carbon materials for carbon dioxide capture.

    PubMed

    Shen, Wenzhong; He, Yue; Zhang, Shouchun; Li, Junfen; Fan, Weibin

    2012-07-01

    A hierarchical microporous carbon material with a Brunauer-Emmett-Teller surface area of 1348 m(2) g(-1) and a pore volume of 0.67 cm(3) g(-1) was prepared from yeast through chemical activation with potassium hydroxide. This type of material contains large numbers of nitrogen-containing groups (nitrogen content >5.3 wt%), and, consequently, basic sites. As a result, this material shows a faster adsorption rate and a higher adsorption capacity of CO(2) than the material obtained by directly carbonizing yeast under the same conditions. The difference is more pronounced in the presence of N(2) or H(2)O, showing that chemical activation of discarded yeast with potassium hydroxide could afford high-performance microporous carbon materials for the capture of CO(2).

  17. Preparation and photoluminescence of monolithic silica glass doped with Tb3+ ions using SiO2-PVA nanocomposite

    NASA Astrophysics Data System (ADS)

    Ikeda, Hiroshi; Murata, Takahiro; Fujino, Shigeru

    2014-05-01

    The monolithic silica glass doped with Tb3+ ions was fabricated using the SiO2-PVA nanocomposite as the glass precursor. In order to dope Tb3+ ions in the monolithic silica glass, the mesoporous SiO2-PVA nanocomposite was immersed in the Tb3+ ions contained solution and subsequently sintered at 1100 °C in air. Consequently the monolithic transparent silica glass was obtained, exhibiting green fluorescence attributed to 5D4 → 7F5 main transitions under UV excitation. The Tb concentration in the sintered glass could be controlled by immersion time of the nanocomposite in the solution.

  18. Innovative Route to Prepare of Au/C Catalysts by Replication of Gold-containing Mesoporous Silicas

    NASA Astrophysics Data System (ADS)

    Kerdi, Fatmé; Caps, Valérie; Tuel, Alain

    Gold-catalyzed aerobic epoxidations in the liquid phase are generally performed in low-polarity solvents, in which conventional oxide-supported catalysts are poorly dispersed. To improve the wettability of the catalytic powder and, thus, the efficiency of the catalyst, gold nanoparticles (NPs) have been dispersed on meso-structured carbons. Gold is first introduced in functionalized mesostructured silica and particles are formed inside the porosity. Silica pores are then impregnated with a carbon precursor and the composite material is heated at 900 °C under vacuum or nitrogen. Silica is then removed by acid leaching, leading to partially encapsulated gold particles in mesoporous carbon. Carbon prevents aggregation of gold particles at high temperature, both the mean size and distribution being similar to those observed in silica. However, while Au@SiO2 exhibit significant catalytic activity in the aerobic oxidation of trans-stilbene in the liquid phase, its Au@C mesostructured replica is quite inactive.

  19. Water-dispersible Hollow Microporous Organic Network Spheres as Substrate for Electroless Deposition of Ultrafine Pd Nanoparticles with High Catalytic Activity and Recyclability.

    PubMed

    Wang, Zhifang; Chang, Jing; Hu, Yuchen; Yu, Yifu; Guo, Yamei; Zhang, Bin

    2016-11-22

    Microporous organic networks (MONs) have been considered as an ideal substrate to stabilize active metal nanoparticles. However, the development of highly water-dispersible hollow MONs nanostructures which can serve as both the reducing agent and stabilizer is highly desirable but still challenging. Here we report a template-assisted method to synthesize hollow microporous organic network (H-MON) spheres using silica spheres as hard template and 1,3,5-triethynylbenzene as the building blocks through a Glaser coupling reaction. The obtained water-dispersible H-MON spheres bearing sp- and sp(2) -hybridized carbon atoms possess a highly conjugated electronic structure and show low reduction potential; thus, they can serve as a reducing agent and stabilizer for electroless deposition of highly dispersed Pd clusters to form a Pd/H-MON spherical hollow nanocomposite. Benefitting from their high porosity, large surface area, and excellent solution dispersibility, the as-prepared Pd/H-MON hollow nanocomposite exhibits a high catalytic performance and recyclability toward the reduction of 4-nitrophenol.

  20. Separation of enantiomers on chiral stationary phase based on cellulase: Effect of preparation method and silica particle diameters on chiral recognition ability.

    PubMed

    Matsunaga, Hisami; Haginaka, Jun

    2016-10-07

    Cellulase (Cel) was immobilized onto aminopropyl-silica gels via its amino and carboxy groups, respectively, using N,N'-disuccinimidyl carbonate, and 1-ethyl-3-(3'-dimethylaminopropyl)carbodimide and N-hydroxysulfosuccinimide. They were termed N-Cel and C-Cel, respectively. Despite their smaller retention factors on a C-Cel column, the enantioseparation factors and resolution of β-blockers, propranolol, alprenolol, oxprenolol and pindolol, were similar with N- and C-Cel columns. In addition, C-Cel was prepared using aminopropyl-silica gels, whose nominal particle diameters were 5 and 3, and 2.1μm, respectively. A C-Cel column prepared with 2.1-μm aminopropyl-silica gels gave the highest enantioselectivity and column efficiency among three C-Cel columns. Furthermore, the influence of N,N-dimethyl-n-octylamine (DMOA) or cellobiose concentrations on the retentivity and enantioselectivity for β-blockers on a C-Cel column was investigated. The results indicate that single-site competition of β-blockers with DMOA or cellobiose on the catalytic binding site of Cel and the further bindings at the secondary site in a non-competitive fashion could occur. Furthermore, the enantioselective bindings of β-blockers could occur at the catalytic biding cite of Cel and at the secondary binding site.

  1. Catalytic effect of transition metals on microwave-induced degradation of atrazine in mineral micropores.

    PubMed

    Hu, Erdan; Cheng, Hefa

    2014-06-15

    With their high catalytic activity for redox reactions, transition metal ions (Cu(2+) and Fe(3+)) were exchanged into the micropores of dealuminated Y zeolites to prepare effective microporous mineral sorbents for sorption and microwave-induced degradation of atrazine. Due to its ability to complex with atrazine, loading of copper greatly increased the sorption of atrazine. Atrazine sorption on iron-exchanged zeolites was also significantly enhanced, which was attributed to the hydrolysis of Fe(3+) polycations in mineral micropores and electrostatic interactions of protonated atrazine molecules with the negatively charged pore wall surface. Copper and iron species in the micropores also significantly accelerated degradation of the sorbed atrazine (and its degradation intermediates) under microwave irradiation. The catalytic effect was attributed to the easy reducibility and high oxidation activity of Cu(2+) and Fe(3+) species stabilized in the micropores of the zeolites. It was postulated that the surface species of transition metals (monomeric Cu(2+), Cu(2+)-O-Cu(2+) complexes, FeO(+), and dinuclear Fe-O-Fe-like species) in the mineral micropores were thermally activated under microwave irradiation, and subsequently formed highly reactive sites catalyzing oxidative degradation of atrazine. The transition metal-exchanged zeolites, particularly the iron-exchanged ones, were relatively stable when leached under acidic conditions, which suggests that they are reusable in sorption and microwave-induced degradation. These findings offer valuable insights on designing of effective mineral sorbents that can selectively uptake atrazine from aqueous solutions and catalyze its degradation under microwave irradiation.

  2. Effect of Heteroatoms in Ordered Microporous Carbons on Their Electrochemical Capacitance.

    PubMed

    Itoi, Hiroyuki; Nishihara, Hirotomo; Kyotani, Takashi

    2016-11-22

    Micropores play a more important role in enhancing the electrochemical capacitance than mesopores and macropores; therefore, the effect of heteroatom doping into micropores on the electrochemical behavior is interesting. However, heteroatom doping into porous carbon materials would potentially change their pore structures and pore sizes, which also affect their electrochemical capacitive behaviors. To gain insight into the intrinsic effects of heteroatoms on the electrochemical capacitive behaviors, zeolite-templated carbon (ZTC) may be the most suitable candidate. ZTC is an ordered microporous carbon with a uniform micropore size of 1.2 nm, a high surface area, and a large micropore volume. In this work, a series of ZTCs containing oxygen, nitrogen, or boron as heteroatoms, with an ordered pore structure and the same pore size, are prepared. By examining their electrochemical capacitive behaviors in an organic electrolyte, the effect of heteroatom doping can be isolated and discussed without considering the effects of pore structure and pore size. Acid anhydride groups are found to generate pseudocapacitance in two potential ranges, -1.0 to -0.3 V (vs Ag/AgClO4) and -0.2 to 0.4 V. B is introduced into the ZTC framework solely as -B(OH)2, which is found to be an electrochemically inert species. N is introduced as pyridine (3.0%), pyridone/pyrrole (23.8%), quaternary (66.6%), and oxidized N (6.6%), and these species exhibit noticeable pseudocapacitance in the microporous carbon.

  3. Preparation of TiO2-SiO2 via sol-gel method: Effect of Silica precursor on Catalytic and Photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Fatimah, I.

    2017-02-01

    TiO2-SiO2have been synthesized by the sol-gel method from titanium isopropoxide and varied silica precursors: tetraethyl orthosilicate and tetra methyl ortho silicate. To study the effect of the precursor, prepared materials were characterized by X-ray diffraction, scanning electron microscopy, Diffuse Reflectance UV-vis optical absorption, and also gas sorption analysis. XRD patterns showed the formation of TiO2 anatase in the TiO2-SiO2 composite with different crystallite size from different silica precursor as well as the different surface morphology. The DRUV-vis absorption spectra exhibit similar band gap energy correspond to 3.21eV value while the surface area, pore volume and pore radius of the materials seems to be affected by the precursor. The higher specific surface area contributes to give the enhanced activity in phenol hydroxylation and methylene blue photodegradation.

  4. One-step preparation of CdS nanocrystals supported on thiolated silica-gel matrix and evaluation of photocatalytic performance.

    PubMed

    Andrade, George R S; Nascimento, Cristiane C; Neves, Erick C; Barbosa, Cintya D'Angeles Espirito Santo; Costa, Luiz P; Barreto, Ledjane S; Gimenez, Iara F

    2012-02-15

    Here we report the use of a thiol-functionalized silica-gel to prepare supported CdS nanocrystals by a facile one-step procedure. Upon changing the relative proportion of the matrix we obtained nanocrystals with different average sizes and size distributions, as evidenced by spectroscopic measurements as well as TEM images. Photoluminescence spectra also indicated that the main effect of the matrix is related to the size control since the spectral profiles were found to be strongly dependent on the excitation wavelength. The performance of the material in the photocatalytic degradation of two commercial dyes (methylene blue and rhodamine 6G) has been tested under sunlight radiation, showing promising results. Almost complete decolorization has been observed after 80 min of exposure, with no adsorption on the silica surface.

  5. Well-defined hollow nanochanneled-silica nanospheres prepared with the aid of sacrificial copolymer nanospheres and surfactant nanocylinders

    NASA Astrophysics Data System (ADS)

    Kim, Young Yong; Hwang, Bora; Song, Sungjin; Ree, Brian J.; Kim, Yongjin; Cho, Seo Yeon; Heo, Kyuyoung; Kwon, Yong Ku; Ree, Moonhor

    2015-08-01

    A new approach for synthesizing well-defined hollow nanochanneled-silica nanosphere particles is demonstrated, and the structural details of these particles are described for the first time. Positively charged styrene copolymer nanospheres with a clean, smooth surface and a very narrow size distribution are synthesized by surfactant-free emulsion copolymerization and used as a thermal sacrificial core template for the production of core-shell nanoparticles. A surfactant/silica composite shell with a uniform thickness is successfully produced and deposited onto the polymeric core template by charge density matching between the polymer nanosphere template surface and the negatively charged silica precursors and then followed by selective thermal decomposition of the polymeric core and the surfactant cylinder domains in the shell, producing the hollow nanochanneled-silica nanospheres. Comprehensive, quantitative structural analyses collectively confirm that the obtained nanoparticles are structurally well defined with a hollow core and a shell composed of cylindrical nanochannels that provide facile accessibility to the hollow interior space. Overall, the hollow nanochanneled-silica nanoparticles have great potential for applications in various fields.A new approach for synthesizing well-defined hollow nanochanneled-silica nanosphere particles is demonstrated, and the structural details of these particles are described for the first time. Positively charged styrene copolymer nanospheres with a clean, smooth surface and a very narrow size distribution are synthesized by surfactant-free emulsion copolymerization and used as a thermal sacrificial core template for the production of core-shell nanoparticles. A surfactant/silica composite shell with a uniform thickness is successfully produced and deposited onto the polymeric core template by charge density matching between the polymer nanosphere template surface and the negatively charged silica precursors and then

  6. Electrochemical synthesis of a microporous conductive polymer based on a metal-organic framework thin film.

    PubMed

    Lu, Chunjing; Ben, Teng; Xu, Shixian; Qiu, Shilun

    2014-06-16

    A new approach to preparing 3D microporous conductive polymer has been demonstrated in the electrochemical synthesis of a porous polyaniline network with the utilization of a MOF thin film supported on a conducting substrate. The prepared porous polyaniline with well-defined uniform micropores of 0.84 nm exhibits a high BET surface area of 986 m(2) g(-1) and a high electric conductivity of 0.125 S cm(-1) when doped with I2, which is superior to existing porous conducting materials of porous MOFs, CMPs, and COFs.

  7. Well-defined hollow nanochanneled-silica nanospheres prepared with the aid of sacrificial copolymer nanospheres and surfactant nanocylinders.

    PubMed

    Kim, Young Yong; Hwang, Bora; Song, Sungjin; Ree, Brian J; Kim, Yongjin; Cho, Seo Yeon; Heo, Kyuyoung; Kwon, Yong Ku; Ree, Moonhor

    2015-09-21

    A new approach for synthesizing well-defined hollow nanochanneled-silica nanosphere particles is demonstrated, and the structural details of these particles are described for the first time. Positively charged styrene copolymer nanospheres with a clean, smooth surface and a very narrow size distribution are synthesized by surfactant-free emulsion copolymerization and used as a thermal sacrificial core template for the production of core-shell nanoparticles. A surfactant/silica composite shell with a uniform thickness is successfully produced and deposited onto the polymeric core template by charge density matching between the polymer nanosphere template surface and the negatively charged silica precursors and then followed by selective thermal decomposition of the polymeric core and the surfactant cylinder domains in the shell, producing the hollow nanochanneled-silica nanospheres. Comprehensive, quantitative structural analyses collectively confirm that the obtained nanoparticles are structurally well defined with a hollow core and a shell composed of cylindrical nanochannels that provide facile accessibility to the hollow interior space. Overall, the hollow nanochanneled-silica nanoparticles have great potential for applications in various fields.

  8. Preparation and physical characterization of calcium sulfate cement/silica-based mesoporous material composites for controlled release of BMP-2

    PubMed Central

    Tan, Honglue; Yang, Shengbing; Dai, Pengyi; Li, Wuyin; Yue, Bing

    2015-01-01

    As a commonly used implant material, calcium sulfate cement (CSC), has some shortcomings, including low compressive strength, weak osteoinduction capability, and rapid degradation. In this study, silica-based mesoporous materials such as SBA-15 were synthesized and combined with CSC to prepare CSC/SBA-15 composites. The properties of SBA-15 were characterized by X-ray diffraction, transmission electron microscopy, and nitrogen adsorption–desorption isotherms. SBA-15 was blended into CSC at 0, 5, 10, and 20 wt%, referred to as CSC, CSC-5S (5% mass ratio), CSC-10S (10% mass ratio), and CSC-20S (20% mass ratio), respectively. Fourier-transform infrared spectroscopy and compression tests were used to determine the structure and mechanical properties of the composites, respectively. The formation of hydroxyapatite on composite surfaces was analyzed using scanning electron microscopy and X-ray diffraction after soaking in simulated body fluid. BMP-2 was loaded into the composites by vacuum freeze-drying, and its release characteristics were detected by Bradford protein assay. The in vitro degradation of the CSC/SBA-15 composite was investigated by measuring weight loss. The results showed that the orderly, nanostructured, mesoporous SBA-15 possessed regular pore size and structure. The compressive strength of CSC/SBA-15 increased with the increase in SBA-15 mass ratio, and CSC-20S demonstrated the maximum strength. Compared to CSC, hydroxyapatite that formed on the surfaces of CSC/SBA-15 was uniform and compact. The degradation rate of CSC/SBA-15 decreased with increasing mass ratio of SBA-15. The adsorption of BMP-2 increased and released at a relatively slow rate; the release rate of BMP-2 in CSC-20S was the slowest, and presented characteristics of low doses of release. In vitro experiments demonstrated that the physical properties of pure CSC incorporated with SBA-15 could be improved significantly, which made the CSC/SBA-15 composite more suitable for bone repair

  9. Pyridine-containing block copolymer/silica core-shell nanoparticles for one-step preparation of superhydrophobic surfaces.

    PubMed

    Liang, Junyan; Wang, Li; He, Ling; Sun, Shaodong

    2013-07-14

    Two poly(4-vinylpyridine)-b-polystyrene diblock copolymer/silica core-shell nanoparticles (P4VP-b-PS/SiO2 NPs) are developed in this work. Confirmed by DLS analysis and TEM observation, one comprises a SiO2 core surrounded by a P4VP-b-PS shell and the other comprises a P4VP-b-PS core surrounded by a SiO2 shell, which is facilely prepared by the in situ hydrolysis of tetraethyl orthosilicate (TEOS) using cationic P4VP-b-PS micelles obtained in a THF-H2C2O4 (aq, 0.1 mol L(-1)) mixture and a DMF-H2C2O4 (aq, 0.01 mol L(-1)) mixture as template, respectively. The SCA, CAH, SA and SEM measurements reveal that one-step deposition of P4VP-b-PS/SiO2 NPs with SiO2 cores formed at a high level of TEOS creates a superhydrophobic surface with an SCA of 160°, a CAH of 2° and an SA of around 4° originating from the formation of a typical micro-nanoscale binary structure (MNBS). For the NPs with SiO2 cores formed at a low level of TEOS, the superhydrophobicity with a SCA of 151°, CAH of 3° and SA of around 5° can be induced by the transition of the surface microstructure from an uneven and discontinuous MNBS, created by a one-step deposition process, to the coexistence of MNBS and a nanoscale structure (NS) after annealing with toluene for 30 min. In contrast, one-step deposition of P4VP-b-PS/SiO2 NPs with P4VP-b-PS cores and SiO2 shells usually results in the inhomogeneous precipitation of SiO2 from bulk P4VP-b-PS along with the production of micro-cracks, with which is impossible to achieve surface superhydrophobicity.

  10. Preparation of aqueous colloidal mesostructured and mesoporous silica nanoparticles with controlled particle size in a very wide range from 20 nm to 700 nm

    NASA Astrophysics Data System (ADS)

    Yamada, Hironori; Urata, Chihiro; Ujiie, Hiroto; Yamauchi, Yusuke; Kuroda, Kazuyuki

    2013-06-01

    Particle size control of colloidal mesoporous silica nanoparticles (CMPS) in a very wide range is quite significant for the design of CMPS toward various applications, such as catalysis and drug delivery. Various types of CMPS and their precursors (colloidal mesostructured silica nanoparticles (CMSS)) with different particle sizes (ca. 20-700 nm) were newly prepared from tetraalkoxysilanes with different alkoxy groups (Si(OR)4, R = Me, Et, Pr, and Bu) in the presence of alcohols (R'OH, R' = Me, Et, Pr, and Bu) as additives. CMSS with larger particle size were obtained by using tetrabutoxysilane (TBOS) and by increasing the amount of BuOH, which is explained by both the difference in the hydrolysis rates of tetraalkoxysilanes themselves and the effect of added alcohols on the hydrolysis rates of tetraalkoxysilanes. Larger amounts of alcohols with longer alkyl chains decrease the hydrolysis rates of tetraalkoxysilanes and the subsequent formation rates of silica species. Thus, the preferential particle growth of CMSS to nucleation occurs, and larger CMSS are formed. Highly dispersed CMPS were prepared by the removal of surfactants of CMSS by dialysis which can lead to the preparation of CMPS without aggregation. Therefore, the particle size control through the tuning of the hydrolysis rate of tetraalkoxysilanes can be conducted by a one-pot and easy approach. Even larger CMPS (ca. 700 nm in size) show relatively high dispersibility. This dispersibility will surely contribute to the design of materials both retaining nanoscale characteristics and avoiding various nanorisks.Particle size control of colloidal mesoporous silica nanoparticles (CMPS) in a very wide range is quite significant for the design of CMPS toward various applications, such as catalysis and drug delivery. Various types of CMPS and their precursors (colloidal mesostructured silica nanoparticles (CMSS)) with different particle sizes (ca. 20-700 nm) were newly prepared from tetraalkoxysilanes with

  11. Pressure induced swelling in microporous materials

    DOEpatents

    Vogt, Thomas; Hriljac, Joseph A.; Lee, Yongjae

    2006-07-11

    A method for capturing specified materials which includes contacting a microporous material with a hydrostatic fluid having at least one specified material carried therein, under pressure which structurally distorts the lattice sufficiently to permit entry of the at least one specified material. The microporous material is capable of undergoing a temporary structural distortion which alters resting lattice dimensions under increased ambient pressure and at least partially returning to rest lattice dimensions when returned to ambient pressure. The pressure of the fluid is then reduced to permit return to at least partial resting lattice dimension while the at least one specified material is therein. By this method, at least one specified material is captured in the microporous material to form a modified microporous material.

  12. Fabrication of bulk-modified carbon paste electrode containing alpha-PW12O40(3-) polyanion supported on modified silica gel: Preparation, electrochemistry and electrocatalysis.

    PubMed

    Hamidi, Hassan; Shams, Esmaeil; Yadollahi, Bahram; Esfahani, Farhad Kabiri

    2008-01-15

    Alpha-PW(12)O(40)(3-) (PW(12)) supported on the surface of silica gel derivatized by 3-aminopropyl(triethoxy)silane (devoted briefly as SiNH(3)PW(12)) was synthesized and used as bulk modifier to fabricate a renewable three-dimensional chemically modified electrode. The electrochemical behavior of the modified electrode was characterized by cyclic voltammetry. There is an ionic bonding character between PW(12) and the surface amino groups of modified silica, which greatly improves the stability of SiNH(3)PW(12)-modified carbon paste electrode due to insolubility of silica gel in water. The SiNH(3)PW(12) bulk-modified carbon paste electrode not only maintains the electrochemical activity of PW(12), but also exhibits remarkable advantages of renewability, as well as simple preparation and inexpensive material. The modified electrode offers an excellent and stable electrocatalytic response for the reduction of IO(3)(-) and hydrogen peroxide. The SiNH(3)PW(12)-CPE is successfully applied as an electrochemical detector to monitor IO(3)(-) in flow injection analysis (FIA). The catalytic peak current was found to be linear with the IO(3)(-) concentration in the range 5x10(-6) to 1x10(-3)molL(-1). The detection limit of the proposed method was found to be 3.1x10(-6)molL(-1) for IO(3)(-) determination.

  13. Filtration performance of microporous ceramic supports.

    PubMed

    Belouatek, Aissa; Ouagued, Abdellah; Belhakem, Mustapha; Addou, Ahmed

    2008-04-24

    The use of inorganic membranes in pollution treatment is actually limited by the cost of such membranes. Advantages of inorganic membranes are their chemical, thermal and pH properties. The purpose of this work was the development of microporous ceramic materials based on clay for liquid waste processing. The supports or ceramic filters having various compositions were prepared and thermally treated at 1100 degrees C. The results show that, at the temperature studied, porosity varied according to the support composition from 12% for the double-layered (ceramic) support to 47% for the activated carbon- filled support with a mean pore diameter between 0.8 and 1.3 microm, respectively. Volumes of 5 l of distilled water were filtered tangentially for 3 h under an applied pressure of 3.5 and 5.5 bar. The retention of tubular supports prepared was tested with molecules of varying size (Evans blue, NaCl and Sacharose). The study of the liquid filtration and flow through these supports showed that the retention rate depends on support composition and pore diameter, and solute molecular weight. The S1 support (mixture of barbotine and 1% (w/w) activated carbon) gave a flux for distilled water of 68 L/m2 h while the double-layered support resulted in a flux of 8 L/m2 h for the same solution at the pressure of 3.5 bar. At a pressure of 5.5 bar an increase in the distilled water flux through the various supports was observed. It was significant for the S1 support (230 L/m h).

  14. CO2 capture using zeolite 13X prepared from bentonite

    NASA Astrophysics Data System (ADS)

    Chen, Chao; Park, Dong-Wha; Ahn, Wha-Seung

    2014-02-01

    Zeolite 13X was prepared using bentonite as the raw material by alkaline fusion followed by a hydrothermal treatment without adding any extra silica or alumina sources. The prepared zeolite 13X was characterized by X-ray powder diffraction, N2-adsorption-desorption measurements, and scanning electron microscopy. The CO2 capture performance of the prepared zeolite 13X was examined under both static and flow conditions. The prepared zeolite 13X showed a high BET surface area of 688 m2/g with a high micropore volume (0.30 cm3/g), and exhibited high CO2 capture capacity (211 mg/g) and selectivity to N2 (CO2/N2 = 37) at 25 °C and 1 bar. In addition, the material showed fast adsorption kinetics, and stable CO2 adsorption-desorption recycling performance at both 25 and 200 °C.

  15. A simple and convenient approach for preparing core-shell-like silica@nickel species nanoparticles: highly efficient and stable catalyst for the dehydrogenation of 1,2-cyclohexanediol to catechol.

    PubMed

    Chen, Bao-Hui; Liu, Wei; Li, An; Liu, Ya-Juan; Chao, Zi-Sheng

    2015-01-21

    A simple and convenient approach denoted as gel-deposition-precipitation (G-D-P) for the preparation of core-shell-like silica@nickel species nanoparticles was studied systematically. Core-shell-like silica@nickel species nanoparticles consisted of a Si-rich core and a Ni-rich shell. The G-D-P process included two steps: one was the deposition-precipitation of nickel over the gelled colloidal silica particle, generating core-shell-like silica@nickel species nanoparticles, and the other was the aging period. It was found that the nickel phyllosilicate layer was formed mainly during the aging period and served as the protective cover to resist against aggregation of the nanoparticles, which could be utilized for regulating the dispersion of nickel over the silica@nickel species nanoparticles. In the present paper, the silica@nickel species nanoparticles were used as the catalysts for preparing catechol via dehydrogenation of 1,2-cyclohexanediol. Their catalytic activity and long-term stability were compared to those of a catalyst prepared by a conventional deposition-precipitation (D-P) approach. The higher activity and better stability of the title reaction over the silica@nickel species nanoparticles catalyst prepared by G-D-P than those over the catalyst prepared by D-P could be due to the higher dispersion of metallic nickel stabilized by the layers of nickel phyllosilicates. Moreover, it was found that the dehydrogenation of 1,2-cyclohexanediol to catechol was a structurally sensitive reaction.

  16. Microporous polyurethane material for size selective heterogeneous catalysis of the Knoevenagel reaction.

    PubMed

    Dey, Sandeep Kumar; de Sousa Amadeu, Nader; Janiak, Christoph

    2016-06-14

    The first polyurethane material which is microporous (BET surface area of 312 m(2) g(-1)) is prepared by solvothermal synthesis and acts as highly efficient and recyclable heterogeneous catalyst in the Knoevenagel condensation showing size selectivity, and in the Henry reaction showing substrate selectivity under mild reaction conditions.

  17. C18 silica packed capillary columns with monolithic frits prepared with UV light emitting diode: usefulness in nano-liquid chromatography and capillary electrochromatography.

    PubMed

    D'Orazio, Giovanni; Fanali, Salvatore

    2012-04-06

    In this paper the potential of fused silica capillaries packed with RP18 silica particles entrapped with monolithic frits using both nano-liquid chromatography (nano-LC) and capillary electrochromatography (CEC) was investigated. Frits were prepared after removing a short part of the polyimide layer on the capillary wall and irradiating the polymerization mixture with an UV-light emitter diode (LED) at 370 nm. The capillary, was rotated during the polymerization procedure in order to obtain a homogeneous monolith. The distance of the LED from the capillary and the exposure time to UV light were studied in order to obtain frits with good porosity and high robustness. A mixture containing five alkylbenzenes was selected as sample and analyzed by both nano-LC and CEC. The standard mixture was baseline separated with good efficiency in the range 78,000-93,000 and 99,000-113,000 plates/m in nano-LC and CEC, respectively. The columns resulted to be very robust and the prepared monolithic frits allowed working with backpressure as high as 400 bar (nano-LC). In addition high voltages were applied in CEC (25-30 kV) without bubbles formation in absence of pressure assistance during runs.

  18. Preparation and characterization - including in situ Small Angle X-Ray Scattering - of gas chromatographic capillary columns with mesoporous silica thin films as stationary phases.

    PubMed

    Lefebvre, D; Rayes, R Sayah-El; Jousseaume, V; Maret, M; Veyre, L; Charleux, B; Thieuleux, C; Ricoul, F

    2015-09-25

    In this study the preparation of various mesoporous silica thin films as new stationary phases for gas chromatography (GC) columns is presented. The synthesis was performed inside capillaries via a sol-gel process using a templating route. The as-obtained columns were found to be highly efficient for the fast separation of light n-alkanes (C1-C5) mixture; these columns exhibiting a normalized retention 30 times higher than that of a commercially available silica column used as standard. A particular effort was directed towards the characterization of the stationary phase physical features: thin film inspection by Scanning Electron Microscopy and, for the first time to our knowledge, in situ SAXS characterization using synchrotron radiation were used to study the impact of the pore-network structuration on the GC properties. Worm-like, cubic and hexagonal phases were observed for specific preparation conditions. Unexpectedly, the normalized retention relative to film thickness appeared higher with disordering of the pores network.

  19. Preparation of magnetic photocatalyst nanoparticles—TiO{sub 2}/SiO{sub 2}/Mn–Zn ferrite—and its photocatalytic activity influenced by silica interlayer

    SciTech Connect

    Laohhasurayotin, Kritapas; Pookboonmee, Sudarat; Viboonratanasri, Duangkamon; Kangwansupamonkon, Wiyong

    2012-06-15

    Highlights: ► TiO{sub 2}/SiO{sub 2}/Mn–Zn ferrite acts as magnetic photocatalyst nanoparticle. ► SiO{sub 2} interlayer is used to prevent electron migration between photocatalyst and magnetic core. ► TiO{sub 2}/Mn–Zn ferrite without SiO{sub 2} interlayer shows poor magnetic and photocatalytic property. -- Abstract: A magnetic photocatalyst, TiO{sub 2}/SiO{sub 2}/Mn–Zn ferrite, was prepared by stepwise synthesis involving the co-precipitation of Mn–Zn ferrite as a magnetic core, followed by a coating of silica as the interlayer, and titania as the top layer. The particle size and distribution of magnetic nanoparticles were found to depend on the addition rate of reagent and dispersing rate of reaction. The X-ray diffractometer and transmission electron microscope were used to examine the crystal structures and the morphologies of the prepared composites. Vibrating sample magnetometer was also used to reveal their superparamagnetic property. The UV–Vis spectrophotometer was employed to monitor the decomposition of methylene blue in the photocatalytic efficient study. It was found that at least a minimum thickness of the silica interlayer around 20 nm was necessary for the inhibition of electron transference initiated by TiO{sub 2} and Mn–Zn ferrite.

  20. Preparation and Characterization of Sulfonic Acid Functionalized Silica and Its Application for the Esterification of Ethanol and Maleic Acid

    NASA Astrophysics Data System (ADS)

    Sirsam, Rajkumar; Usmani, Ghayas

    2016-04-01

    The surface of commercially available silica gel, 60-200 mesh size, was modified with sulfonic acid through surface activation, grafting of 3-Mercaptopropyltrimethoxysilane, oxidation and acidification of 3-Mercaptopropylsilica. Sulfonic Acid Functionalization of Silica (SAFS) was confirmed by Fourier Transform Infra-red (FTIR) spectroscopy and thermal gravimetric analysis. Acid-base titration was used to estimate the cation exchange capacity of the SAFS. Catalytic activity of SAFS was judged for the esterification of ethanol with maleic acid. An effect of different process parameters viz. molar ratio, catalyst loading, speed of agitation and temperature were studied and optimized by Box Behnken Design (BBD) of Response Surface Methodology (RSM). Quadratic model developed by BBD-RSM reasonably satisfied an experimental and predicted values with correlation coefficient value R2 = 0.9504.

  1. Unique Separation Behavior of a C60 Fullerene-Bonded Silica Monolith Prepared by an Effective Thermal Coupling Agent.

    PubMed

    Kubo, Takuya; Murakami, Yoshiki; Tsuzuki, Madoka; Kobayashi, Hiroshi; Naito, Toyohiro; Sano, Tomoharu; Yan, Mingdi; Otsuka, Koji

    2015-12-07

    Herein, we report a newly developed C60 fullerene-bonded silica monolith in a capillary with unique retention behavior due to the structure of C60 fullerene. N-Hydroxysuccinimide (NHS)-conjugated C60 fullerene was successfully synthesized by a thermal coupling agent, perfluorophenyl azide (PFPA), and assigned by spectroscopic analyses. Then, NHS-PFPA-C60 fullerene was attached onto the surface of a silica monolith in a capillary. The capillary provided specific separation ability for polycyclic aromatic hydrocarbons in liquid chromatography by an effective π-π interaction. Furthermore, corannulene, which has a hemispherical structure, was selectively retained in the capillary based on the specific structural recognition due to the spherical C60 fullerene. This is the first report revealing the spherical recognition ability by C60 fullerene in liquid chromatographic separation.

  2. New Method for Development of Carbon Coated Silica Phases for Liquid Chromatography Part I. Preparation of Carbon Phases

    PubMed Central

    Paek, Changyub; McCormick, Alon V.; Carr, Peter W.

    2011-01-01

    Owing to its combination of unique selectivity and mechanical strength, commercial carbon clad zirconia (C/ZrO2) has been widely used for many applications, including fast two-dimensional liquid chromatography (2DLC). However, the low surface area available (only 20 - 30 m2/g for commercial porous ZrO2) limits its retentivity. We have recently addressed this limitation by developing a carbon phase coated on the high surface area of HPLC grade alumina (C/Al2O3). This material provides higher retentivity and comparable selectivity, but its use is still limited by how few HPLC quality types of alumina particles (e.g., particle size, surface area, pore size) are available. In this work, we have developed useful carbon phases on silica particles, which are available in various particle sizes, pore sizes and forms of HPLC grade. To make the carbon phase on silica, we first treat the silica surface with a monolayer or less of metal cations that bind to deprotonated silanols to provide catalytic sites for carbon deposition. After Al (III) treatment, a carbon phase is formed on the silica surface by chemical vapor deposition at 700 °C using hexane as the carbon source. The amount of Al (III) on the surface was varied to assess its effect on carbon deposition, and the carbon loading was varied at different Al (III) levels to assess its effect on the chromatographic properties of the various carbon adsorbents. We observed that use of a concentration of Al (III) corresponding to a full monolayer leads to the most uniform carbon coating. A carbon coating sufficient to cover all the Al (III) sites, required about 4 – 5 monolayers in this work, provided the best chromatographic performance. The resulting carbon phases behave as reversed phases with reasonable efficiency (50,000 – 79,000 plates/meter) for non-aromatic test species. PMID:21295308

  3. Application of graphene nanoplatelets silica composite, prepared by sol-gel technology, as a novel sorbent in two microextraction techniques.

    PubMed

    Heidari, Mahmoud; Bahrami, Abdolrahman; Ghiasvand, Ali Reza; Shahna, Farshid Ghorbani; Soltanian, Ali Reza; Rafieiemam, Maryam

    2015-12-01

    In this study, the application of a novel nanomaterial composite was investigated in two microextraction techniques of solid-phase microextraction and a needle trap device in a variety of sampling conditions. The optimum sampling temperature and relative humidity were 10°C and 20%, respectively, for both techniques with two sorbents of graphene/silica composite and polydimethyl siloxane. The two microextraction techniques with the proposed sorbent showed recoveries of 95.2 and 94.6% after 7 days. For the needle trap device the optimums desorption time and temperature were 3 min at 290°C and for SPME these measures were 1 and 1.5 min at 240-250°C for the graphene/silica composite and polydimethyl siloxane, respectively. The relative standard division obtained in inter- and intra-day comparative studies were 3.3-14.3 and 5.1-25.4, respectively. For four sample the limit of detection was 0.021-0.25 ng/mL, and the limit of quantitation was 0.08-0.75 ng/mL. The results show that the graphene/silica composite is an appropriate extraction media for both techniques. Combining an appropriate sorbent with microextraction techniques, and using these in conjunction with a sensitive analytical instrument can introduce a strong method for sampling and analysis of occupational and environmental pollutants in air.

  4. Preparation and characterization of gold nanoparticles and nanowires loaded into rod-shaped silica by a one-step procedure

    NASA Astrophysics Data System (ADS)

    Mnasri, Najib; Nyalosaso, Jeff L.; Kachbouri, Sana; Zajac, Jerzy; Elaloui, Elimame; Charnay, Clarence

    2017-01-01

    Rod-shaped mesoporous silica nanoparticles (RMSN) with built-in gold nanoparticles or thin gold nanowires in the pore channels were in situ synthesized via a one-step procedure. The insertion of a hydrophobic gold precursor into the mesopores of RMSN was reached through a micellar solubilization mechanism and gold nanoparticles were achieved through a thermal reduction. The resulting RMSN and Au-RMSN samples were characterized by using X-ray diffraction, transmission and scanning microscopies (TEM and SEM), X-ray photoelectron spectroscopy (XPS), nitrogen physisorption and solid-state Nuclear Magnetic Resonance (NMR). The interaction of Au precursor (a carbene complex) with the thiol group at the silica surface was identified and found to play a crucial role in the dispersion of the uniform metal nanoparticles at the internal surface of RMSN. Moreover, TEM micrographs revealed the absence of large gold particles outside the mesopore network. The shape of Au nanoparticles and their loading amount in the mesoporous silica could be easily tuned by altering the concentration of gold precursor.

  5. Hierarchical mesoporous/microporous carbon with graphitized frameworks for high-performance lithium-ion batteries

    SciTech Connect

    Lv, Yingying; Fang, Yin; Qian, Xufang; Tu, Bo; Wu, Zhangxiong; Asiri, Abdullah M.; Zhao, Dongyuan

    2014-11-01

    A hierarchical meso-/micro-porous graphitized carbon with uniform mesopores and ordered micropores, graphitized frameworks, and extra-high surface area of ∼2200 m{sup 2}/g, was successfully synthesized through a simple one-step chemical vapor deposition process. The commercial mesoporous zeolite Y was utilized as a meso-/ micro-porous template, and the small-molecule methane was employed as a carbon precursor. The as-prepared hierarchical meso-/micro-porous carbons have homogeneously distributed mesopores as a host for electrolyte, which facilitate Li{sup +} ions transport to the large-area micropores, resulting a high reversible lithium ion storage of 1000 mA h/g and a high columbic efficiency of 65% at the first cycle.

  6. Highly Monodisperse Microporous Polymeric and Carbonaceous Nanospheres with Multifunctional Properties

    PubMed Central

    Ouyang, Yi; Shi, Huimin; Fu, Ruowen; Wu, Dingcai

    2013-01-01

    Fabrication of monodisperse porous polymeric nanospheres with diameters below 500 nm remains a great challenge, due to serious crosslinking between neighboring nanospheres during pore-making process. Here we show how a versatile hypercrosslinking strategy can be used to prepare monodisperse microporous polystyrene nanospheres (MMPNSs) with diameters as low as ca. 190 nm. In our approach, an unreactive crosslinked PS outer skin as protective layer can be in-situ formed at the very beginning of hypercrosslinking treatment to minimize the undesired inter-sphere crosslinking. The as-prepared MMPNSs with a well-developed microporous network demonstrate unusual multifunctional properties, including remarkable colloidal stability in aqueous solution, good adsorption-release property for drug, and large adsorption capacity toward organic vapors. Surprisingly, MMPNSs can be directly transformed into high-surface-area monodisperse carbon nanospheres with good colloidal stability via a facile hydrothermal-assisted carbonization procedure. These findings provide a new benchmark for fabricating well-defined porous nanospheres with great promise for various applications. PMID:23478487

  7. Core–shell Ag@SiO{sub 2} nanoparticles of different silica shell thicknesses: Preparation and their effects on photoluminescence of lanthanide complexes

    SciTech Connect

    Kang, Jie; Li, Yuan; Chen, Yingnan; Wang, Ailing; Yue, Bin; Qu, Yanrong; Zhao, Yongliang; Chu, Haibin

    2015-11-15

    Highlights: • Ag@SiO{sub 2} nanoparticles of different silica shell thicknesses were prepared via the Stöber process. • Sm and Dy complexes with benzoate, 1,10-phenanthroline and 2,2′-bipyridine were synthesized. • The complex-doped Ag@SiO{sub 2} composites show stronger luminescent intensities than pure complexes. • The luminescent intensities of the composites strongly depend on the SiO{sub 2} shell thickness. - Abstract: Three kinds of almost spherical core–shell Ag@SiO{sub 2} nanoparticles of different silica shell thicknesses (10, 25 and 80 nm) were prepared via the Stöber process. The Ag core nanoparticles were prepared by reducing silver nitrate with sodium citrate. The size, morphology and structure of core–shell Ag@SiO{sub 2} nanoparticles were characterized by transmission electron microscopy. Subsequently, eight kinds of lanthanide complexes with benzoate, 1,10-phenanthroline and 2,2′-bipyridine were synthesized. The composition of the lanthanide complexes was characterized by elemental analysis, IR and UV spectra. Finally, lanthanide complexes were attached to the surface of Ag@SiO{sub 2} nanoparticles to form lanthanide-complex-doped Ag@SiO{sub 2} nanocomposites. The results show that the complex-doped Ag@SiO{sub 2} nanocomposites display much stronger luminescence intensities than the lanthanide complexes. Furthermore, the luminescence intensities of the lanthanide-complex-doped Ag@SiO{sub 2} nanocomposites with SiO{sub 2} shell thickness of 25 nm are stronger than those of the nanocomposites with SiO{sub 2} shell thickness of 10 and 80 nm.

  8. Activation of the Solid Silica Layer of Aerosol-Based C/SiO₂ Particles for Preparation of Various Functional Multishelled Hollow Microspheres.

    PubMed

    Li, Xiangcun; Luo, Fan; He, Gaohong

    2015-05-12

    Double-shelled C/SiO2 hollow microspheres with an outer nanosheet-like silica shell and an inner carbon shell were reported. C/SiO2 aerosol particles were synthesized first by a one-step rapid aerosol process. Then the solid silica layer of the aerosol particles was dissolved and regrown on the carbon surface to obtain novel C/SiO2 double-shelled hollow microspheres. The new microspheres prepared by the facile approach possess high surface area and pore volume (226.3 m(2) g(-1), 0.51 cm(3) g(-1)) compared with the original aerosol particles (64.3 m(2) g(-1), 0.176 cm(3) g(-1)), providing its enhanced enzyme loading capacity. The nanosheet-like silica shell of the hollow microspheres favors the fixation of Au NPs (C/SiO2/Au) and prevents them from growing and migrating at 500 °C. Novel C/C and C/Au/C (C/Pt/C) hollow microspheres were also prepared based on the hollow nanostructure. C/C microspheres (482.0 m(2) g(-1), 0.92 cm(3) g(-1)) were ideal electrode materials. In particular, the Au NPs embedded into the two carbon layers (C/Au/C, 431.2 m(2) g(-1), 0.774 cm(3) g(-1)) show a high catalytic activity and extremely chemical stability even at 850 °C. Moreover, C/SiO2/Au, C/Au/C microspheres can be easily recycled and reused by an external magnetic field because of the presence of Fe3O4 species in the inner carbon shell. The synthetic route reported here is expected to simplify the fabrication process of double-shelled or yolk-shell microspheres, which usually entails multiple steps and a previously synthesized hard template. Such a capability can facilitate the preparation of various functional hollow microspheres by interfacial design.

  9. Preparation and evaluation of monodispersed, submicron, non-porous silica particles functionalized with β-CD derivatives for chiral-pressurized capillary electrochromatography.

    PubMed

    Yangfang, Lu; Hui, Wang; Yun, Xue; Xue, Gu; Yan, Wang; Chao, Yan

    2015-09-01

    Submicron, non-porous, chiral silica stationary phase has been prepared by the immobilization of functionalized β-CD derivatives to isocyanate-modified silica via chemical reaction and applied to the pressurized capillary electrochromatography (pCEC) enantio-separation of various chiral compounds. The submicron, non-porous, cyclodextrin-based chiral stationary phases (sub_μm-CSP2) exhibited excellent chiral recognition of a wide range of analytes including clenbuterol hydrochloride, mexiletine hydrochloride, chlorpheniramine maleate, esmolol hydrochloride, and metoprolol tartrate. The synthesized submicron particles were regularly spherical and uniformly non-porous with an average diameter of around 800 nm and a mean pore size of less than 2 nm. The synthesized chiral stationary phase was packed into 10 cm × 100 μm id capillary columns. The sub_μm-CSP2 column used in the pCEC system showed better separation of the racemates and at a higher rate compared to those used in the capillary liquid chromatography mode (cLC) system. The sub_μm-CSP2 possessed high mechanical strength, high stereoselectivity, and long lifespan, demonstrating rapid enantio-separation and good resolution of samples. The column provided an efficiency of up to 170,000 plates/m for n-propylbenzene.

  10. Preparation and evaluation of o-phenanthroline immobilized on a hybrid silica monolith modified with ionic liquids for reversed-phase pressurized capillary electrochromatography.

    PubMed

    Qin, Wenfei; Lü, Haixia; Xie, Zenghong

    2014-12-01

    A novel o-phenanthroline-immobilized ionic-liquid-modified hybrid monolith for capillary electrochromatography was synthesized based on chloropropyl-silica, which was prepared by the in situ polymerization of tetramethoxysilane and 3-chloropropyltrimethoxysilane via a sol-gel process. The morphology of the hybrid monolith was characterized by scanning electron microscopy, and relatively stable anodic electroosmotic flow was observed under a broad pH ranged from pH 3.0 to 9.0. The separation mechanism was investigated by separating four neutral molecules (toluene, dimethylformamide, formamide, and thiourea). The obtained hybrid monolith possessed an obviously reversed-phase retention mechanism, but when the acetonitrile content in the mobile phase was >90% v/v, a weak hydrophilic mechanism was observed on the resultant o-phenanthroline-modified chloropropyl-silica hybrid monolith. The reproducibility of the column was also investigated by measuring relative standard deviations of the migration time for four neutral molecules. Relative standard deviations of run to run (n = 3), day to day (n = 3), and column to column (n = 3) were in the range of 0.4-0.7, 0.9-2.1, and 1.4-3.3%, respectively. Basic separations of various polar analytes including phenols and aromatic amines were successfully achieved.

  11. Preparation of xylenol orange functionalized silica gel as a selective solid phase extractor and its application for preconcentration--separation of mercury from waters.

    PubMed

    Fan, Jing; Wu, Chunlai; Wei, Yafang; Peng, Chuanyun; Peng, Pingan

    2007-06-25

    A new selective solid phase extractor was prepared from silica gel modified with xylenol orange (SGMXO). The solid phase extractor is stable in 6molL(-1) HCl, common organic solvents, and pH 1.0-9.0 buffer solutions. In the batch experiments, Hg(II) can be adsorbed on SGMXO at pH 1.0 with 90.0% retention, whereas the retention of other common coexisting metal ions such as Cd(II), Pb(II), Cu(II), Ni(II), Co(II), Mn(II), Zn(II), and Fe(III) is less than 4.1%.. The adsorption equilibration for Hg(II) was achieved within 3min. At optimum conditions, the adsorption capacity of the extractor is 18.26micromolg(-1) of dry modified silica gel, and the preconcentration factor is as high as 333. The recovery is still higher than 95% for the preconcentration of 10ngmL(-1) Hg(II). The new solid phase extractor has been used for the preconcentration of low level of Hg(II) in surface water, tap water in chemistry laboratory and student's dormitory and a simulated sea water samples, recoveries of 98.2-100.6% were obtained. It is showed that low level of Hg(II) can be effectively preconcentrated by this new selective solid phase extractor.

  12. Preparation and kinetic performance assessment of thick film 10-20 μm open tubular silica capillaries in normal phase high pressure liquid chromatography.

    PubMed

    Forster, Simon; Kolmar, Harald; Altmaier, Stephan

    2013-11-08

    It is well-known that the open tubular column design basically can offer very high plate numbers. Experimental realization has however not kept pace with theoretical considerations, lacking efficient methods for the deposition of a thick film porous layer within a microbore capillary. A previously published sol-gel synthesis method was extended from 20 μm to 10 μm inner diameter fused silica capillaries and the resulting columns were compared to a monolithic reference capillary in terms of kinetic performance at pressure maximum. Column permeability was investigated and pressure/flow-diagrams were obtained with a 400-fold permeability gain for the open tubes. Structural characterizations regarding layer thickness and surface porosity were carried out and displayed via scanning electron microscopy and nitrogen sorption analysis. Chromatographic results in normal phase mode at elevated mobile phase flow rate reveal the intrinsic performance potential of this column format when it comes to kinetic performance limitation plots, which were constructed for all columns prepared and compared to the monolithic silica reference capillary.

  13. Preparation of Dufulin imprinted polymer on surface of silica gel and its application as solid-phase extraction sorbent.

    PubMed

    Miao, Shan Shan; Wang, Hua Zi; Lu, Yi Chen; Geng, Hao Ran; Yang, Hong

    2014-04-01

    A new molecularly imprinted polymer (MIP) based on silica-gel surface was developed using Dufulin (Duf) as a template, methacrylic acid (MAA) as a functional monomer, ethyleneglycol dimethacrylate (EGDMA) as a crosslinker, and azodiisobutyronitrile (AIBN) as an initiator. The synthetic samples were characterized by the techniques of Fourier transmission infrared spectrometry (FT-IR) and scanning electron microscope (SEM). Batch experiments were performed to evaluate adsorption isotherms, adsorption kinetics and selective recognition of the MIP. Binding experiments demonstrated that the MIP had a good adsorption capacity, fast mass transfer rate and high recognition selectivity to Dufulin. When the MIP was used as a solid-phase extraction (SPE) material, the recoveries of Dufulin for spiked water, soil and wheat samples were 88.98-102.16%, 85.31-99.57% and 87.84-100.19%, along with LOD of 0.0008 mg L(-1), 0.010 mg kg(-1) and 0.023 mg kg(-1), respectively. Compared with direct determination of HPLC without MIP-SPE, the highly selective separation and enrichment of Dufulin from the complex environmental media can be achieved by the newly developed molecular imprinting at the surface of silica gel.

  14. Preparation, characterization and luminescent properties of dense nano-silica hybrids loaded with 1,8-naphthalic anhydride.

    PubMed

    Wang, Jinpeng; Sun, Jihong; Li, Yuzhen; Wang, Feng

    2014-03-01

    Novel luminescent dense nano-silica hybrid materials (DNSS) modified with different amounts of (3-aminopropyl)triethoxysilane (APTES) and 1,8-naphthalic anhydride (NA) were successfully synthesized via two steps combined with post-grafting methods. Powder X-ray diffraction (XRD), N2-sorption analysis, Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), thermogravimetric analysis (TGA), photoluminescence (PL) spectroscopy and elemental analysis, as well as time-resolved decays were employed to characterize the resultant hybrid materials. The results revealed that luminescent organic molecules had been successfully loaded onto the amine-modified surface of nano-silica spheres. In addition, their fluorescence intensity and characteristic peak of emission spectra changed with increasing amount of APTES and NA additive. In particular, the characteristic peak showed a red shift from 390 to 450 nm, however, this was inconsistent with results calculated on the basis of the elemental analysis data, most probably because of the dispersion behaviors of NA molecules from the aggregating to the monolayer state. These observations demonstrated the existence of a quantum confinement effectiveness of NA-DNSS samples, and therefore a possible mechanism was put forward.

  15. Preparation of poly(acrylic)/SiO2/EuL3 x 2H2O, hybrid thin films from monodispersed colloidal silica.

    PubMed

    Chien, Wen-Chen; Yu, Yang-Yen; Chen, Shih-Yu; Yang, Chang-Chung

    2010-08-01

    In this study, poly(acrylic)/SiO2/EuL3 x 2H2O hybrid thin films were prepared from various acrylic monomers (MMA and EDMA/TMPTA), lanthanide metal complexes (EuL3 x 2H2O, L = pyridine carboxylic acid), and monodispersed colloidal silica with a coupling agent, 3-(trimethoxysilyl)propyl methacrylate (MSMA). It is a combination of the sol-gel reaction, thermal polymerization, and spin coating. The silica content in the hybrid thin films is fixed at 20 wt%, and the EuL3 x 2H2O content is varied from 0.01 g to 0.07 g. FTIR and EA analysis confirms the chemical structure of the prepared EuL3 x 2H2O and poly(acrylic)/SiO2/EuL3 x 2H2O hybrid thin films. UV-Vis spectra and n&k analysis shows that the hybrid thin film has good transparency in visible light. The refractive index of hybrid thin films can be effectively controlled through the EuL3 x 2H2O content. The PL spectra shows that the strongest emission peak occurs at 615 nm and the emission intensity increases to the peak maximum at an EuL3 x 2H2O content of 0.05 g. Both TGA and PL analysis show that the prepared hybrid thin films from the crosslinked acrylic polymer moiety have much better film uniformity, thermal stability, and fluorescence properties. The TEM diagram shows that the MSMA/SiO2/EuL3 x 2H2O particles with a size 15-20 nm are well dispersed in the reaction solution. The SEM diagram shows that the particle distribution in the prepared hybrid thin films is uniform and no phase separation is observed. Finally, AFM analysis indicates that the prepared hybrid thin films have an excellent surface planarity.

  16. Cellulose-silica aerogels.

    PubMed

    Demilecamps, Arnaud; Beauger, Christian; Hildenbrand, Claudia; Rigacci, Arnaud; Budtova, Tatiana

    2015-05-20

    Aerogels based on interpenetrated cellulose-silica networks were prepared and characterised. Wet coagulated cellulose was impregnated with silica phase, polyethoxydisiloxane, using two methods: (i) molecular diffusion and (ii) forced flow induced by pressure difference. The latter allowed an enormous decrease in the impregnation times, by almost three orders of magnitude, for a sample with the same geometry. In both cases, nanostructured silica gel was in situ formed inside cellulose matrix. Nitrogen adsorption analysis revealed an almost threefold increase in pores specific surface area, from cellulose aerogel alone to organic-inorganic composite. Morphology, thermal conductivity and mechanical properties under uniaxial compression were investigated. Thermal conductivity of composite aerogels was lower than that of cellulose aerogel due to the formation of superinsulating mesoporous silica inside cellulose pores. Furthermore, composite aerogels were stiffer than each of reference aerogels.

  17. Processing of CuAlMn Shape Memory Foams with Open Spherical Pores by Silica-Gel Beads Infiltration Method

    NASA Astrophysics Data System (ADS)

    Li, Hua; Yuan, Bin; Gao, Yan

    2016-10-01

    A molten metal infiltration process with amorphous SiO2 (silica-gel) beads as space holders was used to prepare Cu-based shape memory foams in this article. We found that the silica-gel beads with micropores inside expanded when being heated to elevated temperatures and that proper control of the expansion of silica-gel beads helped form necks between the beads with different bonding extent, which had been taken advantage of to have a good control of the foam morphology and porosity, by carefully designing suitable procedures and choosing proper parameters for the process. In addition, we studied in detail the effect of heating temperature, silica-gel bead density, and infiltration pressure of the present process on the morphology and porosity of CuAlMn shape memory foams. By coordinating these three key parameters, CuAlMn shape memory foams with open spherical pores and adjustable porosity from 66 to 85 pct were reliably produced.

  18. Lithographically defined microporous carbon-composite structures

    SciTech Connect

    Burckel, David Bruce; Washburn, Cody M.; Lambert, Timothy N.; Finnegan, Patrick Sean; Wheeler, David R.

    2016-12-06

    A microporous carbon scaffold is produced by lithographically patterning a carbon-containing photoresist, followed by pyrolysis of the developed resist structure. Prior to exposure, the photoresist is loaded with a nanoparticulate material. After pyrolysis, the nanonparticulate material is dispersed in, and intimately mixed with, the carbonaceous material of the scaffold, thereby yielding a carbon composite structure.

  19. Micropore extrusion-induced alignment transition from perpendicular to parallel of cylindrical domains in block copolymers

    NASA Astrophysics Data System (ADS)

    Qu, Ting; Zhao, Yongbin; Li, Zongbo; Wang, Pingping; Cao, Shubo; Xu, Yawei; Li, Yayuan; Chen, Aihua

    2016-02-01

    The orientation transition from perpendicular to parallel alignment of PEO cylindrical domains of PEO-b-PMA(Az) films has been demonstrated by extruding the block copolymer (BCP) solutions through a micropore of a plastic gastight syringe. The parallelized orientation of PEO domains induced by this micropore extrusion can be recovered to perpendicular alignment via ultrasonication of the extruded BCP solutions and subsequent annealing. A plausible mechanism is proposed in this study. The BCP films can be used as templates to prepare nanowire arrays with controlled layers, which has enormous potential application in the field of integrated circuits.The orientation transition from perpendicular to parallel alignment of PEO cylindrical domains of PEO-b-PMA(Az) films has been demonstrated by extruding the block copolymer (BCP) solutions through a micropore of a plastic gastight syringe. The parallelized orientation of PEO domains induced by this micropore extrusion can be recovered to perpendicular alignment via ultrasonication of the extruded BCP solutions and subsequent annealing. A plausible mechanism is proposed in this study. The BCP films can be used as templates to prepare nanowire arrays with controlled layers, which has enormous potential application in the field of integrated circuits. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr09140c

  20. Preparation of chitosan/mesoporous silica nanoparticle composite hydrogels for sustained co-delivery of biomacromolecules and small chemical drugs

    NASA Astrophysics Data System (ADS)

    Zhu, Min; Zhu, Yufang; Zhang, Lingxia; Shi, Jianlin

    2013-08-01

    We have developed composite hydrogels of chitosan (CS) and mesoporous silica nanoparticles (MSNs) in this study. The gelation rate, gel strength, drug delivery behavior and chondrocyte proliferation properties were investigated. The introduction of MSNs into CS accelerated the gelation process at body temperature and also increased the elastic modulus G‧ from 1000 to 1800 Pa. When we used gentamicin (GS) and bovine serum albumin (BSA) as model small chemical drugs and biomacromolecules, respectively, the CS/MSN hydrogels released GS and BSA in a sustained manner simultaneously, but the CS hydrogels only showed sustained BSA release. Furthermore, in vitro chondrocyte culture showed that the CS/MSN composite hydrogels indeed performed much better in supporting chondrocyte growth and maintaining chondrocytic phenotype compared to the CS hydrogels. Therefore, the results suggest that the CS/MSN composite hydrogels can be potentially very useful for cartilage regeneration.

  1. Preparation of magnetic nano-composite: barium hexaferrite loaded in the ordered meso-porous silica matrix (MCM-41).

    PubMed

    Emamian, H R; Honarbakhsh-Raouf, A; Ataie, A

    2010-04-01

    In this work a magnetic nano-composite was synthesized by modified incorporation of iron-barium complex into ordered meso-porous silica (MCM-41) as a matrix. The MCM-41 was synthesized by silylation treatment which was accompanied by pH adjusting. Low angle XRD patterns of both annealed MCM-41 and resulted composite exhibited the characteristic reflection of high quality hexagonal meso-structures. TEM image of the composite material revealed that the hexagonal ordered meso-structure host material was not affected by wet impregnation and subsequent calcination in order to incorporate with barium hexaferrite. Also, TEM images accompanied by EDS analysis confirmed the formation of second phase consists of barium and iron ions inside the MCM-41 channels. The resulted composite material showed a super-paramagnetic nature at room temperature.

  2. Preparation of submicrometer monodispersed magnetic silica particles using a novel water in oil microemulsion: properties and application for enzyme immobilization.

    PubMed

    Tuttolomondo, Maria Victoria; Villanueva, Maria Emilia; Alvarez, Gisela Solange; Desimone, Martín Federico; Díaz, Luis Eduardo

    2013-10-01

    The synthesis of monodispersed magnetic silica nanoparticles (MSN) is described using a water-in-oil reverse microemulsion system that does not require the use of co-surfactants. Sodium silicate, Tween 20 as a neutral surfactant and 1-butanol as the organic phase were used. There are several advantages of the proposed method including a saturation magnetization value of 10 emu/g for the particles obtained, uniformity of size and that they are easily functionalized to bind urease covalently. Moreover, the intra-day, inter-day and long-term stability results confirm that the procedure was successful and the enzyme-linked MSNs were stable over repeated uses and storage retaining more than 75% activity after 4 months.

  3. One-pot and efficient synthesis of triazolo[1,2-a]indazole-triones via reaction of arylaldehydes with urazole and dimedone catalyzed by silica nanoparticles prepared from rice husk.

    PubMed

    Hamidian, Hooshang; Fozooni, Samieh; Hassankhani, Asadollah; Mohammadi, Sayed Zia

    2011-10-26

    A novel synthesis of triazolo[1,2-a]indazole-1,3,8-trione derivatives by reaction of urazole, dimedone and aromatic aldehydes under conventional heating and microwave irradiation and solvent-free conditions using silica nanoparticles prepared from rice husk ash as catalyst is described. The new method features high yields, multicomponent reactions and environmental friendliness.

  4. Characteristics of ultra low-k nanoporous and fluorinated silica based films prepared by plasma enhanced chemical vapor deposition

    SciTech Connect

    Abbasi-Firouzjah, M.; Shokri, B.

    2013-12-07

    Low dielectric constant (low-k) silica based films were deposited on p-type silicon and polycarbonate substrates by radio frequency (RF) plasma enhanced chemical vapor deposition method at low temperature. A mixture of tetraethoxysilane vapor, oxygen, and tetrafluoromethane (CF{sub 4}) was used for the deposition of the films in forms of two structures called as SiO{sub x}C{sub y} and SiO{sub x}C{sub y}F{sub z}. Properties of the films were controlled by amount of porosity and fluorine content in the film matrix. The influence of RF power and CF{sub 4} flow on the elemental composition, deposition rate, surface roughness, leakage current, refractive index, and dielectric constant of the films were characterized. Moreover, optical emission spectroscopy was applied to monitor the plasma process at the different parameters. Electrical characteristics of SiO{sub x}C{sub y} and SiO{sub x}C{sub y}F{sub z} films with metal-oxide-semiconductor structure were investigated using current-voltage analysis to measure the leakage current and breakdown field, as well as capacitance-voltage analysis to obtain the film's dielectric constant. The results revealed that SiO{sub x}C{sub y} films, which are deposited at lower RF power produce more leakage current, meanwhile the dielectric constant and refractive index of these films decreased mainly due to the more porosity in the film structure. By adding CF{sub 4} in the deposition process, fluorine, the most electronegative and the least polarized atom, doped into the silica film and led to decrease in the refractive index and the dielectric constant. In addition, no breakdown field was observed in the electrical characteristics of SiO{sub x}C{sub y}F{sub z} films and the leakage current of these films reduced by increment of the CF{sub 4} flow.

  5. A dual-spatially-confined reservoir by packing micropores within dense graphene for long-life lithium/sulfur batteries

    NASA Astrophysics Data System (ADS)

    Li, Hongfei; Yang, Xiaowei; Wang, Xiaomin; He, Yu-Shi; Ye, Fangmin; Liu, Meinan; Zhang, Yuegang

    2016-01-01

    In lithium/sulfur batteries, micropores could bring about strong interactions with polysulfides, but could not alleviate the partial polysulfide overflowing outside because of the volume expansion of the lithiated sulfur. A dual-spatially-confined reservoir for sulfur by wrapping microporous carbon with dense graphene, micro@meso-porous DSC (dual-spatial carbon), is synthesized to solve this issue. Such a structure is prepared through two distinctive methods: graphene promoted in situ hydrothermal carbonization of organics to grow micropores on itself, and liquid mediated drying of graphene hydrogel to form mesoporous graphene frameworks. In contrast to previously reported hierarchical carbon/S, the inner micropores are mainly responsible for loading sulfur, which could help confine its particle size, thus increasing the electrical/ionic conductivity and the utilization of sulfur, and restrain lithium polysulfide dissolution because of strong interaction with pore walls; while the outer mesopores act as another reservoir to stabilize the overflowed polysulfide and to enhance the Li+ transport. The S-micro@meso-porous DSC cathode exhibits better discharge capacity and cycling performance than S-microporous AC and S-micro@macro-porous DSC, i.e., 59% and 37% higher capacity remaining at 0.5 C than the latter two, respectively.In lithium/sulfur batteries, micropores could bring about strong interactions with polysulfides, but could not alleviate the partial polysulfide overflowing outside because of the volume expansion of the lithiated sulfur. A dual-spatially-confined reservoir for sulfur by wrapping microporous carbon with dense graphene, micro@meso-porous DSC (dual-spatial carbon), is synthesized to solve this issue. Such a structure is prepared through two distinctive methods: graphene promoted in situ hydrothermal carbonization of organics to grow micropores on itself, and liquid mediated drying of graphene hydrogel to form mesoporous graphene frameworks. In

  6. Preparation and characterization of micro-cell membrane chromatographic column with silica-based porous layer open tubular capillary as cellular membrane carrier.

    PubMed

    Zhang, Fugeng; Zhao, Xinchao; Xu, Bei; Cheng, Shuai; Tang, Cheng; Duan, Hongquan; Xiao, Xuefeng; Du, Wuxun; Xu, Liang

    2016-04-01

    Cell membrane chromatography (CMC) is a powerful tool to study membrane protein interactions and to screen active compounds extracted from natural products. Unfortunately, a large amount of cells are typically required for column preparation in order to carry out analyses in an efficient manner. Micro-CMC (mCMC) has recently been developed by using a silica capillary as a membrane carrier. However, a reduced retention of analytes is generally associated with mCMC mostly due to a low ligand (cellular membrane) capacity. To solve this common problem, in this work a silica-based porous layer open tubular (PLOT) capillary was fabricated and, to the best of our knowledge, for the first time applied to mCMC. The mCMC column was prepared by physical adsorption of rabbit red blood cell (rRBC) membranes onto the inner surface of the PLOT capillary. The effects of the PLOT capillaries fabricated by different feed compositions, on the immobilization amount of cellular membranes (represented by the fluorescence intensity of the capillary immobilized with fluorescein isothiocyanate isomer-labeled cellular membranes) and on the dynamic binding capacity (DBC) of verapamil (VP, a widely used calcium antagonist which specific interacts with L-type calcium channel proteins located on cellular membrane of rRBC) have been systematically investigated. The fluorescence intensity of the mCMC column when combined with the PLOT capillary was found to be more than five times higher than the intensity using a bare capillary. This intriguing result indicates that the PLOT capillary exhibits a higher cellular membrane capacity. The DBC of VP in the PLOT column was found to be more than nine times higher than that in the bare capillary. An rRBC/CMC column was also prepared for comparative studies. As a result, mCMC provides similar chromatographic retention factors and stability with common CMC; however, the cellular membrane consumption for mCMC was found to be more than 460 times lower than

  7. Silica sodalite without occluded organic matters by topotactic conversion of lamellar precursor.

    PubMed

    Moteki, Takahiko; Chaikittisilp, Watcharop; Shimojima, Atsushi; Okubo, Tatsuya

    2008-11-26

    Novel pure silica sodalite with hollow sodalite-cages has been synthesized for the first time by topotactic conversion of layered silicate (RUB-15) precursor. This success has been achieved by stepwise syntheses from silicate monomers, through clusters and layers, to microporous crystals. The pretreatment of layered silicate with small carboxylic acids before conversion is a crucial step. The obtained sodalite possesses accessible micropores, as confirmed by physical adsorption of hydrogen molecules. This plate-like silica sodalite would be very promising as fillers in mixed-matrix membranes for hydrogen separation.

  8. Ceria and titania incorporated silica based catalyst prepared from rice husk: adsorption and photocatalytic studies of methylene blue.

    PubMed

    Adam, Farook; Muniandy, Lingeswarran; Thankappan, Radhika

    2013-09-15

    Titania and ceria incorporated rice husk silica based catalyst was synthesized via sol-gel method using CTAB and glycerol as surface directing agents at room temperature and labeled as RHS-50Ti10Ce. The catalyst was used to study the adsorption and photodegradation of methylene blue (MB) under UV irradiation. The powder XRD pattern of RHS-50Ti10Ce was much broader (2θ=25-30°) than that of the parent RHS (2θ=22°). The catalyst exhibited type IV isotherm with H3 hysteresis loop, and the TEM images showed partially ordered pore arrangements. The TGA-DTG thermograms confirmed the complete removal of the templates after calcination at 500°C. RHS-50Ti10Ce exhibited excellent adsorption capability with more than 99% removal of MB from a 40 mg L(-1) solution in just 15 min. It also decolorized an 80 mg L(-1) MB solution under UV irradiation in 210 min, which was comparable with the commercialized pure anatase TiO2.

  9. Preparation of end-capped pH-sensitive mesoporous silica nanocarriers for on-demand drug delivery.

    PubMed

    Moreira, André F; Gaspar, Vítor M; Costa, Elisabete C; de Melo-Diogo, Duarte; Machado, Paulo; Paquete, Catarina M; Correia, Ilídio J

    2014-11-01

    Nanocarriers with a pH responsive behavior are receiving an ever growing attention due to their potential for promoting on-demand drug release and thus increase the therapeutic effectiveness of anti-tumoral pharmaceutics. However, the majority of these systems require costly, time-consuming and complex chemical modifications of materials or drugs to synthesize nanoparticles with pH triggered release. Herein, the development of dual drug loaded pH-responsive mesoporous silica nanoparticles (MSNs) with a calcium carbonate-based coating is presented as an effective alternative. This innovative approach allowed the loading of a non-steroidal anti-inflammatory drug (Ibuprofen) and Doxorubicin, with high efficiency. The resulting dual drug loaded MSNs have spherical morphology and a mean size of 171nm. Our results indicate that under acidic conditions the coating disassembles and the drugs are rapidly released, whereas at physiologic pH the release is slower and gradually increases with time. Furthermore, an improved cytotoxic effect was obtained for Doxorubicin-Ibuprofen MSNs coated with CaCO3 in comparison with non-coated particles. The cytotoxic effect of dual loaded carbonate coated particles, was similar to that of Doxorubicin+Ibuprofen free drug administration at 72h, even with the delivery of a significantly lower amount of drug by MSNs-CaCO3. These results suggest that the carbonate coating of MSNs is a promising approach to create a pH-sensitive template for a delivery system with application in cancer therapy.

  10. Bis-clickable Mesoporous Silica Nanoparticles: Straightforward Preparation of Light-Actuated Nanomachines for Controlled Drug Delivery with Active Targeting.

    PubMed

    Noureddine, Achraf; Gary-Bobo, Magali; Lichon, Laure; Garcia, Marcel; Zink, Jeffrey I; Wong Chi Man, Michel; Cattoën, Xavier

    2016-07-04

    Bis(clickable) mesoporous silica nanospheres (ca. 100 nm) were obtained by the co-condensation of TEOS with variable amounts (2-5 % each) of two clickable organosilanes in the presence of CTAB. Such nanoparticles could be easily functionalized with two independent functions using the copper-catalyzed alkyne-azide cycloaddition (CuAAC) reaction to transform them into nanomachines bearing cancer cell targeting ligands with the ability to deliver drugs on-demand. The active targeting was made possible after anchoring folic acid by CuAAC click reaction, whereas the controlled delivery was performed by clicked azobenzene fragments. Indeed, the azobenzene groups are able to obstruct the pores of the nanoparticles in the dark whereas upon irradiation in the UV or in the blue range, their trans-to-cis photoisomerization provokes disorder in the pores, enabling the delivery of the cargo molecules. The on-command delivery was proven in solution by dye release experiments, and in vitro by doxorubicin delivery. The added value of the folic acid ligand was clearly evidenced by the difference of cell killing induced by doxorubicin-loaded nanoparticles under blue irradiation, depending on whether the particles featured the clicked folic acid ligand or not.

  11. Preparation, characterization, and evaluation in vivo of Ins-SiO₂-HP55 (insulin-loaded silica coating HP55) for oral delivery of insulin.

    PubMed

    Zhao, Xiuhua; Shan, Chang; Zu, Yuangang; Zhang, Ying; Wang, Weiguo; Wang, Kunlun; Sui, Xiaoyu; Li, Ruiqiang

    2013-09-15

    Insulin is the most effective and durable drug in the treatment of advanced stage diabetes. However, oral delivering insulin was a tough task for rapid enzymatic degradation. In this work, we designed and developed a delivery system composed of enteric nanosphere for oral delivery of insulin. The silica was selected for loading insulin, which surface has a lot of pores with a powerful adsorption capacity, advantages for permeability and slow-release. The insulin-loaded silica (Ins-SiO2) was prepared by adsorption in HCl solution. The Ins-SiO2 obtained was coated with the hydroxypropyl methylcellulose phthalate (HP55) by desolvation method, which is a good enteric coating material. The Ins-SiO2-HP55, an enteric nanosphere of insulin obtained were characterized by transmission electron microscope (TEM), surface area, Fourier-transform infrared (FT-IR), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The results showed that insulin was loaded most in the pores of silica, while the HP55 coated on the extent of Ins-SiO2. In vitro drug release results revealed that the release of insulin from Ins-SiO2-HP55 was markedly reduced in simulated gastric fluid (SGF). By contrast, the release amount of insulin from Ins-SiO2-HP55 was increased significantly in simulated intestinal fluid (SIF). In vivo evaluation on diabetic animals showed the blood glucose level of diabetic rats could be effectively reduced after oral administration Ins-SiO2-HP55. There is marked hypoglycemic effect after 1h of taking the Ins-SiO2-HP55. After 3h, the GLU of rats of the Ins-SiO2-HP55 stably kept from 4.85 to 2.67 mmol/L that was significantly less than the normal level (6.7 mmol/L). However, that of rats taking raw insulin kept from 8.03 to 6.56 mmol/L that is higher than the normal level. These results suggested that Ins-SiO2-HP55 could have potential value in oral administration systems of diabetes chemotherapy.

  12. One-pot preparation of a mixed-mode organic-silica hybrid monolithic capillary column and its application in determination of endogenous gibberellins in plant tissues.

    PubMed

    Zhang, Zheng; Hao, Yan-Hong; Ding, Jun; Xu, Sheng-Nan; Yuan, Bi-Feng; Feng, Yu-Qi

    2015-10-16

    A newly improved one-pot method, based on "thiol-ene" click chemistry and sol-gel approach in microemulsion system, was developed for the preparation of C8/PO(OH)2-silica hybrid monolithic capillary column. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The monolithic column was demonstrated to have cation exchange/reversed-phase (CX/RP) mixed-mode retention for analytes on nano-liquid chromatography (nano-LC). On the basis of the developed nano-LC system with MS detector coupled to pipette tip solid phase extraction (PT-SPE) and derivatization process, we then realized simultaneous determination of 10 gibberellins (GAs) with low limits of detection (LODs, 0.003-0.025 ng/mL). Furthermore, 6 endogenous GAs in only 5mg rice leaves (fresh weight) were successfully detected and quantified. The developed PT-SPE-nano-LC-MS strategy may offer promising applications in the determination of low abundant bioactive molecules from complex matrix.

  13. Recovery of silica from electronic waste for the synthesis of cubic MCM-48 and its application in preparing ordered mesoporous carbon molecular sieves using a green approach

    NASA Astrophysics Data System (ADS)

    Liou, Tzong-Horng

    2012-07-01

    The electronics industry is one of the world's fastest growing manufacturing industries. However, e-waste has become a serious pollution problem. This study reports the recovery of e-waste for preparing valuable MCM-48 and ordered mesoporous carbon for the first time. Specifically, this study adopts an alkali-extracted method to obtain sodium silicate precursors from electronic packaging resin ash. The influence of synthesis variables such as gelation pH, neutral/cationic surfactant ratio, hydrothermal treatment temperature, and calcination temperature on the mesophase of MCM-48 materials is investigated. Experimental results confirm that well-ordered cubic MCM-48 materials were synthesized in strongly acidic and strongly basic media. The resulting mesoporous silica had a high surface area of 1,317 m2/g, mean pore size of about 3.0 nm, and a high purity of 99.87 wt%. Ordered mesoporous carbon with high surface area (1,715 m2/g) and uniform pore size of CMK-1 type was successfully prepared by impregnating MCM-48 template using the resin waste. The carbon structure was sensitive to the sulfuric acid concentration and carbonization temperature. Converting e-waste into MCM-48 materials not only eliminates the disposal problem of e-waste, but also transforms industrial waste into a useful nanomaterial.

  14. Preparation of hybrid organic-inorganic mesoporous silicas applied to mercury removal from aqueous media: Influence of the synthesis route on adsorption capacity and efficiency.

    PubMed

    Pérez-Quintanilla, Damián; Sánchez, Alfredo; Sierra, Isabel

    2016-06-15

    New hybrid organic-inorganic mesoporous silicas were prepared by employing three different synthesis routes and mercury adsorption studies were done in aqueous media using the batch technique. The organic ligands employed for the functionalization were derivatives of 2-mercaptopyrimidine or 2-mercaptothiazoline, and the synthesis pathways used were post-synthesis, post-synthesis with surface ion-imprinting and co-condensation with ion-imprinting. The incorporation of functional groups and the presence of ordered mesopores in the organosilicas was confirmed by XRD, TEM and SEM, nitrogen adsorption-desorption isotherms, (13)C MAS-NMR, (29)Si MAS-NMR, elemental and thermogravimetric analysis. The highest adsorption capacity and selectivity observed was for the material functionalized with 2-mercaptothiazoline ligand by means the co-condensation with ion-imprinting route (1.03 mmol g(-1) at pH 6). The prepared material could be potential sorbent for the extraction of this heavy metal from environmental and drinking waters.

  15. Preparation and retention mechanism study of graphene and graphene oxide bonded silica microspheres as stationary phases for high performance liquid chromatography.

    PubMed

    Zhang, Xiaoqiong; Chen, Sha; Han, Qiang; Ding, Mingyu

    2013-09-13

    Graphene oxide (GO) bonded stationary phase for high performance liquid chromatography (HPLC) was fabricated by coating GO sheets onto aminosilica microspheres via covalent coupling. Graphene (G) functionalized HPLC stationary phase was then prepared through hydrazine reduction of GO bonded silica (GO@SiO2) composite, which was the first example of using graphene as stationary-phase component for HPLC. Effective separations of the tested neutral and polar compounds on both GO@SiO2 and graphene bonded silica (G@SiO2) columns were achieved under the optimal experimental conditions. Compared with commercial C18 column, the different chromatographic performances of GO and graphene bonded columns were ascribed to their unique retention mechanisms. The polyaromatic scaffold of GO and graphene gives π-π stacking property and hydrophobic effect, and other retention mechanisms, such as π-π electron-donor-acceptor (EDA) interaction for the separation of nitroaromatic compounds and hydrogen bonding for hydroxyl and amino compounds, may also be taken into consideration. Experimental results indicated that the mixed-mode retention mechanism can facilitate the separation of analytes with similar hydrophobicity, which is a unique property compared with C18 column. Additionally, G@SiO2 showed higher affinity to aromatic analytes in contrast with GO@SiO2 and its retention mechanism was not consistent with the typical reversed phase behavior. The separation of aromatic compounds on G@SiO2 column relies primarily on the π-π stacking interaction and then the hydrophobicity, while the two interactions have equal shares on GO@SiO2 column.

  16. Encapsulation of biomolecules for bioanalytical purposes: preparation of diclofenac antibody-doped nanometer-sized silica particles by reverse micelle and sol-gel processing.

    PubMed

    Tsagkogeorgas, Fotios; Ochsenkühn-Petropoulou, Maria; Niessner, Reinhard; Knopp, Dietmar

    2006-07-28

    In recent years, the sol-gel technique has attracted increasing interest as a unique approach to immobilize biomolecules for bioanalytical applications as well as biochemical and biophysical studies. For this purpose, crushed biomolecule-doped sol-gel glass monoliths have been widely used. In the present work, for the first time, the encapsulation of anti-diclofenac antibodies in silica nanoparticles was carried out by a combination of reverse micelle and sol-gel technique. Cyclohexane was used for the preparation of the microemulsion as organic solvent, while surfactant Igepal CO-520 was found to be the optimal stabilizer. The antibody source was a purified IgG fraction originating from a polyclonal rabbit antiserum. Tetramethyl orthosilicate (TMOS) was used as precursor. Rather uniform, monodispersed and spherical silica particles of about 70nm diameter size were fabricated, as was demonstrated by transmission electron microscopy (TEM) and scanning electron microscopy/energy dispersive X-ray fluorescence analysis (SEM/EDX). The biological activity of the encapsulated antibodies was evaluated by incubation of the nanoparticles with a diclofenac standard solution and analysis of the filtrate and followed washing solutions by a highly sensitive enzyme-linked immunosorbent assay (ELISA), using non-doped particles as blanks. While only about 6% of the added diclofenac was nonspecifically retained by the blank, the corresponding amount of about 66% was much higher with the antibody-doped particles. An obvious advantage of this approach is the general applicability of the developed technique for a mild immobilization of different antibody species.

  17. Preparation and characterization of multi-carboxyl-functionalized silica gel for removal of Cu (II), Cd (II), Ni (II) and Zn (II) from aqueous solution

    NASA Astrophysics Data System (ADS)

    Li, Min; Li, Ming-yu; Feng, Chang-gen; Zeng, Qing-xuan

    2014-09-01

    In this paper, the multi-carboxyl-functionalized silica gel was prepared by surface grafting method and applied for the removal of Cu (II), Cd (II), Ni (II) and Zn (II) from aqueous solution. The adsorbent was characterized by FT-IR, thermogravimetry, Brunauer-Emmett-Teller surface area measurement and elemental analysis, and it proved that the organic functional group, carboxyl group, was grafted successfully onto the silica gel surface. The effect of solution pH on removal efficiencies of Cu (II), Cd (II), Ni (II) and Zn (II) was investigated and it was found that with the exception of Zn (II), the removal efficiencies of the rest of metal ions increased with the increasing of pH in the solution, the maximum removal efficiency occurred at pH 6.0, whereas the maximum removal efficiency for Zn (II) was found to be at pH 7.0. Adsorption equilibrium data were well fitted to Langmuir than Freundlich isotherm model and the maximum adsorption capacity for Cu (II), Cd (II), Ni (II) and Zn (II) was 47.07, 41.48, 30.80 and 39.96 mg/g, respectively. Competitive adsorption experiments demonstrated that the adsorbent material had excellent adsorption amount and high affinity for the Cu (II) in the binary systems. In addition, the column experiments were used to investigate stability and reusability of the adsorbent, the dynamic adsorption performance, and desorption of metal ions absorbed from the adsorbent. The results confirmed that the adsorbent presents good dynamic adsorption performance for Cu (II), Cd (II), Ni (II) and Zn (II) and these metal ions adsorbed were easy to be desorbed from the adsorbent. The adsorption capacities of metal ions did not present an obvious decrease after five cycles of adsorption-desorption.

  18. Tuning preparation conditions towards optimized separation performance of thermally polymerized organo-silica monolithic columns in capillary liquid chromatography.

    PubMed

    Gharbharan, Deepa; Britsch, Denae; Soto, Gabriela; Weed, Anna-Marie Karen; Svec, Frantisek; Zajickova, Zuzana

    2015-08-21

    Tuning of preparation conditions, such as variations in the amount of a porogen, concentration of an aqueous acid catalyst, and adjustment in polymerization temperature and time, towards optimized chromatographic performance of thermally polymerized monolithic capillaries prepared from 3-(methacryloyloxy)propyltrimethoxysilane has been carried out. Performance of capillary columns in reversed-phase liquid chromatography was assessed utilizing various sets of solutes. Results describing hydrophobicity, steric selectivity, and extent of hydrogen bonding enabled comparison of performance of hybrid monolithic columns prepared under thermal (TSG) and photopolymerized (PSG) conditions. Reduced amounts of porogen in the polymerization mixture, and prolonged reaction times were necessary for the preparation of monolithic columns with enhanced retention and column efficiency that reached to 111,000 plates/m for alkylbenzenes with shorter alkyl chains. Both increased concentration of catalyst and higher temperature resulted in faster polymerization but inevitably in insufficient time for pore formation. Thermally polymerized monoliths produced surfaces, which were slightly more hydrophobic (a methylene selectivity of 1.28±0.002 TSG vs 1.20±0.002 PSG), with reduced number of residual silanols (a caffeine/phenol selectivity of 0.13±0.001 TSG vs 0.17±0.003 PSG). However, steric selectivity of 1.70±0.01 was the same for both types of columns. The batch-to-batch repeatability was better using thermal initiation compared to monolithic columns prepared under photopolymerized conditions. RSD for retention factor of benzene was 3.7% for TSG capillaries (n=42) vs. 6.6% for PSG capillaries (n=18). A similar trend was observed for columns prepared within the same batch.

  19. Wear and Friction Behavior of Metal Impregnated Microporous Carbon Composites

    NASA Technical Reports Server (NTRS)

    Goller, Gultekin; Koty, D. P.; Tewari, S. N.; Singh, M.; Tekin, A.

    1996-01-01

    Metal-matrix composites have been prepared by pressure-infiltration casting of copper-base alloy melts into microporous carbon preforms. The carbon preforms contained varying proportions of amorphous carbon and graphite. Load dependence of the wear and friction behavior of the composite pins has been examined under ambient conditions against cast-iron plates, using a pin-on-plate reciprocating wear tester. The wear resistance of the composite is significantly improved, as compared with the base alloy. Contrary to the normally expected behavior, the addition of graphite to the amorphous carbon does not reduce the friction coefficient, especially at high loads. The wear and friction behavior of the composites is very sensitive to the size and distribution of the microstructural constituents.

  20. Zeotile-2: A microporous analogue of MCM-48

    NASA Astrophysics Data System (ADS)

    Kremer, Sebastien P. B.; Kirschhock, Christine E. A.; Aerts, Alexander; Aerts, Caroline A.; Houthoofd, Kristof J.; Grobet, Piet J.; Jacobs, Pierre A.; Lebedev, Oleg I.; Van Tendeloo, Gustaaf; Martens, Johan A.

    2005-07-01

    Ordered mesoporous materials with specific microporosity in the mesopore walls can be assembled by a secondary templating synthesis departing from a clear subcolloidal suspension dedicated to the tetrapropylammonium (TPA) mediated synthesis of colloidal Silicalite-1. A typical member of this material family is Zeotile-2. Zeotile-2 is mesostructurally similar to the cubic MCM-48 material with exceptional long-range order of the mesostructure. Zeotile-2 samples in which the TPA was either left or evacuated were prepared by leaching in boiling ethanolic acetic acid and calcination. The evacuation of the TPA gave rise to a substantial micropore volume revealed with nitrogen adsorption isotherms. The mesoporosity was independent of the presence of the TPA. Molecular separations of isooctane/octane mixtures illustrated the occurrence of molecular shape selectivity similar to MFI-type zeolites.

  1. Wear and friction behavior of metal impregnated microporous carbon composites

    SciTech Connect

    Goller, G.; Koty, D.P.; Tewari, S.N.; Singh, M.; Tekin, A.

    1996-11-01

    Metal-matrix composites have been prepared by pressure-infiltration casting of copper-base alloy melts into microporous carbon preforms. The carbon preforms contained varying proportions of amorphous carbon and graphite. Load dependence of the wear and friction behavior of the composite pins has been examined under ambient conditions against cast-iron plates, using a pin-on-plate reciprocating wear tester. The wear resistance of the composite is significantly improved, as compared with the base alloy. Contrary to the normally expected behavior, the addition of graphite to the amorphous carbon does not reduce the friction coefficient, especially at high loads. The wear and friction behavior of the composites is very sensitive to the size and distribution of the microstructural constituents.

  2. Electron transfer reactions in microporous solids

    SciTech Connect

    Mallouk, T.E.

    1993-01-01

    Basic thrust the research program involves use of microporous solids (zeolites, clays, layered and tunnel structure oxide semiconductors) as organizing media for artificial photosynthetic systems. Purpose of the microporous solid is twofold. First, it induces spatial organization of photoactive and electroactive components (sensitizers, semiconductor particles, electron relays, and catalysts) at the solid-solution interface, enhancing the quantum efficiency of charge separation and separating physically the ultimate electron donor and acceptor in the electron transport chain. Second, since the microcrystalline solid admits only molecules of a certain charge and size, it is possible to achieve permanent charge separation by sieving chemical photoproducts (e.g., H[sub 2] and I[sub 3][sup [minus

  3. Method for making a microporous membrane

    NASA Technical Reports Server (NTRS)

    Gavalas, Lillian Susan (Inventor)

    2013-01-01

    A method for making a microporous membrane comprises the steps of: providing a plurality of carbon nanotubes having a hollow interior diameter of 20 Angstroms or less; sonicating the plurality of carbon nanotubes utilizing a solution comprising deionized, distilled water and a surfactant that coats at least one of the plurality of carbon nanotubes; collecting the coated carbon nanotubes; forming a matrix that supports the plurality of carbon nanotubes; embedding the coated carbon nanotubes into the matrix; rinsing the coated nanotubes to remove at least a portion of the surfactant; curing the nanotube-matrix assembly; and cutting the nanotube-matrix assembly to a particular thickness so as to open the ends of the embedded nanotubes. The hollow interiors of the plurality of embedded carbon nanotubes comprise the pores of the microporous membrane.

  4. Water Adsorption Equilibria on Microporous Carbons

    DTIC Science & Technology

    1988-11-01

    of water adsorption on activated carbon is the presence of a large hysteresis loop indicating that the amount adsorbed depends on the past exposure...conditions of the carbon. The theories to describe hysteresis in microporous adsorbents and the experimental evidence to support each theory have been...observed behaviors on activated carbon. Neither the Dubinin- Serpinsky, nor the Sircar equations provide any explanation for hysteresis . It appears that

  5. Ketoprofen mesoporous silica nanoparticles SBA-15 hard gelatin capsules: preparation and in vitro/in vivo characterization.

    PubMed

    Abd-Elrahman, Ahmed A; El Nabarawi, Mohamed A; Hassan, Doaa H; Taha, Amal A

    2016-11-01

    SBA-15 is used to enhance the bioavailability of poorly soluble ketoprofen (KP) through stabilization of its amorphous state. Additionally, the current work provides a complete in vitro and in vivo study on preformulated KP-SBA-15 sample and formulated KP-SBA-15 in hard gelatin capsule. Loading of KP was done by a novel method called immersion-rotavapor method. KP was quantified by extraction and thermal gravimetric analysis (TGA). Characterization of the loaded SBA-15 sample was done by high resolution transmission electron microscopy (HRTEM), small angle X-ray diffraction (SAXRD), nitrogen adsorption/desorption isotherms, differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy and dissolution profiles. The loaded sample was formulated in hard gelatin capsule. The anti-inflammatory and analgesic studies were carried out on 24 adult male albino rats. TGA and extraction results showed 54.4 wt% of drug incorporated. Characterization of KP-SBA-15 sample confirmed the successful encapsulation of KP into the carrier pores in a molecular amorphous state. Additionally, loading of KP did not affect the mesoporous internal structure. During the first 5 min, the dissolution study showed very high release rates; nearly 50% of KP was released. These results were reflected on the in vivo study resulting in 82% inhibition in edema after 1 h and maximum analgesia after 30 min from the administration of the formulated sample. SBA-15 mesoporous silica nanoparticle proved to be a very promising drug delivery carrier that can be used as a facile way to enhance the bioavailability of poorly soluble drugs.

  6. Preparation of NO2-Aged Silver-Functionalized Silica-Aerogel and Silver Mordenite Samples

    SciTech Connect

    Jordan, Jacob A.; Bruffey, Stephanie H.

    2016-10-01

    Reprocessing used nuclear fuel can result in the volatilization of radioactive gaseous species, including 129I, into the various process off-gas streams. In order to comply with US regulatory requirements, plant off-gas streams must be treated to remove the iodine prior to discharging the off-gas into the environment. The performance of available gas removal methods depends not only on the concentration of the volatile radioisotope of interest, but also on other constituents that could be present in the reprocessing off-gas streams. Some of the constituents, such as NOx produced during fuel dissolution, are known to have deleterious effects on the capture performance of silver-based sorbents used for iodine removal. Commercially available reduced silver mordenite (AgZ) has an iodine saturation concentration of 7.0-9.0 wt%, and its iodine sorption capacity is reduced by 20-50% as a result of NO2 aging. Silverfunctionalized silica aerogel (AgAerogel), an alternative for iodine capture, has an initial iodine saturation of 29.0 wt% and its iodine capacity is only reduced by 15% from NO2 aging. Understanding the differences in aging behavior between AgZ and AgAerogel is critical to determining the behavior of these sorbents under realistic off-gas conditions. To assist in future technical studies on this topic, samples of both AgZ and AgAerogel were aged with NO2. In the experiment, 10.2190 g of AgZ and 10.1771 g of AgAerogel were exposed to a static 0.75% NO2/dry air blend for a period of 28 days. The samples were then removed and stored under argon until needed for future experiments.=

  7. Inorganic dual-layer microporous supported membranes

    DOEpatents

    Brinker, C. Jeffrey; Tsai, Chung-Yi; Lu, Yungfeng

    2003-03-25

    The present invention provides for a dual-layer inorganic microporous membrane capable of molecular sieving, and methods for production of the membranes. The inorganic microporous supported membrane includes a porous substrate which supports a first inorganic porous membrane having an average pore size of less than about 25 .ANG. and a second inorganic porous membrane coating the first inorganic membrane having an average pore size of less than about 6 .ANG.. The dual-layered membrane is produced by contacting the porous substrate with a surfactant-template polymeric sol, resulting in a surfactant sol coated membrane support. The surfactant sol coated membrane support is dried, producing a surfactant-templated polymer-coated substrate which is calcined to produce an intermediate layer surfactant-templated membrane. The intermediate layer surfactant-templated membrane is then contacted with a second polymeric sol producing a polymeric sol coated substrate which is dried producing an inorganic polymeric coated substrate. The inorganic polymeric coated substrate is then calcined producing an inorganic dual-layered microporous supported membrane in accordance with the present invention.

  8. Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

    NASA Astrophysics Data System (ADS)

    He, Feng

    The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single

  9. Fluorescence probing investigation of the mechanism of formation of MSU-type mesoporous silica prepared in fluoride medium.

    PubMed

    Lesaint, Cédric; Lebeau, Bénédicte; Marichal, Claire; Patarin, Joël; Zana, Raoul

    2005-09-13

    The mechanism of formation of a MSU-type siliceous material from tetraethyl orthosilicate (TEOS) in the presence of the nonionic surfactant tergitol T-15-S-12, sulfuric acid, and sodium fluoride has been investigated using mainly fluorescence probing techniques and, to a lesser extent, dynamic light scattering (DLS) and 29Si NMR spectroscopy. The tergitol micelles present in the systems obtained by progressively generating the reaction mixture giving rise to the mesostructured material by adding to an appropriate tergitol solution sulfuric acid, TEOS, and NaF were characterized by fluorescence probing (micelle aggregation number, micropolarity, and microviscosity) and also by dynamic light scattering (apparent micelle diameter). 29Si NMR experiments were also performed on selected systems after hydrolysis of the TEOS. The fluorescence probing techniques were also used to follow the changes of micelle characteristics with time during the evolution of the full reaction mixture from a limpid solution to a system containing a minor amount of condensed siliceous material. The synthesized solid material was characterized by X-ray diffraction and nitrogen adsorption-desorption analyses. The micelle aggregation number N was found to change only little, and the micropolarity remained constant when going from the tergitol solution to the full reaction mixture. The results of DLS measurements agree with this finding. Besides, while the condensation of silica took place after addition of NaF, the N value increased only very little with time up to the point where a small amount of mesostructured material precipitated out. These results indicate that the interaction between tergitol micelles and the siliceous species formed in the system by the hydrolysis of TEOS and also between micelles and the growing siliceous species must be very weak. As in our previous studies of the mechanism of formation of MCM41-type material from sodium silicate in the presence of

  10. Micropores and methods of making and using thereof

    DOEpatents

    Perroud, Thomas D.; Patel, Kamlesh D.; Meagher, Robert J.

    2016-08-02

    Disclosed herein are methods of making micropores of a desired height and/or width between two isotropic wet etched features in a substrate which comprises single-level isotropic wet etching the two features using an etchant and a mask distance that is less than 2.times. a set etch depth. Also disclosed herein are methods using the micropores and microfluidic devices comprising the micropores.

  11. Macroporous Polymers with Aligned Microporous Walls from Pickering High Internal Phase Emulsions.

    PubMed

    Zhu, Yun; Zhang, Ranran; Zhang, Shengmiao; Chu, Yeqian; Chen, Jianding

    2016-06-21

    A novel class of macroporous polymers, open macroporous polymers with aligned microporous void walls, were prepared by combining particle-stabilized high internal phase emulsion (Pickering HIPE) and unidirectional freezing technique. These Pickering HIPEs were prepared by utilizing poly(urethane urea)/(vinyl ester resin) nanoparticles as the sole stabilizer, and this nanoparticles also acted as building blocks for the resulting macroporous polymers. Moreover, the morphology and compression modulus of the resulting porous materials could be tuned easily. This means now Pickering-HIPE templated open-cell foams can be prepared, and this route was normally achieved with surfactant and/or chemical reaction involved.

  12. Synthesis and modification of mesoporous silica and the preparation of molecular sieve thin films via pulsed laser deposition

    NASA Astrophysics Data System (ADS)

    Coutinho, Decio Heringer

    2001-07-01

    Hexagonal mesoporous DAM-1 (Dallas Amorphous Material-1) was prepared using Vitamin E TPGS as the structure-directing agent. Depending upon the temperature and gel composition, highly ordered and hydrothermally stable DAM-1 with various morphologies could be achieved including spheres, gyroids, discoid, hexagonal plates and rods. This synthesis was modified to prepare hybrid organic-inorganic amine and thiol bifunctionalized DAM-1 by direct co-condensation under acidic conditions. Patterned DAM-1 thin films were prepared on patterned transparencies utilizing pulsed laser deposition (PLD) and line patterning techniques. DAM-1 laser ablation onto the patterned substrate followed by hydrothermal treatment resulted in a densely packed film. Removal of the patterned lines by sonication revealed patterned DAM-1 films. Thin films of zeolite type X were also prepared using the PLD technique. Laser ablation of zeolite X onto TiN-coated silicon wafers followed by a hydrothermal treatment resulted in partially oriented, crystalline membranes. Hydrothermal treatment of PLD films on stainless steel mesh produced a coated wire mesh with a 3-mum thick zeolite X film. A novel strategy for imprinting mesoporous SBA-15 that combines a triblock copolymer template and a chiral ruthenium complex is reported. A chiral PEO helix was formed by the chiral ruthenium complex interaction with the block copolymer during the synthesis of SBA-15. Upon removal of the chiral ruthenium complex, a stereospecfic cavity was created. Preliminary results indicated stereoselective absorption of Delta or Λ-Ru(phen)3 2+ isomer from a racemic mixture could be achieved depending on the chirality of the PEO chain. Practicum Two. The industrial practicum report describes the process development unit (PDU) 3-pentenenitrile (3PN) refining operation. This distillation works was operated to refine crude 3PN product, which contained 3PN, 2-methyl-3-butenenitrile (2M3BN), and other byproducts. This report also

  13. Investigation of the sample preparation and curing treatment effects on mechanical properties and bioactivity of silica rich metakaolin geopolymer.

    PubMed

    Catauro, M; Bollino, F; Papale, F; Lamanna, G

    2014-03-01

    In many biomedical applications both the biological and mechanical behaviours of implants are of relevant interest; in the orthopaedic field, for example, favourable bioactivity and biocompatibility capabilities are necessary, but at the same time the mechanical characteristics of the implants must be such as to allow one to support the body weight. In the present work, the authors have examined the application of geopolymers with composition H24AlK7Si31O79 and ratio Si/Al=31 to be used in biomedical field, considering two different preparation methods: one of the activators (KOH) has been added as pellets in the potassium silicate solution, in the other as a water solution with 8M concentration. Moreover, a different water content was used and only some of the synthesized samples were heat treated. The chemical and microstructural characterizations of those materials have been carried out by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Subsequently, the effects of the adopted preparation on the mechanical and biological properties have been studied: compressive strength tests have demonstrated that more fragile specimens were obtained when KOH was added as a solution. The bioactivity was successfully evaluated with the soaking of the samples in a simulated body fluid (SBF) for 3 weeks. The formation of a layer of hydroxyapatite on the surface of the materials has been shown both by SEM micrographs and EDS analyses.

  14. Preparation of magnetic core-shell iron oxide@silica@nickel-ethylene glycol microspheres for highly efficient sorption of uranium(VI).

    PubMed

    Tan, Lichao; Zhang, Xiaofei; Liu, Qi; Wang, Jun; Sun, Yanbo; Jing, Xiaoyan; Liu, Jingyuan; Song, Dalei; Liu, Lianhe

    2015-04-21

    We report a facile approach for the formation of magnetic core-shell iron oxide@silica@nickel-ethylene glycol (Fe3O4@SiO2@Ni-L) microspheres. The structure and morphology of Fe3O4@SiO2@Ni-L are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen sorption isotherm. The composite possesses a high specific surface area of 382 m(2) g(-1). The obtained core/shell structure is composed of a superparamagnetic core with a strong response to external fields, which are recovered readily from aqueous solutions by magnetic separation. When used as the adsorbent for uranium(vi) in water, the as-prepared Fe3O4@SiO2@Ni-L multi-structural microspheres exhibit a high adsorption capacity, which is mainly attributed to the large specific surface area and typical mesoporous characteristics of Fe3O4@SiO2@Ni-L microspheres. This work provides a promising approach for the design and synthesis of multifunctional microspheres, which can be used for water treatment, as well as having other potential applications in a variety of biomedical fields including drug delivery and biosensors.

  15. Bactericidal activity and silver release of porous ceramic candle filter prepared by sintering silica with silver nanoparticles/zeolite for water disinfection

    NASA Astrophysics Data System (ADS)

    Trinh Nguyen, Thuy Ai; Phu Dang, Van; Duy Nguyen, Ngoc; Le, Anh Quoc; Thanh Nguyen, Duc; Hien Nguyen, Quoc

    2014-09-01

    Porous ceramic candle filters (PCCF) were prepared by sintering silica from rice husk with silver nanoparticles (AgNPs)/zeolite A at about 1050 °C to create bactericidal PCCF/AgNPs for water disinfection. The silver content in PCCF/AgNPs was of 300-350 mg kg-1 determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and the average pore size of PCCF/AgNPs was of 50-70 Å measured by Brunauer-Emmett-Teller (BET) method. The bactericidal activity and silver release of PCCF/AgNPs have been investigated by flow test with water flow rate of 5 L h-1 and initial inoculation of E. coli in inlet water of 106 CFU/100 mL. The volume of filtrated water was collected up to 500 L. Results showed that the contamination of E. coli in filtrated water was <1 CFU/100 mL and the content of silver released from PCCF/AgNPs into filtrated water was <1 μg L-1, it is low, far under the WHO guideline of 100 μg L-1 at maximum for drinking water. Based on the content of silver in PCCF/AgNPs and in filtrated water, it was estimated that one PCCF/AgNPs could be used to filtrate of ˜100 m3 water. Thus, as-prepared PCCF/AgNPs releases low content of silver into water and shows effectively bactericidal activity that is promising to apply as point-of-use water treatment technology for drinking water disinfection.

  16. A dual-spatially-confined reservoir by packing micropores within dense graphene for long-life lithium/sulfur batteries.

    PubMed

    Li, Hongfei; Yang, Xiaowei; Wang, Xiaomin; He, Yu-Shi; Ye, Fangmin; Liu, Meinan; Zhang, Yuegang

    2016-01-28

    In lithium/sulfur batteries, micropores could bring about strong interactions with polysulfides, but could not alleviate the partial polysulfide overflowing outside because of the volume expansion of the lithiated sulfur. A dual-spatially-confined reservoir for sulfur by wrapping microporous carbon with dense graphene, micro@meso-porous DSC (dual-spatial carbon), is synthesized to solve this issue. Such a structure is prepared through two distinctive methods: graphene promoted in situ hydrothermal carbonization of organics to grow micropores on itself, and liquid mediated drying of graphene hydrogel to form mesoporous graphene frameworks. In contrast to previously reported hierarchical carbon/S, the inner micropores are mainly responsible for loading sulfur, which could help confine its particle size, thus increasing the electrical/ionic conductivity and the utilization of sulfur, and restrain lithium polysulfide dissolution because of strong interaction with pore walls; while the outer mesopores act as another reservoir to stabilize the overflowed polysulfide and to enhance the Li(+) transport. The S-micro@meso-porous DSC cathode exhibits better discharge capacity and cycling performance than S-microporous AC and S-micro@macro-porous DSC, i.e., 59% and 37% higher capacity remaining at 0.5 C than the latter two, respectively.

  17. Random lasing of microporous surface of Cr{sup 2+}:ZnSe crystal induced by femtosecond laser

    SciTech Connect

    Yang, Xianheng; Feng, Guoying E-mail: zhoush@scu.edu.cn; Yao, Ke; Yi, Jiayu; Zhang, Hong; Zhou, Shouhuan E-mail: zhoush@scu.edu.cn

    2015-06-15

    We demonstrate a random lasing emission based on microporous surface of Cr{sup 2+}:ZnSe crystal prepared by femtosecond pulsed laser ablation in high vacuum (below 5 × 10{sup −4} Pa). The scanning electron microscope results show that there are a mass of micropores with an average size of ∼13 μm and smaller ones with ∼1.2 μm on the surface of Cr{sup 2+}:ZnSe crystal. The adjacent micropore spacing of the smaller micropores ranges from 1 μm to 5 μm. Under 1750 nm excitation of Nd:YAG (355 nm) pumped optical parametric oscillator, a random lasing emission with center wavelength of 2350 nm and laser-like threshold of 0.3 mJ/pulse is observed. The emission lifetime of 2350 nm laser reduces from 800 ns to 30 ns as the pump energy increases above threshold. The emission spectra and decay time of smooth surface, groove and microporous surface of Cr{sup 2+}:ZnSe crystal are contrasted. The optional pump wavelength range is from 1500 nm to 1950 nm, which in accordance with the optical absorption property of Cr{sup 2+}:ZnSe crystal. The peak position of excitation spectra is almost identical to the strongest absorption wavelength.

  18. Effects of CO2 activation on electrochemical performance of microporous carbons derived from poly(vinylidene fluoride)

    NASA Astrophysics Data System (ADS)

    Lee, Seul-Yi; Park, Soo-Jin

    2013-11-01

    In this work, we have prepared microporous carbons (MPCs) derived from poly(vinylidene fluoride) (PVDF), and the physical activation of MPCs using CO2 gas is subsequently carried out with various activation temperatures to investigate the electrochemical performance. PVDF is successfully converted into MPCs with a high specific surface area and well-developed micropores. After CO2 activation, the specific surface areas of MPCs (CA-MPCs) are enhanced by 12% compared with non-activated MPCs. With increasing activation temperature, the micropore size distributions of A-MPCs also become narrower and shift to larger pore size. It is also confirmed that the CO2 activation had developed the micropores and introduced the oxygen-containing groups to MPCs‧ surfaces. From the results, the specific capacitances of the electrodes in electric double layer capacitors (EDLCs) based on CA-MPCs are distinctly improved through CO2 activation. The highest specific capacitance of the A-MPCs activated at 700 °C is about 125 F/g, an enhancement of 74% in comparison with NA-MPCs, at a discharge current of 2 A/g in a 6 M KOH electrolyte solution. We also found that micropore size of 0.67 nm has a specific impact on the capacitance behaviors, besides the specific surface area of the electrode samples.

  19. Self-formation of microporous polysulfone hollow fiber using a single nozzle spinneret and reduction of phase-inversion speed

    NASA Astrophysics Data System (ADS)

    Kim, Hyung Jin; Jang, Chang Sik; Kim, Byeong Hee; Seo, Young Ho

    2016-06-01

    This study proposed a simple fabrication technique for microporous hollow fibers whose inner channel was naturally formed because of a slow phase inversion speed. Conventionally, microporous hollow fibers have been fabricated by extruding a polymer solution through the outer nozzle and a bore liquid through the inner nozzle of a dual nozzle spinneret. Injecting a bore liquid played a key role for the formation of a hollow structure. In this study, the self-formation of a hollow structure of microporous fiber was developed using a single nozzle spinneret without a bore liquid. A sharp tip single nozzle spinneret of 200 µm in diameter was fabricated by the wetting effect of a liquid pre-polymer of polydimethylsiloxane, and polysulfone solution was extruded through the prepared single nozzle spinneret. The temperature of the coagulant bath was controlled in order to reduce the speed of phase change, because the phase-change speed depended on the temperature of the coagulant solution. An inner channel in the microporous fiber was successfully fabricated by reducing the phase-change speed and by increasing the solidification speed. The inner diameter of the microporous hollow fiber was decreased as the temperature of the coagulant bath was increased, and eventually the inner channel was not formed at the higher bath temperature rather than 25 °C.

  20. A facile route to preparation of high purity nanoporous silica from acid-leached residue of serpentine.

    PubMed

    Bai, Penn; Sharratt, Paul; Yeo, Tze Yuen; Bu, Jie

    2014-09-01

    As the current cost of mineral carbonation is too high for an economically viable industrial process, it is desirable to produce value-added products from CO2 mineralization process. In this work, a facile and cost-effective process was developed for the production of high purity SiO2 from acid-leached serpentine residue. The Si extraction rate is fast even under ambient conditions due to the highly defective structure of the residue. The reaction kinetics were studied and it was found that the Si extraction rate was under a combination of chemical reaction control and film diffusion control. The SiO2 sample prepared has high purity with a nanoporous structure, which renders it a potential candidate for applications such as an adsorbent and a catalyst support.

  1. Preparation of high efficiency and low carry-over immobilized enzymatic reactor with methacrylic acid-silica hybrid monolith as matrix for on-line protein digestion.

    PubMed

    Yuan, Huiming; Zhang, Lihua; Zhang, Yukui

    2014-12-05

    In this work, a novel kind of organic-silica hybrid monolith based immobilized enzymatic reactor (IMER) was developed. The monolithic support was prepared by a single step "one-pot" strategy via the polycondensation of tetramethoxysilane and vinyltrimethoxysilane and in situ copolymerization of methacrylic acid and vinyl group on the precondensed siloxanes with ammonium persulfate as the thermal initiator. Subsequently, the monolith was activated by N-(3-dimethylaminopropyl) - N'-ethylcarbodiimide (EDC) and N-hydroxysuccinimide (NHS), followed by the modification of branched polyethylenimine (PEI) to improve the hydrophilicity. Finally, after activated by EDC and NHS, trypsin was covalently immobilized onto the monolithic support. The performance of such a microreactor was evaluated by the in sequence digestion of bovine serum albumin (BSA) and myoglobin, followed by MALDI-TOF-MS analysis. Compared to those obtained by traditional in-solution digestion, not only higher sequence coverages for BSA (74±1.4% vs. 59.5±2.7%, n=6) and myoglobin (93±3% vs. 81±4.5%, n=6) were obtained, but also the digestion time was shortened from 24h to 2.5 min, demonstrating the high digestion efficiency of such an IMER. The carry-over of these two proteins on the IMER was investigated, and peptides from BSA could not be found in mass spectrum of myoglobin digests, attributed to the good hydrophilicity of our developed monolithic support. Moreover, the dynamic concentration range for protein digestion was proved to be four orders of magnitude, and the IMER could endure at least 7-day consecutive usage. Furthermore, such an IMER was coupled with nano-RPLC-ESI/MS/MS for the analysis of extracted proteins from Escherichia coli. Compared to formerly reported silica hybrid monolith based IMER and the traditional in-solution counterpart, by our developed IMER, although the identified protein number was similar, the identified distinct peptide number was improved by 7% and 25% respectively

  2. Molecular engineering of porous silica using aryl templates

    DOEpatents

    Loy, D.A.; Shea, K.J.

    1994-06-14

    A process is described for manipulating the porosity of silica using a series of organic template groups covalently incorporated into the silicate matrix. The templates in the bridged polysilsesquioxanes are selectively removed from the material by oxidation with oxygen plasma or other means, leaving engineered voids or pores. The size of these pores is dependent upon the length or size of the template or spacer. The size of the templates is measured in terms of Si-Si distances which range from about 0.67 nm to 1.08 nm. Changes introduced by the loss of the templates result in a narrow range of micropores (i.e. <2 nm). Both aryl and alkyl template groups are used as spacers. Novel microporous silica materials useful as molecular sieves, desiccants, and catalyst supports are produced. 3 figs.

  3. Molecular engineering of porous silica using aryl templates

    DOEpatents

    Loy, Douglas A.; Shea, Kenneth J.

    1994-01-01

    A process for manipulating the porosity of silica using a series of organic template groups covalently incorporated into the silicate matrix. The templates in the bridged polysilsesquioxanes are selectively removed from the material by oxidation with oxygen plasma or other means, leaving engineered voids or pores. The size of these pores is dependent upon the length or size of the template or spacer. The size of the templates is measured in terms of Si-Si distances which range from about 0.67 nm to 1.08 nm. Changes introduced by the loss of the templates result in a narrow range of micropores (i.e. <2 nm). Both aryl and alkyl template groups are used as spacers. Novel microporous silica materials useful as molecular seives, dessicants, and catalyst supports are produced.

  4. Nanoelectrospray aerosols from microporous polymer wick sources

    NASA Astrophysics Data System (ADS)

    Tepper, Gary; Kessick, Royal

    2009-02-01

    Nanoelectrospray aerosols were formed from microporous polymer wick sources. Current-voltage characteristics were measured as a function of solution electrical conductivity and surface tension and two distinct electrospray modes were observed. In the first mode, when the maximum capillary flow rate through the wick exceeds the electrospray flow rate, a single electrospray forms from a droplet at the end of the wick. In the second mode, when the maximum capillary flow rate is less than the electrospray flow rate, a multitude of microscopic nanoelectrospray sources are formed from within the surface of the wick tip.

  5. Solvent-resistant microporous polymide membranes

    DOEpatents

    Miller, Warren K.; McCray, Scott B.; Friesen, Dwayne T.

    1998-01-01

    An asymmetric microporous membrane with exceptional solvent resistance and highly desirable permeability is disclosed. The membrane is made by a solution-casting or solution-spinning process from a copolyamic acid comprising the condensation reaction product in a solvent of at least three reactants selected from certain diamines and dianhydrides and post-treated to imidize and in some cases cross-link the copolyamic acid. The membrane is useful as an uncoated membrane for ultrafiltration, microfiltration, and membrane contactor applications, or may be used as a support for a permselective coating to form a composite membrane useful in gas separations, reverse osmosis, nanofiltration, pervaporation, or vapor permeation.

  6. Solvent-resistant microporous polymide membranes

    DOEpatents

    Miller, W.K.; McCray, S.B.; Friesen, D.T.

    1998-03-10

    An asymmetric microporous membrane with exceptional solvent resistance and highly desirable permeability is disclosed. The membrane is made by a solution-casting or solution-spinning process from a copolyamic acid comprising the condensation reaction product in a solvent of at least three reactants selected from certain diamines and dianhydrides and post-treated to imidize and in some cases cross-link the copolyamic acid. The membrane is useful as an uncoated membrane for ultrafiltration, microfiltration, and membrane contactor applications, or may be used as a support for a permselective coating to form a composite membrane useful in gas separations, reverse osmosis, nanofiltration, pervaporation, or vapor permeation.

  7. Microporous polyvinyl chloride: novel reactor for PVC/CaCO3 nanocomposites

    NASA Astrophysics Data System (ADS)

    Xiong, Chuanxi; Lu, Shengjun; Wang, Dongyan; Dong, Lijie; Jiang, David D.; Wang, Qinggang

    2005-09-01

    Microporous polyvinyl chloride (PVC) with pore size of 0.2-2 µm has been obtained by the foaming of PVC powders using a solution of 2,2'-azo-bis-iso-butyronitrile in a co-solvent of butanone and cyclohexanone. The PVC/CaCO3 hybrid powders deposited with CaCO3 nanoparticles have been synthesized using the microporous PVC as reactors of CaCO3 nanoparticles, i.e., the reaction of Ca(OH)2 with CO2 occurs inside the pore of microporous PVC. The in situ PVC/CaCO3 nanocomposites have been prepared by melt blending in situ PVC/CaCO3 hybrid powders. The images of SEM and TEM show that the in situ CaCO3 nanoparticles are uniformly dispersed in the PVC matrix and the sizes of the CaCO3 nanoparticles are less than 50 nm. TEM images and XRD patterns for the in situ CaCO3 strongly suggest that pseudo-amorphous crystals and defect-rich crystals are formed. The mechanical properties and DMA data indicate that the in situ PVC/CaCO3 nanocomposites exhibit much higher strength, toughness, modulus and glass temperature than common PVC/CaCO3 nanocomposites. This novel nanotechnology has potential applications in preparation of organic-inorganic hybrid nanocomposites.

  8. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... as to prevent potential microbial adulteration of the food. (g) To assure safe use of the microporous... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Filters, microporous polymeric. 177.2250 Section 177.2250 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN...

  9. Nanoscale assembly of lanthanum silica with dense and porous interfacial structures

    PubMed Central

    Ballinger, Benjamin; Motuzas, Julius; Miller, Christopher R.; Smart, Simon; Diniz da Costa, João C.

    2015-01-01

    This work reports on the nanoscale assembly of hybrid lanthanum oxide and silica structures, which form patterns of interfacial dense and porous networks. It was found that increasing the molar ratio of lanthanum nitrate to tetraethyl orthosilicate (TEOS) in an acid catalysed sol-gel process alters the expected microporous metal oxide silica structure to a predominantly mesoporous structure above a critical lanthanum concentration. This change manifests itself by the formation of a lanthanum silicate phase, which results from the reaction of lanthanum oxide nanoparticles with the silica matrix. This process converts the microporous silica into the denser silicate phase. Above a lanthanum to silica ratio of 0.15, the combination of growth and microporous silica consumption results in the formation of nanoscale hybrid lanthanum oxides, with the inter-nano-domain spacing forming mesoporous volume. As the size of these nano-domains increases with concentration, so does the mesoporous volume. The absence of lanthanum hydroxide (La(OH)3) suggests the formation of La2O3 surrounded by lanthanum silicate. PMID:25644988

  10. Organically modified silicas on metal nanowires.

    PubMed

    Dean, Stacey L; Stapleton, Joshua J; Keating, Christine D

    2010-09-21

    Organically modified silica coatings were prepared on metal nanowires using a variety of silicon alkoxides with different functional groups (i.e., carboxyl groups, polyethylene oxide, cyano, dihydroimidazole, and hexyl linkers). Organically modified silicas were deposited onto the surface of 6-μm-long, ∼300-nm-wide, cylindrical metal nanowires in suspension by the hydrolysis and polycondensation of silicon alkoxides. Syntheses were performed at several ratios of tetraethoxysilane to an organically modified silicon alkoxide to incorporate desired functional groups into thin organosilica shells on the nanowires. These coatings were characterized using transmission electron microscopy, X-ray photoelectron spectroscopy, and infrared spectroscopy. All of the organically modified silicas prepared here were sufficiently porous to allow the removal of the metal nanowire cores by acid etching to form organically modified silica nanotubes. Additional functionality provided to the modified silicas as compared to unmodified silica prepared using only tetraethoxysilane precursors was demonstrated by chromate adsorption on imidazole-containing silicas and resistance to protein adsorption on polyethyleneoxide-containing silicas. Organically modified silica coatings on nanowires and other nano- and microparticles have potential application in fields such as biosensing or nanoscale therapeutics due to the enhanced properties of the silica coatings, for example, the prevention of biofouling.

  11. Fused silica capillaries with two segments of different internal diameters and inner surface roughnesses prepared by etching with supercritical water and used for volume coupling electrophoresis.

    PubMed

    Horká, Marie; Karásek, Pavel; Roth, Michal; Šlais, Karel

    2017-02-22

    In this work, single-piece fused silica capillaries with two different internal diameter segments featuring different inner surface roughness were prepared by new etching technology with supercritical water and used for volume coupling electrophoresis. The concept of separation and online pre-concentration of analytes in high conductivity matrix is based on the online large-volume sample pre-concentration by the combination of transient isotachophoretic stacking and sweeping of charged proteins in micellar electrokinetic chromatography using non-ionogenic surfactant. The modified surface roughness step helped to the significant narrowing of the zones of examined analytes. The sweeping and separating steps were accomplished simultaneously by the use of phosphate buffer (pH 7) containing ethanol, non-ionogenic surfactant Brij 35, and polyethylene glycol (PEG 10000) after sample injection. Sample solution of a large volume (maximum 3.7 μL) dissolved in physiological saline solution was injected into the wider end of capillary with inlet inner diameter from 150, 185 or 218 μm. The calibration plots were linear (R(2) ∼ 0.9993) over a 0.060-1 μg/mL range for the proteins used, albumin and cytochrome c. The peak area RSDs from at least 20 independent measuremens were below 3.2%. This online pre-concentration technique produced a more than 196-fold increase in sensitivity, and it can be applied for detection of, e.g. the presence of albumin in urine (0.060 μg/mL).

  12. Preparation and characterization of glycidyl methacrylate organo bridges grafted mesoporous silica SBA-15 as ibuprofen and mesalamine carrier for controlled release.

    PubMed

    Rehman, Fozia; Rahim, Abdur; Airoldi, Claudio; Volpe, Pedro L O

    2016-02-01

    Mesoporous silica SBA-15 was synthesized and functionalized with bridged polysilsesquioxane monomers obtained by the reaction of 3-aminopropyltriethoxy silane with glycidyl methacrylate in 2:1 ratio. The synthesized mesoporous silica materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-ray diffraction, thermogravimetry and scanning electron microscopy. The nuclear magnetic resonance in the solid state is in agreement with the sequence of carbon distributed in the attached organic chains, as expected for organically functionalized mesoporous silica. After functionalization with organic bridges the BET surface area was reduced from 1311.80 to 494.2m(2)g(-1) and pore volume was reduced from 1.98 to 0.89cm(3)g(-1), when compared to original precursor silica. Modification of the silica surface with organic bridges resulted in high loading capacity and controlled release of ibuprofen and mesalamine in biological fluids. The Korsmeyer-Peppas model better fits the release data indicating Fickian diffusion and zero order kinetics for synthesized mesoporous silica. The drug release rate from the modified silica was slow in simulated gastric fluid, (pH1.2) where less than 10% of mesalamine and ibuprofen were released in initial 8h, while comparatively high release rates were observed in simulated intestinal (pH6.8) and simulated body fluids (pH7.2). The preferential release of mesalamine at intestinal pH suggests that the modified silica could be a simple, efficient, inexpensive and convenient carrier for colon targeted drugs, such a mesalamine and also as a controlled drug release system.

  13. Superhydrophobicity of silica nanoparticles modified with polystyrene

    NASA Astrophysics Data System (ADS)

    Sun, X. L.; Fan, Z. P.; Zhang, L. D.; Wang, L.; Wei, Z. J.; Wang, X. Q.; Liu, W. L.

    2011-01-01

    Polystyrene/silica nanoparticles were prepared by radical polymerization of silica nanoparticles possessing vinyl groups and styrene with benzoyl peroxide. The resulting vinyl silica nanoparticles, polystyrene/silica nanoparticles were characterized by means of Fourier transformation infrared spectroscopy, scanning electron microscopy and UV-vis absorption spectroscopy. The results indicated that polystyrene had been successfully grafted onto vinyl silica nanoparticles via covalent bond. The morphological structure of polystyrene/silica nanoparticles film, investigated by scanning electron microscopy, showed a characteristic rough structure. Surface wetting properties of the polystyrene/silica nanoparticles film were evaluated by measuring water contact angle and the sliding angle using a contact angle goniometer, which were measured to be 159° and 2°, respectively. The excellent superhydrophobic property enlarges potential applications of the superhydrophobic surfaces.

  14. Fabrication and Characterization of High Aspect Ratio Membranes and Microporous Filters made from PMMA

    NASA Astrophysics Data System (ADS)

    Burant, Alex; Augustine, Brian; Hughes, Chris

    2011-03-01

    This experiment shows a new way to create high aspect ratio membranes and microporous filters by curing a liquid monomer, methyl methacrylate (MMA), into poly(methyl methacrylate) (PMMA) structures. Holes were cut in 200 μ m PMMA sheets by laser cutting. Membranes were made by filling these holes with wax and cooling until the wax solidified. The liquid monomer solution was flowed over the wax-filled holes and photopolymerized to make a thin membrane. The membrane thickness could be controlled by adding 3-10 μ m, 30-50 μ m, or 50-100 μ m silica beads to the monomer solution. Filters were made by filling the holes with curing solution containing 3-10 μ m beads, photopolymerizing, and etching the silica with hydrofluoric acid. The filter porosity could be controlled by varying the weight percentage of silica beads added to the monomer solution. Scanning electron microscopy was used as a method for characterizing both membrane thickness and filter porosity.

  15. Granular bamboo-derived activated carbon for high CO(2) adsorption: the dominant role of narrow micropores.

    PubMed

    Wei, Haoran; Deng, Shubo; Hu, Bingyin; Chen, Zhenhe; Wang, Bin; Huang, Jun; Yu, Gang

    2012-12-01

    Cost-effective biomass-derived activated carbons with a high CO(2) adsorption capacity are attractive for carbon capture. Bamboo was found to be a suitable precursor for activated carbon preparation through KOH activation. The bamboo size in the range of 10-200 mesh had little effect on CO(2) adsorption, whereas the KOH/C mass ratio and activation temperature had a significant impact on CO(2) adsorption. The bamboo-derived activated carbon had a high adsorption capacity and excellent selectivity for CO(2) , and also the adsorption process was highly reversible. The adsorbed amount of CO(2) on the granular activated carbon was up to 7.0 mmol g(-1) at 273 K and 1 bar, which was higher than almost all carbon materials. The pore characteristics of activated carbons responsible for high CO(2) adsorption were fully investigated. Based on the analysis of narrow micropore size distribution of several activated carbons prepared under different conditions, a more accurate micropore range contributing to CO(2) adsorption was proposed. The volume of micropores in the range of 0.33-0.82 nm had a good linear relationship with CO(2) adsorption at 273 K and 1 bar, and the narrow micropores of about 0.55 nm produced the major contribution, which could be used to evaluate CO(2) adsorption on activated carbons.

  16. Fabrication of GaN Microporous Structure at a GaN/Sapphire Interface as the Template for Thick-Film GaN Separation Grown by HVPE

    NASA Astrophysics Data System (ADS)

    Chen, Jianli; Cheng, Hongjuan; Zhang, Song; Lan, Feifei; Qi, Chengjun; Xu, Yongkuan; Wang, Zaien; Li, Jing; Lai, Zhanping

    2016-10-01

    In this paper, a microporous structure at the GaN/sapphire interface has been obtained by an electrochemical etching method via a selective etching progress using an as-grown GaN/sapphire wafer grown by metal organic chemical vapor deposition. The as-prepared GaN interfacial microporous structure has been used as a template for the following growth of thick-film GaN crystal by hydride vapor phase epitaxy (HVPE), facilitating the fabrication of a free-standing GaN substrate detached from a sapphire substrate. The evolution of the interfacial microporous structure has been investigated by varying the etching voltages and time, and the formation mechanism of interfacial microporous structure has been discussed in detail as well. Appropriate interfacial microporous structure is beneficial for separating the thick GaN crystal grown by HVPE from sapphire during the cooling down process. The separation that occurred at the place of interfacial microporous can be attributed to the large thermal strain between GaN and sapphire. This work realized the fabrication of a free-standing GaN substrate with high crystal quality and nearly no residual strain.

  17. Ultra-thin microporous/hybrid materials

    DOEpatents

    Jiang, Ying-Bing [Albuquerque, NM; Cecchi, Joseph L [Albuquerque, NM; Brinker, C Jeffrey [Albuquerque, NM

    2012-05-29

    Ultra-thin hybrid and/or microporous materials and methods for their fabrication are provided. In one embodiment, the exemplary hybrid membranes can be formed including successive surface activation and reaction steps on a porous support that is patterned or non-patterned. The surface activation can be performed using remote plasma exposure to locally activate the exterior surfaces of porous support. Organic/inorganic hybrid precursors such as organometallic silane precursors can be condensed on the locally activated exterior surfaces, whereby ALD reactions can then take place between the condensed hybrid precursors and a reactant. Various embodiments can also include an intermittent replacement of ALD precursors during the membrane formation so as to enhance the hybrid molecular network of the membranes.

  18. Microporous and mesoporous ZSM-5 catalyst for catalytic cracking of C5 raffinate to light olefins.

    PubMed

    Lee, Joongwon; Hong, Ung Gi; Hwang, Sunhwan; Youn, Min Hye; Song, In Kyu

    2014-11-01

    ZSM5 catalysts (PAM(X)-ZSM5) with micropores and mesopores were prepared using polyacrylamide (PAM) as a soft template at different PAM content (X = 0, 0.12, 0.25, 0.53, 0.64, and 0.78 wt%), and they were applied to the production of light olefins (ethylene and propylene) through catalytic cracking of C5 raffinate. The effect of PAM content of PAM(X)-ZSM5 catalysts on the physicochemical properties and catalytic activities was investigated. N2 adsorption-desorption isotherms of PAM(X)-ZSM5 catalysts exhibited a broad hysteresis loop at high relative pressure, indicating the existence of mesopores in the catalysts. It was found that the catalytic performance of PAM(X)-ZSM5 catalysts was closely related to the mesoporosity of the catalysts. Conversion of C5 raffinate and yield for light olefins showed volcano-shaped trends with respect to mesopore/micropore volume ratio of the catalysts. Thus, an optimal PAM content was required to achieve maximum production of light olefins through catalytic cracking of C5 raffinate over microporous and mesoporous PAM(X)-ZSM5 catalysts.

  19. CO2 Capture in the Sustainable Wheat-Derived Activated Microporous Carbon Compartments

    NASA Astrophysics Data System (ADS)

    Hong, Seok-Min; Jang, Eunji; Dysart, Arthur D.; Pol, Vilas G.; Lee, Ki Bong

    2016-10-01

    Microporous carbon compartments (MCCs) were developed via controlled carbonization of wheat flour producing large cavities that allow CO2 gas molecules to access micropores and adsorb effectively. KOH activation of MCCs was conducted at 700 °C with varying mass ratios of KOH/C ranging from 1 to 5, and the effects of activation conditions on the prepared carbon materials in terms of the characteristics and behavior of CO2 adsorption were investigated. Textural properties, such as specific surface area and total pore volume, linearly increased with the KOH/C ratio, attributed to the development of pores and enlargement of pores within carbon. The highest CO2 adsorption capacities of 5.70 mol kg‑1 at 0 °C and 3.48 mol kg‑1 at 25 °C were obtained for MCC activated with a KOH/C ratio of 3 (MCC-K3). In addition, CO2 adsorption uptake was significantly dependent on the volume of narrow micropores with a pore size of less than 0.8 nm rather than the volume of larger pores or surface area. MCC-K3 also exhibited excellent cyclic stability, facile regeneration, and rapid adsorption kinetics. As compared to the pseudo-first-order model, the pseudo-second-order kinetic model described the experimental adsorption data methodically.

  20. Adsorption of pharmaceuticals to microporous activated carbon treated with potassium hydroxide, carbon dioxide, and steam.

    PubMed

    Fu, Heyun; Yang, Liuyan; Wan, Yuqiu; Xu, Zhaoyi; Zhu, Dongqiang

    2011-01-01

    Adsorption of sulfapyridine, tetracycline, and tylosin to a commercial microporous activated carbon (AC) and its potassium hydroxide (KOH)-, CO-, and steam-treated counterparts (prepared by heating at 850°C) was studied to explore efficient adsorbents for the removal of selected pharmaceuticals from water. Phenol and nitrobenzene were included as additional adsorbates, and nonporous graphite was included as a model adsorbent. The activation treatments markedly increased the specific surface area and enlarged the pore sizes of the mesopores of AC (with the strongest effects shown on the KOH-treated AC). Adsorption of large-size tetracycline and tylosin was greatly enhanced, especially for the KOH-treated AC (more than one order of magnitude), probably due to the alleviated size-exclusion effect. However, the treatments had little effect on adsorption of low-size phenol and nitrobenzene due to the predominance of micropore-filling effect in adsorption and the nearly unaffected content of small micropores causative to such effect. These hypothesized mechanisms on pore-size dependent adsorption were further tested by comparing surface area-normalized adsorption data and adsorbent pore size distributions with and without the presence of adsorbed antibiotics. The findings indicate that efficient adsorption of bulky pharmaceuticals to AC can be achieved by enlarging the adsorbent pore size through suitable activation treatments.

  1. CO2 Capture in the Sustainable Wheat-Derived Activated Microporous Carbon Compartments

    PubMed Central

    Hong, Seok-Min; Jang, Eunji; Dysart, Arthur D.; Pol, Vilas G.; Lee, Ki Bong

    2016-01-01

    Microporous carbon compartments (MCCs) were developed via controlled carbonization of wheat flour producing large cavities that allow CO2 gas molecules to access micropores and adsorb effectively. KOH activation of MCCs was conducted at 700 °C with varying mass ratios of KOH/C ranging from 1 to 5, and the effects of activation conditions on the prepared carbon materials in terms of the characteristics and behavior of CO2 adsorption were investigated. Textural properties, such as specific surface area and total pore volume, linearly increased with the KOH/C ratio, attributed to the development of pores and enlargement of pores within carbon. The highest CO2 adsorption capacities of 5.70 mol kg−1 at 0 °C and 3.48 mol kg−1 at 25 °C were obtained for MCC activated with a KOH/C ratio of 3 (MCC-K3). In addition, CO2 adsorption uptake was significantly dependent on the volume of narrow micropores with a pore size of less than 0.8 nm rather than the volume of larger pores or surface area. MCC-K3 also exhibited excellent cyclic stability, facile regeneration, and rapid adsorption kinetics. As compared to the pseudo-first-order model, the pseudo-second-order kinetic model described the experimental adsorption data methodically. PMID:27698448

  2. Silica-supported biomimetic membranes.

    PubMed

    Ariga, Katsuhiko

    2004-01-01

    The hybridization of lipid membranes with inorganic silica-based framework results in mechanically stable biomembrane mimics. This account describes three types of silica-based biomimetic membranes. As the first example, a Langmuir monolayer of dialkylalkoxysilane was polymerized and immobilized onto a porous glass plate. Permeability through the monolayer-immobilized glass was regulated by phase transition of the immobilized monolayer. In the second example, spherical vesicles covalently attached to a silica cover layer (Cerasome) were prepared. The Cerasome was stable enough to be assembled into layer-by-layer films without destruction of its vesicular structure. This material could be an example of the multicellular assembly. Mesoporous silica films densely filling peptide assemblies (Proteosilica) are introduced as the third example. The Proteosilica was synthesized as a transparent film through template sol-gel reaction using amphiphilic peptides.

  3. Effects of CO{sub 2} activation on electrochemical performance of microporous carbons derived from poly(vinylidene fluoride)

    SciTech Connect

    Lee, Seul-Yi; Park, Soo-Jin

    2013-11-15

    In this work, we have prepared microporous carbons (MPCs) derived from poly(vinylidene fluoride) (PVDF), and the physical activation of MPCs using CO{sub 2} gas is subsequently carried out with various activation temperatures to investigate the electrochemical performance. PVDF is successfully converted into MPCs with a high specific surface area and well-developed micropores. After CO{sub 2} activation, the specific surface areas of MPCs (CA-MPCs) are enhanced by 12% compared with non-activated MPCs. With increasing activation temperature, the micropore size distributions of A-MPCs also become narrower and shift to larger pore size. It is also confirmed that the CO{sub 2} activation had developed the micropores and introduced the oxygen-containing groups to MPCs′ surfaces. From the results, the specific capacitances of the electrodes in electric double layer capacitors (EDLCs) based on CA-MPCs are distinctly improved through CO{sub 2} activation. The highest specific capacitance of the A-MPCs activated at 700 °C is about 125 F/g, an enhancement of 74% in comparison with NA-MPCs, at a discharge current of 2 A/g in a 6 M KOH electrolyte solution. We also found that micropore size of 0.67 nm has a specific impact on the capacitance behaviors, besides the specific surface area of the electrode samples. - Graphical abstract: The A-MPC samples with high specific surface area (ranging from 1030 to 1082 m{sup 2}/g), corresponding to micropore sizes of 0.67 and 0.72 nm, and with the amount of oxygen-containing groups ranging from 3.2% to 4.4% have been evaluated as electrodes for EDLC applications. . Display Omitted - Highlights: • Microporous carbons (MPCs) were synthesized without activation process. • Next, we carried out the CO{sub 2} activation of MPCs with activation temperatures. • It had developed the micropores and introduced the O-functional groups to MPCs. • The highest specific capacitance: 125 F/g, an increase of 74% compared to MPCs.

  4. The Effect of Microporous Polymeric Support Modification on Surface and Gas Transport Properties of Supported Ionic Liquid Membranes

    PubMed Central

    Akhmetshina, Alsu A.; Davletbaeva, Ilsiya M.; Grebenschikova, Ekaterina S.; Sazanova, Tatyana S.; Petukhov, Anton N.; Atlaskin, Artem A.; Razov, Evgeny N.; Zaripov, Ilnaz I.; Martins, Carla F.; Neves, Luísa A.; Vorotyntsev, Ilya V.

    2015-01-01

    Microporous polymers based on anionic macroinitiator and toluene 2,4-diisocyanate were used as a support for 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim][PF6]) and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([emim][Tf2N]) immobilization. The polymeric support was modified by using silica particles associated in oligomeric media, and the influence of the modifier used on the polymeric structure was studied. The supported ionic liquid membranes (SILMs) were tested for He, N2, NH3, H2S, and CO2 gas separation and ideal selectivities were calculated. The high values of ideal selectivity for ammonia-based systems with permanent gases were observed on polymer matrixes immobilized with [bmim][PF6] and [emim][Tf2N]. The modification of SILMs by nanosize silica particles leads to an increase of NH3 separation relatively to CO2 or H2S. PMID:26729177

  5. The Effect of Microporous Polymeric Support Modification on Surface and Gas Transport Properties of Supported Ionic Liquid Membranes.

    PubMed

    Akhmetshina, Alsu A; Davletbaeva, Ilsiya M; Grebenschikova, Ekaterina S; Sazanova, Tatyana S; Petukhov, Anton N; Atlaskin, Artem A; Razov, Evgeny N; Zaripov, Ilnaz I; Martins, Carla F; Neves, Luísa A; Vorotyntsev, Ilya V

    2015-12-30

    Microporous polymers based on anionic macroinitiator and toluene 2,4-diisocyanate were used as a support for 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim][PF₆]) and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([emim][Tf₂N]) immobilization. The polymeric support was modified by using silica particles associated in oligomeric media, and the influence of the modifier used on the polymeric structure was studied. The supported ionic liquid membranes (SILMs) were tested for He, N₂, NH₃, H₂S, and CO₂ gas separation and ideal selectivities were calculated. The high values of ideal selectivity for ammonia-based systems with permanent gases were observed on polymer matrixes immobilized with [bmim][PF₆] and [emim][Tf₂N]. The modification of SILMs by nanosize silica particles leads to an increase of NH₃ separation relatively to CO₂ or H₂S.

  6. Inorganic-organic hybrid silica based tin complex as a novel, highly efficient and recyclable heterogeneous catalyst for the one-pot preparation of spirooxindoles in water.

    PubMed

    Ghahremanzadeh, Ramin; Rashid, Zahra; Zarnani, Amir-Hassan; Naeimi, Hossein

    2014-11-14

    In the present study, a tin complex immobilized on silica gel as a novel, green, highly efficient and heterogeneous reusable catalyst was synthesized by grafting 2-amino benzamide onto the silica gel surface as a result of the reaction between isatoic anhydride and 3-aminopropyl-functionalized silica gel, followed by complexing with tin chloride. The resulting organic-inorganic hybrid material was evaluated in the one-pot three-component synthesis of spiro[indoline-pyrazolo[4',3':5,6]pyrido[2,3-d]pyrimidine]trione derivatives in water via the condensation reaction of isatins, barbituric acids, and 1H-pyrazol-5-amines. All the reactions were completed in short reaction times and all the products were obtained in high to excellent yields with high purity. In addition, the synthesized novel catalyst could be separated from the reaction mixture by simple filtration and can be reused up to seven runs without significant loss in activity.

  7. Controlled synthesis of uniform palladium nanoparticles on novel micro-porous carbon as a recyclable heterogeneous catalyst for the Heck reaction.

    PubMed

    Song, Kunpeng; Liu, Peng; Wang, Jingyu; Pang, Lei; Chen, Jian; Hussain, Irshad; Tan, Bien; Li, Tao

    2015-08-21

    Novel dual-porous carbon-supported palladium nanoparticle (Pd NP) catalysts were prepared by sequential carbonization and reduction of microporous organic polymer-encaged PdCl2. The diverse pore structure of microporous organic polymers provides a reservoir for the palladium precursors and prevents Pd NPs from sintering during the carbonization and reaction. The microporous structure has a significant effect on the size and dispersion of palladium NPs. The average size of the Pd NPs (in the range of 4-6 nm) was tuned by changing the pore size distribution and the carbonization temperature. The resulting carbon-supported Pd NPs were characterized by TEM, BET, XRD, and XPS and the Pd loading was calculated by AAS. The encaged Pd NP catalysts prepared by this methodology exhibited outstanding stability and reusability in the Heck reaction and could be reused at least 10 times without appreciable loss of activity.

  8. Matrix effects on the photocatalytic oxidation of alcohols by [nBu4N]4W10O32 incorporated into sol-gel silica.

    PubMed

    Molinari, Alessandra; Bratovcic, Amra; Magnacca, Giuliana; Maldotti, Andrea

    2010-09-07

    Two heterogeneous photocatalysts have been prepared by entrapment of [nBu(4)N](4)W(10)O(32) in a silica matrix, through a sol-gel procedure: SiO(2)/W30% and SiO(2)/W10% with 30% and 10% of decatungstate, respectively. They are characterized by the presence of micropores of about 7 A and 15 A and mesopores of about 25 A. Due to different preparation procedures, SiO(2)/W10% presents a more remarkable porous network than SiO(2)/W30%. The morphological features of SiO(2)/W30% and SiO(2)/W10% differ from those of their parent material SiO(2)/W0%, indicating that incorporation of the decatungstate induces a significant modification of the porous texture of the siliceous material. These photocatalysts demonstrate good stability in the oxygen-assisted photooxidation of 1-pentanol and 3-pentanol, which have been chosen as models of primary and secondary aliphatic alcohols. In particular, photoexcitation (lambda > 290 nm, 25 degrees C, 760 torr of O(2)) leads to conversion of these two substrates to pentanal or 3-pentanone, with a mass balance of about 90%. There is a strong effect of the solid support on the reactivity of the two alcoholic substrates. In particular, oxidation of 1-pentanol with SiO(2)/W10% is about four times faster than with [nBu(4)N](4)W(10)O(32) in homogeneous solution. Preferential adsorption phenomena, due to the hydrophilic character of silica explain the photocatalytic properties of the two heterogeneous systems, because adsorption favours the contact between the photoexcited decatungstate and the primary OH group of 1-pentanol. Moreover, some kind of shape selectivity, due to the microporous structure of the investigated materials, likely contributes to control the conversion yields.

  9. Mesoporous silica coated silica-titania spherical particles: from impregnation to core-shell formation.

    PubMed

    Shiba, Kota; Takei, Toshiaki; Ogawa, Makoto

    2016-11-22

    The coating of solid surfaces with inorganic materials is a promising approach not only to impart various functionalities but also to modify physicochemical properties that are affected by the geometry/structure of the coating. In this study, a silica-hexadecyltrimethylammonium (silica-CTA) hybrid layer was deposited on monodispersed spherical particles composed of titania and octadecylamine (titania-ODA) by a sol-gel reaction of tetraethoxysilane in aqueous CTA/ammonia/methanol solution. The formation of the coating was confirmed by SEM and TEM observations. The coating thickness varied from a few nm to 100 nm depending on the Si/Ti ratio. We found that Si/Ti = 0.68 resulted in the formation of microporous silica-titania particles with the pore size of 0.7 nm as revealed by nitrogen adsorption/desorption measurements. Because the titania-ODA particles can be converted to mesoporous titania particles after removing ODA by acid/base treatment, the silica species can be impregnated into the titania particles and replace ODA under basic conditions. By increasing the Si/Ti molar ratio up to 1.4, silica-titania particles with non-porous structures were obtained. An amorphous to anatase transition occurred at around 800 °C, indicating the complete impregnation of silica inside the titania particles. Further increases of the Si/Ti molar ratio (to 3.4 and 6.8) led to the formation of the silica-CTA shell on the core particles, and the shell was converted to mesoporous silica layers with a pore size of 2 nm after calcination at 550 °C for 5 h. Non-linear control of the pore size/structure is presented for the first time; this will be useful for the precise design of diverse hybrid materials for optical, catalytic and biomedical applications.

  10. Fluoride-assisted synthesis of bimodal microporous SSZ-13 zeolite.

    PubMed

    Zhu, Xiaochun; Kosinov, Nikolay; Hofmann, Jan P; Mezari, Brahim; Qian, Qingyun; Rohling, Roderigh; Weckhuysen, Bert M; Ruiz-Martínez, Javier; Hensen, Emiel J M

    2016-02-21

    The presence of small amount of fluoride in alkaline hydrothermal synthesis of SSZ-13 zeolite yields bimodal microporous particles with substantially improved performance in the methanol-to-olefins (MTO) reaction. Hydrocarbon uptake measurements and fluorescence microspectroscopy of spent catalysts demonstrate enhanced diffusion through micropores at the grain boundaries of nanocrystals running through the zeolite particles. Fluoride-assisted SSZ-13 synthesis is a cheap and scalable approach to optimize the performance of MTO zeolite catalysts.

  11. Microporous polymer films and methods of their production

    DOEpatents

    Aubert, J.H.

    1995-06-06

    A process is described for producing thin microporous polymeric films for a variety of uses. The process utilizes a dense gas (liquefied gas or supercritical fluid) selected to combine with a solvent-containing polymeric film so that the solvent is dissolved in the dense gas, the polymer is substantially insoluble in the dense gas, and two phases are formed. A microporous film is obtained by removal of a dense gas-solvent phase. 9 figs.

  12. Microporous polymer films and methods of their production

    DOEpatents

    Aubert, James H.

    1995-01-01

    A process for producing thin microporous polymeric films for a variety of uses. The process utilizes a dense gas (liquified gas or supercritical fluid) selected to combine with a solvent-containing polymeric film so that the solvent is dissolved in the dense gas, the polymer is substantially insoluble in the dense gas, and two phases are formed. A microporous film is obtained by removal of a dense gas-solvent phase.

  13. In situ formed lithium sulfide/microporous carbon cathodes for lithium-ion batteries.

    PubMed

    Zheng, Shiyou; Chen, Yvonne; Xu, Yunhua; Yi, Feng; Zhu, Yujie; Liu, Yihang; Yang, Junhe; Wang, Chunsheng

    2013-12-23

    Highly stable sulfur/microporous carbon (S/MC) composites are prepared by vacuum infusion of sulfur vapor into microporous carbon at 600 °C, and lithium sulfide/microporous carbon (Li2S/MC) cathodes are fabricated via a novel and facile in situ lithiation strategy, i.e., spraying commercial stabilized lithium metal powder (SLMP) onto a prepared S/MC film cathode prior to the routine compressing process in cell assembly. The in situ formed Li2S/MC film cathode shows high Coulombic efficiency and long cycling stability in a conventional commercial Li-ion battery electrolyte (1.0 M LiPF6 + EC/DEC (1:1 v/v)). The reversible capacities of Li2S/MC cathodes remain about 650 mAh/g even after 900 charge/discharge cycles, and the Coulombic efficiency is close to 100% at a current density of 0.1C, which demonstrates the best electrochemical performance of Li2S/MC cathodes reported to date. Furthermore, this Li2S/MC film cathode fabricated via our in situ lithiation strategy can be coupled with a Li-free anode, such as graphite, carbon/tin alloys, or Si nanowires to form a rechargeable Li-ion cell. As the Li2S/MC cathode is paired with a commercial graphite anode, the full cell of Li2S/MC-graphite (Li2S-G) shows a stable capacity of around 600 mAh/g in 150 cycles. The Li2S/MC cathodes prepared by high-temperate sulfur infusion and SLMP prelithiation before cell assembly are ready to fit into current Li-ion batteries manufacturing processes and will pave the way to commercialize low-cost Li2S-G Li-ion batteries.

  14. SANS Investigations of CO2 Adsorption in Microporous Carbon

    DOE PAGES

    Bahadur, Jitendra; Melnichenko, Yuri B.; He, Lilin; ...

    2015-08-07

    The high pressure adsorption behavior of CO2 at T = 296 K in microporous carbon was investigated by small-angle neutron scattering (SANS) technique. A strong densification of CO2 in micropores accompanied by non-monotonic adsorption-induced pore deformation was observed. The density of confined CO2 increases rapidly with pressure and reaches the liquid –like density at 20 bar, which corresponds to the relative pressure of P/Psat ~0.3. At P > 20 bar density of confined CO2 increases slowly approaching a plateau at higher pressure. The size of micropores first increases with pressure, reaches a maximum at 20 bar,more » and then decreases with pressure. A complementary SANS experiment conducted on the same microporous carbon saturated with neutron-transparent and non-adsorbing inert gas argon shows no deformation of micropores at pressures up to ~200 bars. This result demonstrates that the observed deformation of micropores in CO2 is an adsorption-induced phenomenon, caused by the solvation pressure - induced strain and strong densification of confined CO2 .« less

  15. Hydrothermal synthesis of hollow silica spheres under acidic conditions.

    PubMed

    Yu, Qiyu; Wang, Pengpeng; Hu, Shi; Hui, Junfeng; Zhuang, Jing; Wang, Xun

    2011-06-07

    It is well-known that silica can be etched in alkaline media or in a unique hydrofluoric acid (HF) solution, which is widely used to prepare various kinds of hollow nanostructures (including silica hollow structures) via silica-templating methods. In our experiments, we found that stöber silica spheres could be etched in generic acidic media in a well-controlled way under hydrothermal conditions, forming well-defined hollow/rattle-type silica spheres. Furthermore, some salts such as NaCl and Na(2)SO(4) were found to be favorable for the formation of hollow/rattle-type silica spheres.

  16. Experimental and molecular mechanics and ab initio investigation of activated adsorption and desorption of trichloroethylene in mineral micropores.

    PubMed

    Farrell, James; Luo, Jing; Blowers, Paul; Curry, Joan

    2002-04-01

    This research investigated activated adsorption of a hydrophobic organic contaminant(HOC) in mineral micropores using experimental and molecular modeling techniques. Adsorption of trichloroethylene (TCE) on a silica gel adsorbent was measured using a frontal analysis chromatography technique at atmospheric and elevated fluid pressures. Increasing the fluid pressure yielded increased TCE uptake that was not released upon lowering the pressure back to atmospheric conditions. This showed that the increase in pressure was able to rapidly induce the formation of a desorption-resistant fraction that previous investigations have shown requires months to develop at atmospheric pressure. Grand Canonical Monte Carlo (GCMC) modeling was then used to elucidate the nature of water and TCE behavior within silica micropores. The GCMC modeling showed that molecular scale packing restrictions resulted in pore fluid densities that ranged from 0.28 to 0.78 of those in the bulk solution. The modeling also showed that TCE was able to displace water from hydrophilic mineral pores due to molecular scale packing restrictions. Exothermic isosteric heats for TCE adsorption up to -27 kJ/mol were observed and were greatest in pores of 7 and 8 A. This indicated that TCE adsorption was energetically most favorable in pores that were minimally large enough to accommodate a TCE molecule. The pressure-induced uptake appeared to result primarily from an increase in the packing density in the smallest pores. Ab initio calculations showed that small distortions of a TCE molecule from its low energy conformation require high activation energies. Results from this study indicate that activated adsorption requiring bond angle distortions in the adsorbate may be responsible forthe slow attainment of adsorptive equilibrium of HOCs on microporous solids. Likewise, activated desorption from molecular-sized adsorption sites may contribute to the slow release of HOCs from aquifer sediments.

  17. Preparation of chitin-silica composites by in vitro silicification of two-dimensional Ianthella basta demosponge chitinous scaffolds under modified Stöber conditions.

    PubMed

    Wysokowski, Marcin; Behm, Thomas; Born, René; Bazhenov, Vasilii V; Meissner, Heike; Richter, Gert; Szwarc-Rzepka, Karolina; Makarova, Anna; Vyalikh, Denis; Schupp, Peter; Jesionowski, Teofil; Ehrlich, Hermann

    2013-10-01

    Chitin is a biopolymer found in cell walls of various fungi and skeletal structures of numerous invertebrates. The occurrence of chitin within calcium- and silica-containing biominerals has inspired development of chitin-based hybrids and composites in vitro with specific physico-chemical and material properties. We show here for the first time that the two-dimensional α-chitin scaffolds isolated from the skeletons of marine demosponge Ianthella basta can be effectively silicified by the two-step method with the use of Stöber silica micro- and nanodispersions under Extreme Biomimetic conditions. The chitin-silica composites obtained at 120 °C were characterized by the presence of spherical SiO2 particles homogeneously distributed over the chitin fibers, which probably follows from the compatibility of Si-OH groups to the hydroxyl groups of chitin. The biocomposites obtained were characterized by various analytical techniques such as energy dispersive spectrometry, scanning electron microscopy, thermogravimetric/differential thermal analyses as well as X-ray photoelectron spectroscopy, Fourier transform infrared and Raman spectroscopy to determine possible interactions between silica and chitin molecule. The results presented proved that the character and course of the in vitro chitin silicification in Stöber dispersions depended considerably on the degree of hydrolysis of the SiO2 precursor.

  18. Structure-Property Relationships in Porous 3-D Nanostructures as a Function of Preparation Conditions: Isocyanate Cross-Linked Silica Aerogels

    NASA Technical Reports Server (NTRS)

    Meador, Mary Ann B.; Capadona, Lynn A.; McCorkle, Linda; Padadopoulos, Demetrios S.; Leventis, Nicholas

    2007-01-01

    Sol-gel derived silica aerogels are attractive candidates for many unique thermal, optical, catalytic, and chemical applications because of their low density and high mesoporosity. However, their inherent fragility has restricted use of aerogel monoliths to applications where they are not subject to any load. We have previously reported cross-linking the mesoporous silica structure of aerogels with di-isocyanates, styrenes or epoxies reacting with amine decorated silica surfaces. These approaches have been shown to significantly increase the strength of aerogels with only a small effect on density or porosity. Though density is a prime predictor of properties such as strength and thermal conductivity for aerogels, it is becoming clear from previous studies that varying the silica backbone and size of the polymer cross-link independently can give rise to combinations of properties which cannot be predicted from density alone. Herein, we examine the effects of four processing parameters for producing this type of polymer cross-linked aerogel on properties of the resulting monoliths. We focus on the results of C-13 CP-MAS NMR which gives insight to the size and structure of polymer cross-link present in the monoliths, and relates the size of the cross-links to microstructure, mechanical properties and other characteristics of the materials obtained.

  19. Structure-Property Relationships in Porous 3-D Nanostructures as a Function of Preparation Conditions: Isocyanate Cross-Linked Silica Aerogels

    NASA Technical Reports Server (NTRS)

    Meador, Mary Ann B.; Capadona, Lynn A.; McCorkle, Linda; Papadopoulos, Demetrios S.; Leventis, Nicholas

    2007-01-01

    Sol-gel derived silica aerogels are attractive candidates for many unique thermal, optical, catalytic, and chemical applications because of their low density and high mesoporosity. However, their inherent fragility has restricted use of aerogel monoliths to applications where they are not subject to any load. We have previously reported cross-linking the mesoporous silica structure of aerogels with di-isocyanates, styrenes or epoxies reacting with amine decorated silica surfaces. These approaches have been shown to significantly increase the strength of aerogels with only a small effect on density or porosity. Though density is a prime predictor of properties such as strength and thermal conductivity for aerogels, it is becoming clear from previous studies that varying the silica backbone and size of the polymer cross-link independently can give rise to combinations of properties which cannot be predicted from density alone. Herein, we examine the effects of four processing parameters for producing this type of polymer cross-linked aerogel on properties of the resulting monoliths. We focus on the results of 13C CP-MAS NMR which gives insight to the size and structure of polymer cross-link present in the monoliths, and relates the size of the cross-links to microstructure, mechanical properties and other characteristics of the materials obtained.

  20. Preparation of an aminopropyl imidazole-modified silica gel as a sorbent for solid-phase extraction of carboxylic acid compounds and polycyclic aromatic hydrocarbons.

    PubMed

    Wang, Na; Guo, Yong; Wang, Licheng; Liang, Xiaojing; Liu, Shujuan; Jiang, Shengxiang

    2014-05-21

    In this paper, a kind of aminopropyl imidazole-modified silica sorbent was synthesized and used as a solid-phase extraction (SPE) sorbent for the determination of carboxylic acid compounds and polycyclic aromatic hydrocarbons (PAHs). The resultant aminopropyl imidazole-modified silica sorbent was characterized by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to ensure the successful binding of aminopropyl imidazole on the surface of silica gel. Then the aminopropyl imidazole-modified silica sorbent served as a SPE sorbent for the enrichment of carboxylic acid compounds and PAHs. The new sorbent exhibited high extraction efficiency towards the tested compounds and the results show that such a sorbent can offer multiple intermolecular interactions: electrostatic, π-π, and hydrophobic interactions. Several parameters affecting the extraction recovery, such as the pH of sample solution, the pH of eluent, the solubility of eluent, the volume of eluent, and sample loading, were also investigated. Under the optimized conditions, the proposed method was applied to the analysis of four carboxylic acid compounds and four PAHs in environmental water samples. Good linearities were obtained for all the tested compounds with R(2) larger than 0.9903. The limits of detection were found to be in the range of 0.0065-0.5 μg L(-1). The recovery values of spiked river water samples were from 63.2% to 112.3% with relative standard deviations (RSDs) less than 10.1% (n = 4).

  1. A new approach for the preparation of well-defined Rh and Pt nanoparticles stabilized by phosphine-functionalized silica for selective hydrogenation reactions.

    PubMed

    Llop Castelbou, J; Szeto, K C; Barakat, W; Merle, N; Godard, C; Taoufik, M; Claver, C

    2017-03-18

    In this work, a new methodology for the synthesis of well-defined metallic nanoparticles supported on silica is described. This methodology is based on the surface control provided by SOMC. The nanoparticles are formed via the organometallic approach and are catalytically active in the hydrogenation of p-xylene, 3-hexyne, 4-phenyl-2 butanone, benzaldehyde, and furfural.

  2. Dynamic nuclear polarization NMR spectroscopy allows high-throughput characterization of microporous organic polymers.

    PubMed

    Blanc, Frédéric; Chong, Samantha Y; McDonald, Tom O; Adams, Dave J; Pawsey, Shane; Caporini, Marc A; Cooper, Andrew I

    2013-10-16

    Dynamic nuclear polarization (DNP) solid-state NMR was used to obtain natural abundance (13)C and (15)N CP MAS NMR spectra of microporous organic polymers with excellent signal-to-noise ratio, allowing for unprecedented details in the molecular structure to be determined for these complex polymer networks. Sensitivity enhancements larger than 10 were obtained with bis-nitroxide radical at 14.1 T and low temperature (∼105 K). This DNP MAS NMR approach allows efficient, high-throughput characterization of libraries of porous polymers prepared by combinatorial chemistry methods.

  3. Activated microporous materials through polymerization of microemulsion precursors

    NASA Astrophysics Data System (ADS)

    Venkatesan, Arunkumar

    Microemulsions have been well studied for their unique characteristics. They are isotropic, thermodynamically stable and microstructured mixtures of oil and water stabilized by one or more surfactant species. They are formed spontaneously and are thermodynamically stable. Microemulsion precursors can be polymerized to make microporous solids with controlled pore structure and sizes. These polymeric solids have been studied extensively in the past. Although the fundamental properties of the microporous solids have been studied in depth, the development of specific applications that will utilize the unique properties of these solids has not been exhaustively researched. The current work establishes the feasibility of making activated microporous solids from microemulsion precursors, by the use of a ligand that chelates metals and also attaches itself to the polymer monolith. It also uses a novel 'in-situ' incorporation by combining the formulation and incorporation steps into one. The research objectives are, to formulate a microemulsion system that can yield useful microporous solids upon polymerization and activation, to characterize these solids using existing techniques available for analysis of similar microporous solids, to identify and understand the effect of the variables in the system and to study the influence of these variables on the performance characteristics of this material. Characterization techniques like Differential Scanning Calorimetry, Thermogravimetric Analysis and Scanning Electron Microscopy were used. A hydroxyethylmethylmethacrylate/methylmethacrylate/aqueous phase containing 10% SDS' system was chosen as the precursor microemulsion and the corresponding microporous solids were made. A metal chelating ligand, Congo Red, was incorporated onto the microporous polymer using NaOH as a binding agent. The ability of the resultant 'activated' microporous solid to remove metal ions from solution, was evaluated. The metal ion chosen was chromium

  4. Optical and Geometric Properties of Free Silica Nanoparticles Studied by Small-Angle X-Ray Scattering

    NASA Astrophysics Data System (ADS)

    Langer, Burkhard; Raschpichler, Christopher; Gruner, Mathias; Antonsson, Egill; Goroncy, Christian; Graf, Christina; Rühl, Eckart

    2016-09-01

    Elastic small-angle X-ray scattering (SAXS) of free silica (SiO2) nanoparticles is reported (d = 100-180 nm). The particles were prepared by a modified Stöber synthesis in narrow size distributions with controlled surface roughness and functionalization. Angle-resolved small-angle X-ray scattering patterns are shown to be sensitive to these changes in particle properties. It is reported that there is an exponential decrease in scattered X-ray intensity towards larger scattering angles as well as distinct oscillations, which is fully explained by Mie theory. Small-angle X-ray scattering of mesoporous nanoparticles with rough surfaces is compared to that of microporous nanoparticles with smooth surfaces, revealing distinct differences that are rationalized by diffuse scattering from nanoparticle pores in addition to the dominating contribution of Mie scattering. Furthermore, results from small-angle X-ray scattering experiments on functionalized silica nanoparticles are presented, where the incorporation of the dye fluorescein isothiocyanate is found to cause changes in the optical properties of the nanoparticles, as compared to non-functionalized samples. Small, but distinct deviations in particle size derived from electron microscopy and from small-angle X-ray scattering are observed. These are rationalized by particle shrinking occurring in electron microscopy as well as slight changes in optical properties of the nanoparticle samples.

  5. Synthesis and characterization by FTIR spectroscopy of silica aerogels prepared using several Si(OR)4 and R‧‧Si(OR‧)3 precursors

    NASA Astrophysics Data System (ADS)

    Al-Oweini, Rami; El-Rassy, Houssam

    2009-02-01

    We report the synthesis and Fourier Transform Infrared spectroscopy characterization results dealing with the surface modification of silica aerogels obtained via a two-step sol-gel process where various silicon precursors and co-precursors were used. The hydrolysis and poly-condensation steps were followed by carbon dioxide supercritical drying ( Tc = 31.1 °C; Pc = 73.7 bar). The silicon precursors contain four identical hydrolysable alkoxy groups (methoxy or ethoxy), while in the co-precursors, one of the alkoxy groups is substituted by a non-hydrolysable alkyl group (methyl, ethyl, n-propyl, iso-butyl, n-octyl, vinyl or phenyl). Identically, surface-functionalized silica aerogels were obtained from various silicon precursor/co-precursor combinations and their chemical structures were compared. The infrared spectroscopy revealed the existence of chemically comparable solid networks with some differences due to the nature of the silicon precursors.

  6. Cation siting in low-silica zeolites with potential applications in pressure swing adsorption technology and structural studies of novel tectosilicates

    NASA Astrophysics Data System (ADS)

    Burton, Allen Wayne

    Adsorption and catalytic phenomena in zeolites are influenced by coulombic interactions within zeolite structure as well as by size restrictions imposed by zeolitic micropores. In the first part of this thesis, we investigate materials with potential applications in the selective adsorption of nitrogen. Studies have indicated the performance of LiX adsorbents correlates with the number of accessible lithium cations in the zeolite. However, in zeolite LiX only one-third of the lithium cations interact with adsorbed molecules. This prompted our investigation of other low-silica zeolites. The first zeolite examined was a cancrinite prepared in the presence of 1,3-butanediol. Neutron diffraction studies on the lithium-exchanged cancrinite suggest most of the lithium cations are ideally positioned within the micropores. However, our experiments show that carbonate anions are occluded within the micropores of this cancrinite. Another material examined in this study was zeolite (Ba,K)-GL. Neutron diffraction experiments show that 49 of the extraframework charges are located in the micropores. Unfortunately, less than 20% of these cations are replaced after lithium-exchange. We also attempted to directly synthesize a (Ba,Li)-GL. However, diffraction experiments and chemical analyses show that most of the extraframework charge is compensated by barium. Because of molecular size restrictions imposed by currently known zeolites, there is continued interest in the synthesis of materials that can be used for processing large molecules. This motivated our investigation of two tectosilicates MCM-61 and MCM-47. MCM-61 is an aluminosilicate made in the presence of the potassium-18-Crown-6 complex. Our structure solution shows MCM-61 is formed from novel [610412] polyhedral cage units that connect to form 18-membered-ring cages. The structure of MCM-61 suggests that crown ethers, azamacrocycles, and cryptands may be useful for the syntheses of extra-large pore zeolites. MCM-47 is

  7. Fabrication of microporous calcite block from calcium hydroxide compact under carbon dioxide atmosphere at high temperature.

    PubMed

    Otsu, Akihiro; Tsuru, Kanji; Maruta, Michito; Munar, Melvin L; Matsuya, Shigeki; Ishikawa, Kunio

    2012-01-01

    Effects of carbonation temperature and compacting pressure on basic properties of calcite block were studied using Ca(OH)2 compact made with 0.2-2.0 MPa and their carbonation at 200-800ºC for 1 h. Microporous calcite was obtained only when carbonated at 600ºC using Ca(OH)2 compact made with 0.2 MPa even though thermogravimetry analysis showed that calcite powder was stable up to 920ºC under CO2 atmosphere. CaO formed by carbonation at 700ºC and 800ºC is thought to be caused by the limited CO2 diffusion interior to the Ca(OH)2 compact. Also, unreacted Ca(OH)2 was found for Ca(OH)2 compact prepared with 0.5 MPa or higher pressure even when carbonated at 600ºC. As a result of high temperature carbonation, crystallite size of the calcite, 58.0 nm, was significantly larger when compared to that of calcite prepared at room temperature, 35.5 nm. Porosity and diametral tensile strength of the microporous calcite were 39.5% and 6.4 MPa.

  8. Responsive Guest Encapsulation of Dynamic Conjugated Microporous Polymers.

    PubMed

    Xu, Lai; Li, Youyong

    2016-06-30

    The host-guest complexes of conjugated microporous polymers encapsulating C60 and dye molecules have been investigated systematically. The orientation of guest molecules inside the cavities, have different terms: inside the open cavities of the polymer, or inside the cavities formed by packing different polymers. The host backbone shows responsive dynamic behavior in order to accommodate the size and shape of incoming guest molecule or guest aggregates. Simulations show that the host-guest binding of conjugated polymers is stronger than that of non-conjugated polymers. This detailed study could provide a clear picture for the host-guest interaction for dynamic conjugated microporous polymers. The mechanism obtained could guide designing new conjugated microporous polymers.

  9. Responsive Guest Encapsulation of Dynamic Conjugated Microporous Polymers

    PubMed Central

    Xu, Lai; Li, Youyong

    2016-01-01

    The host-guest complexes of conjugated microporous polymers encapsulating C60 and dye molecules have been investigated systematically. The orientation of guest molecules inside the cavities, have different terms: inside the open cavities of the polymer, or inside the cavities formed by packing different polymers. The host backbone shows responsive dynamic behavior in order to accommodate the size and shape of incoming guest molecule or guest aggregates. Simulations show that the host-guest binding of conjugated polymers is stronger than that of non-conjugated polymers. This detailed study could provide a clear picture for the host-guest interaction for dynamic conjugated microporous polymers. The mechanism obtained could guide designing new conjugated microporous polymers. PMID:27356483

  10. Micropore and nanopore fabrication in hollow antiresonant reflecting optical waveguides

    PubMed Central

    Holmes, Matthew R.; Shang, Tao; Hawkins, Aaron R.; Rudenko, Mikhail; Measor, Philip; Schmidt, Holger

    2011-01-01

    We demonstrate the fabrication of micropore and nanopore features in hollow antiresonant reflecting optical waveguides to create an electrical and optical analysis platform that can size select and detect a single nanoparticle. Micropores (4 μm diameter) are reactive-ion etched through the top SiO2 and SiN layers of the waveguides, leaving a thin SiN membrane above the hollow core. Nanopores are formed in the SiN membranes using a focused ion-beam etch process that provides control over the pore size. Openings as small as 20 nm in diameter are created. Optical loss measurements indicate that micropores did not significantly alter the loss along the waveguide. PMID:21922035

  11. Synthesis of microporous boron-substituted carbon (b/c) materials using polymeric precursors for hydrogen physisorption.

    PubMed

    Chung, T C Mike; Jeong, Youmi; Chen, Qiang; Kleinhammes, Alfred; Wu, Yue

    2008-05-28

    This paper discusses a new synthesis route to prepare microporous boron substituted carbon (B/C) materials that show a significantly higher hydrogen binding energy and physisorption capacity, compared with the corresponding carbonaceous (C) materials. The chemistry involves a pyrolysis of the designed boron-containing polymeric precursors, which are the polyaddition and polycondensation adducts between BCl3 and phenylene diacetylene and lithiated phenylene diacetylene, respectively. During pyrolysis, most of the boron moieties were transformed into a B-substituted C structure, and the in situ formed LiCl byproduct created a microporous structure. The microporous B/C material with B content > 7% and surface area > 700 m2/g has been prepared, which shows a reversible hydrogen physisorption capacity of 0.6 and 3.2 wt % at 293 and 77 K, respectively, under 40 bar of hydrogen pressure. The physisorption results were further warranted by absorption isotherms indicating a binding energy of hydrogen molecules of approximately 11 kJ/mol, significantly higher than the 4 kJ/mol reported on most graphitic surfaces.

  12. Infrared spectra of silica polymorphs

    NASA Astrophysics Data System (ADS)

    Koike, C.; Noguchi, R.; Chihara, H.; Suto, H.; Ohtaka, O.; Imai, Y.; Matsumoto, T.; Tsuchiyama, A.

    The existence of silica within several debris disks has been suggested. We investigate the annealing conditions of α-cristobalite, and further prepare various types of silica, including α-cristobalite, α-quartz, coesite, stishovite, and fused quartz, which are natural, synthetic or commercial samples. We compare the results to previous studies and find that α-cristobalite synthesized at higher temperature than annealed silica. The interesting result of features similar to those of forsterite should be highlighted, where αcristobalite and coesite showed similar peaks at 16, 33, and 69 μm as forsterite. The 69 μm band for αcristobalite is especially very broad and strong, and shifts largely to a shorter wavelengths under cooling to low temperatures. The band for coesite, however, is very sharp, and shifts only a small amount to longer wavelengths under cooling to low temperatures. The peak positions of 16 and 69-μm band due to α-cristobalite can become index for temperature of silica dust. We discuss the possibility of silica detection around debris disks.

  13. Formation of titanium carbide coating with micro-porous structure

    NASA Astrophysics Data System (ADS)

    Luo, Yong; Ge, Shirong; Jin, Zhongmin; Fisher, John

    2010-03-01

    Micro-porous titanium carbide coating was successfully synthesized in a vacuum gas carburizing furnace by using a sequential diffusion technology. The composition and structure of the as-synthesized TiC were examined by X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and glow discharge mass spectrometry (GDMS), and scanning electron microscopy (SEM). All of the XRD, XPS and GDMS analysis results indicate that carbon atoms effectively diffused into the titanium alloys and formed a uniform acicular TiC coating with micro-porous structure.

  14. A large deformation poroplasticity theory for microporous polymeric materials

    NASA Astrophysics Data System (ADS)

    Anand, Lallit

    2017-01-01

    A coupled theory accounting for fluid diffusion and large deformations of elastic-viscoplastic microporous polymeric materials is presented. The theory is intended to represent the coupled deformation-diffusion response of a material which at a microscopic scale consists of a porous polymeric skeleton and a freely moving fluid in a fully connected pore space. Potential applications of the theory include modeling the response of polymer microfiltration membranes, as well as modeling the response of several hydrated biological tissues which are microporous polymeric materials containing a high concentration of liquids.

  15. Distribution and Speciation of Nutrient Elements around Micropores

    SciTech Connect

    Jassogne, Laurence; Hettiarachchi, Ganga; Chittleborough, David; McNeill, Ann

    2009-07-21

    In Australia a class of soils known as duplex soils covers approximately 20% of the continent. Their defining characteristic is a sharp texture contrast between the A (or E) and B horizon. The upper B horizon at the point of contact with the E horizon is often highly sodic and of such a high strength that root growth and proliferation, water conductivity, aeration, water storage, and water uptake are restricted. Roots growing in these soils rely on channels created by previous roots or cracks arising from shrink-swell forces associated with seasonal wetting and drying. Although the characteristics of rhizospheres compared with the soil matrix are well documented there is a paucity of knowledge about how long these changes persist after roots decay. This knowledge is fundamental to our understanding of root growth in duplex soils in which plants rely on pore networks formed by previous plants to proliferate in the subsoil. In this study we investigated the heterogeneous chemistry of micropores in situ using synchrotron-based {mu}-x-ray fluorescence spectroscopy (XRF), {mu}-x-ray absorption near edge structure spectroscopy (XANES), and extended {mu}-x-ray absorption fine structure spectroscopy (EXAFS). The distribution maps of Ca, Mn, Fe, Cu, and Zn at micrometer resolution were collected using {mu}-XRF. Subsequently, specific locations with higher concentrations (hot spots) of Mn, Fe, Cu, or Zn were selected and XANES and EXAFS spectra were collected to study the speciation of these elements around the micropore compared with the soil matrix. The {mu}-XRF maps showed that Mn was depleted around one of the micropores studied but accumulated around another micropore. Copper and Zn accumulated around the micropores, whereas Ca was predominantly inside micropores. There was no difference between matrix and micropore surface with respect to the distribution of Fe. Around micropores Mn was present in reduced form (Mn II) and Fe was in its oxidized form (Fe III). Manganese

  16. Preparation of a novel ionic hybrid stationary phase by non-covalent functionalization of single-walled carbon nanotubes with amino-derivatized silica gel for fast HPLC separation of aromatic compounds.

    PubMed

    Aral, Hayriye; Çelik, K Serdar; Aral, Tarık; Topal, Giray

    2016-03-01

    Single-walled carbon nanotubes (SWCNTs) were immobilized on spherical silica gel with a 4-μm average particle size and a 60-Å average pore size. The amino-derivatized silica gel was non-covalently coated with carboxylated SWCNTs to preserve the structure of the nanotubes and their physico-chemical properties. The novel ionic hybrid stationary phase was characterized by scanning electron microscopy (SEM), infra-red (IR) spectroscopy and elemental analysis, and then, it was used to fill an empty 150×4.6mm(2) high-performance liquid chromatography (HPLC) column. Chromatographic parameters, such as the theoretical plate number, retention factor and peak asymmetry factor, and analytical parameters, such as the limit of detection (LOD), limit of quantification (LOQ), linear range, calibration equation, and R(2) value, and quantitative analysis parameters were calculated for all of the analytes. Using different mobile phases, five different classes of aromatic hydrocarbons were separated in a very short analysis time of 4-8min. Furthermore, a high theoretical plate number (up to 25000) and an excellent peak asymmetry factor (1.0) were obtained. The results showed that the surface of the SWNTs had very strong interactions with aromatic groups, therefore providing high selectivity for the separation of different classes of aromatic compounds. This study indicates that SWCNTs enable the extension of the application range of the newly prepared stationary phases for the fast separation of aromatic compounds by HPLC.

  17. Facile preparation of raisin-bread sandwich-structured magnetic graphene/mesoporous silica composites with C18-modified pore-walls for efficient enrichment of phthalates in environmental water.

    PubMed

    Huang, Danni; Wang, Xianying; Deng, Chunhui; Song, Guoxin; Cheng, Hefa; Zhang, Xiangmin

    2014-01-17

    In this study, novel raisin-bread sandwich-structured magnetic graphene/mesoporous silica composites with C18-modified interior pore-walls (mag-graphene@mSiO2-C18) were synthesized by coating mesoporous silica layers onto each side of magnetic graphene through a surfactant-mediated co-condensation sol-gel process. The prepared functionalized nanocomposites possessed marvelous properties of extended plate-like morphology, fine water dispersibility, high magnetic response, large surface area (315.4cm(2)g(-1)), uniform pore size (3.3nm) and C18-modified interior pore-walls. Several kinds of phthalates were selected as model analytes to systematically evaluate the performance of adsorbents in extracting hydrophobic molecules followed by gas chromatography-mass spectrometry analyses. Various extraction parameters, including pH value of sample solution, amounts of adsorbents, adsorption time, species and volume of eluting solvent, and desorption time were optimized. The anti-interference ability to macromolecular proteins was also investigated. Method validations such as linearity, recovery, reproducibility, and limit of detection were also studied. Finally, mag-graphene@mSiO2-C18 composites were successfully applied to analyzing phthalates in environmental water samples. The results indicated that this novel approach offered an attractive alternative for rapid, convenient, efficient and selective magnetic solid-phase extraction for targeted hydrophobic compounds.

  18. Sample Desorption/Onization From Mesoporous Silica

    DOEpatents

    Iyer, Srinivas; Dattelbaum, Andrew M.

    2005-10-25

    Mesoporous silica is shown to be a sample holder for laser desorption/ionization of mass spectrometry. Supported mesoporous silica was prepared by coating an ethanolic silicate solution having a removable surfactant onto a substrate to produce a self-assembled, ordered, nanocomposite silica thin film. The surfactant was chosen to provide a desired pore size between about 1 nanometer diameter and 50 nanometers diameter. Removal of the surfactant resulted in a mesoporous silica thin film on the substrate. Samples having a molecular weight below 1000, such as C.sub.60 and tryptophan, were adsorbed onto and into the mesoporous silica thin film sample holder and analyzed using laser desorption/ionization mass spectrometry.

  19. Facile large-scale preparation of mesoporous silica microspheres with the assistance of sucrose and their drug loading and releasing properties.

    PubMed

    Bi, Yanping; Wu, Chaonan; Xin, Ming; Bi, Shuyan; Yan, Chengxin; Hao, Jifu; Li, Fei; Li, Shou

    2016-03-16

    Mesoporous silica microspheres (MSMs) with a pore-size larger than 10nm and a large pore-volume have attracted considerable attention for their application in delivering poorly water-soluble drugs. Here we developed a simple method for large-scale synthesis of MSMs using sodium silicate as silica precursor. The novelty of this approach lies in the use of sucrose solution to achieve large size and volume of nanopores. The highest values of pore size and pore volume are 13.2 nm and 1.97 cm(3)/g, respectively. Importantly, the method is reliable and easily upscalable. The blank and drug-loaded MSMs were characterized by differential scanning calorimetry (DSC) and X-ray powder diffraction (XRPD). Ibuprofen and resveratrol were successfully loaded into the nanopores of MSMs in amorphous and nanocrystalline form and showed high drug-loadings and enhanced dissolution rates. This kind of MSMs appears to be a promising candidate as a new oral drug delivery vehicle providing a rapid drug release.

  20. Incorporating Nano-silica as a Binder to Improve Corrosion Resistance of High Alumina Refractory Castables

    NASA Astrophysics Data System (ADS)

    Ramezani, Abbas; Mohebi, Mohammad Masoud; Souri, Alireza

    2013-04-01

    In this study, four types of castables as calcium-aluminate cement (CAC)-bonded and nano-silica (NS)-bonded castables based on tabular-alumina and bauxite aggregates were prepared to investigate the replacement of the calcium-aluminate cement by NS. All samples were allowed to dry at 110 °C then fired at 800 and 1200 °C. Bulk density and apparent porosity of samples were measured. The molten aluminum static corrosion test (cup test) results showed that NS-bonded specimens had higher resistance to corrosion compared to CAC-bonded samples (based on the measured average aluminum penetration depth into the refractory texture). However no penetration was observed in bauxite NS-bonded samples. The results were consistent with dynamic corrosion test in aluminum melt carried out at 800 °C for 100 h. The small pore size in NS-bonded castables was found to be the main cause for high corrosion resistance as micro-pores prevented the melt to penetrate into the refractory.

  1. Catalyst free silica templated porous carbon nanoparticles from bio-waste materials.

    PubMed

    Kumar, Anuj; Hegde, Gurumurthy; Manaf, Shoriya Aruni Bt Abdul; Ngaini, Z; Sharma, K V

    2014-10-28

    Porous Carbon Nanoparticles (PCNs) with well-developed microporosity were obtained from bio-waste oil palm leaves (OPL) using single step pyrolysis in nitrogen atmosphere at 500-600 °C in tube-furnace without any catalysis support. The key approach was using silica (SiO2) bodies of OPL as a template in the synthesis of microporous carbon nanoparticles with very small particle sizes of 35-85 nm and pore sizes between 1.9-2 nm.

  2. Fundamental Studies of Crystal Growth of Microporous Materials

    NASA Technical Reports Server (NTRS)

    Singh, Ramsharan; Doolittle, John, Jr.; Payra, Pramatha; Dutta, Prabir K.; George, Michael A.; Ramachandran, Narayanan; Schoeman, Brian J.

    2003-01-01

    Microporous materials are framework structures with well-defined porosity, often of molecular dimensions. Zeolites contain aluminum and silicon atoms in their framework and are the most extensively studied amongst all microporous materials. Framework structures with P, Ga, Fe, Co, Zn, B, Ti and a host of other elements have also been made. Typical synthesis of microporous materials involve mixing the framework elements (or compounds, thereof) in a basic solution, followed by aging in some cases and then heating at elevated temperatures. This process is termed hydrothermal synthesis, and involves complex chemical and physical changes. Because of a limited understanding of this process, most synthesis advancements happen by a trial and error approach. There is considerable interest in understanding the synthesis process at a molecular level with the expectation that eventually new framework structures will be built by design. The basic issues in the microporous materials crystallization process include: (a) Nature of the molecular units responsible for the crystal nuclei formation; (b) Nature of the nuclei and nucleation process; (c) Growth process of the nuclei into crystal; (d) Morphological control and size of the resulting crystal; (e) Surface structure of the resulting crystals; and (f) Transformation of frameworks into other frameworks or condensed structures.

  3. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... accordance with good manufacturing practice so as to prevent potential microbial adulteration of the food. (g... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Filters, microporous polymeric. 177.2250 Section 177.2250 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN...

  4. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... accordance with good manufacturing practice so as to prevent potential microbial adulteration of the food. (g... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Filters, microporous polymeric. 177.2250 Section 177.2250 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN...

  5. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... accordance with good manufacturing practice so as to prevent potential microbial adulteration of the food. (g... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Filters, microporous polymeric. 177.2250 Section 177.2250 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN...

  6. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... accordance with good manufacturing practice so as to prevent potential microbial adulteration of the food. (g... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Filters, microporous polymeric. 177.2250 Section 177.2250 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN...

  7. Rendering non-energetic microporous coordination polymers explosive.

    PubMed

    McDonald, Kyle A; Bennion, Jonathan C; Leone, Amanda K; Matzger, Adam J

    2016-09-18

    Adsorption of oxidizing guest molecules into a non-energetic microporous coordination polymer produces explosives with desirable oxygen balance, high heat released upon decomposition, and suppressed vapor pressure of the guest. Here, this results in primary explosives, materials very sensitive to impact, that have the potential to be used as replacements for lead-based initiators.

  8. Preparation and application of methylcalix[4]resorcinarene-bonded silica particles as chiral stationary phase in high-performance liquid chromatography.

    PubMed

    Tan, Huey Min; Soh, Shu Fang; Zhao, Jia; Yong, E L; Gong, Yinhan

    2011-01-01

    Two new types of methylcalix[4]resorcinarene-bonded stationary phases, (3-(C-methylcalix[4]resorcinarene)-2-hydroxypropoxy)-propylsilyl-appended silica particles (MCR-HPS) and bromoacetate-substituted MCR-HPS particles (BAMCR-HPS), have been synthesized and used as chiral stationary phases for high-performance liquid chromatography (HPLC) for the first time. The synthetic stationary phases are characterized by means of elemental analysis and Fourier-transform infrared spectroscopy. The chromatographic behavior of MCR-HPS and BAMCR-HPS was studied with several disubstituted benzenes and some chiral drug compounds under both normal phase and reversed-phase conditions. The results show that MCR-HPS has excellent selectivity for the separation of aromatic positional isomers and BAMCR-HPS exhibits excellent performance for separation of enantiomers of chiral compounds.

  9. Preparation and evaluation of open tubular C18-silica monolithic microcartridges for preconcentration of peptides by on-line solid phase extraction capillary electrophoresis.

    PubMed

    Ortiz-Villanueva, Elena; Benavente, Fernando; Giménez, Estela; Yilmaz, Fatma; Sanz-Nebot, Victoria

    2014-10-10

    In this study, C18-silica monoliths were synthesized as a porous layer in open tubular capillary columns, to be cut later into microcartridges for the analysis of neuropeptides by on-line solid-phase extraction capillary electrophoresis with UV and MS detection (SPE-CE-UV and SPE-CE-MS). First, several types of C18-silica monolithic (MtC18) microcartridges were used to analyse standard solutions of five neuropeptides (i.e. dynorphin A (1-7), substance P (7-11), endomorphin 1, methionine enkephalin and [Ala]-methionine enkephalin). The MtC18 sorbents were especially selective against endomorphin 1 and substance P (7-11)). The best results in terms of sensitivity and inter-microcartridge reproducibility were achieved with the microcartridges obtained from a 10-cm open tubular capillary column with a thin monolithic coating with large through-pores (1-5μm). Run-to-run repeatability, microcartridge durability, linearity ranges and LODs were studied by MtC18-SPE-CE-MS. As expected due to their greater selectivity, the best LOD enhancement was obtained for End1 and SP (7-11) (50 times with regard to CE-MS). Finally, the suitability of the methodology for analysing biological fluids was tested with plasma samples spiked with End1 and SP (7-11). Results obtained were promising because both neuropeptides could be detected at 0.05μgmL(-1), which was almost the same concentration level as for the standard solutions (0.01μgmL(-1)).

  10. Suppressed N2O formation during NH3 selective catalytic reduction using vanadium on zeolitic microporous TiO2.

    PubMed

    Lee, Seung Gwan; Lee, Hyun Jeong; Song, Inhak; Youn, Seunghee; Kim, Do Heui; Cho, Sung June

    2015-08-03

    Emission of N2O from mobile and off-road engine is now being currently regulated because of its high impact compared to that of CO2, thereby implying that N2O formation from the exhaust gas after-treatment system should be suppressed. Selective catalytic reduction using vanadium supported TiO2 catalyst in mobile and off-road engine has been considered to be major source for N2O emission in the system. Here we have demonstrated that vanadium catalyst supported on zeolitic microporous TiO2 obtained from the hydrothermal reaction of bulk TiO2 at 400 K in the presence of LiOH suppresses significantly the N2O emission compared to conventional VOx/TiO2 catalyst, while maintaining the excellent NOx reduction, which was ascribed to the location of VOx domain in the micropore of TiO2, resulting in the strong metal support interaction. The use of zeolitic microporous TiO2 provides a new way of preparing SCR catalyst with a high thermal stability and superior catalytic performance. It can be also extended further to the other catalytic system employing TiO2-based substrate.

  11. Suppressed N2O formation during NH3 selective catalytic reduction using vanadium on zeolitic microporous TiO2

    PubMed Central

    Lee, Seung Gwan; Lee, Hyun Jeong; Song, Inhak; Youn, Seunghee; Kim, Do Heui; Cho, Sung June

    2015-01-01

    Emission of N2O from mobile and off-road engine is now being currently regulated because of its high impact compared to that of CO2, thereby implying that N2O formation from the exhaust gas after-treatment system should be suppressed. Selective catalytic reduction using vanadium supported TiO2 catalyst in mobile and off-road engine has been considered to be major source for N2O emission in the system. Here we have demonstrated that vanadium catalyst supported on zeolitic microporous TiO2 obtained from the hydrothermal reaction of bulk TiO2 at 400 K in the presence of LiOH suppresses significantly the N2O emission compared to conventional VOx/TiO2 catalyst, while maintaining the excellent NOx reduction, which was ascribed to the location of VOx domain in the micropore of TiO2, resulting in the strong metal support interaction. The use of zeolitic microporous TiO2 provides a new way of preparing SCR catalyst with a high thermal stability and superior catalytic performance. It can be also extended further to the other catalytic system employing TiO2-based substrate. PMID:26235671

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

  13. Preparation and characterization of polydimethylsiloxane/poly(vinylalcohol) coated solid phase microextraction fibers using sol-gel technology.

    PubMed

    Lopes, Alexandre Leite; Augusto, Fabio

    2004-11-12

    The applicability of a composite composed of polydimethylsiloxane (PDMS) and poly(vinyl alcohol) (PDMS/PVA) as coating sorbent for SPME fibers is demonstrated here. Fused silica (FS) fibers were coated with PDMS/PVA composite through a sol-gel process, using methyltrimethoxysilane as reticulating agent. The chemical and physical properties of the sol-gel PDMS/PVA composite were determined by infrared spectroscopy and thermogravimetric analysis. Electron scanning microscopy of the prepared fibers, showed that the coating obtained was highly microporous, having a thickness of approximately 5 microm. The fibers were tested for the headspace extraction of several organic compounds (o-xylene, naphthalene, ethyl caprate, p-chlorotoluene and PCB) prior to gas chromatographic analysis. The extractive capacity of the PDMS/PVA coating was found to be superior to that of pure conventional PDMS fibers.

  14. Aminated hollow silica spheres for electrochemical DNA biosensor

    NASA Astrophysics Data System (ADS)

    Ariffin, Eda Yuhana; Heng, Lee Yook; Futra, Dedi; Ling, Tan Ling

    2015-09-01

    An electrochemical DNA biosensor for e.coli determination based on aminated hollow silica was successfully developed. Aminated hollow silica spheres were prepared through the reaction of Tween 20 template and silica precursor. The template was removed by the thermal decomposition at 620°C. Hollow silica spheres were modified with (3-Aminopropyl) triethoxysilane (APTS) to form aminated hollow silica spheres.Aminated DNA probe were covalently immobilized on to the amine functionalized hollow silica spheres through glutaradehyde linkers. The formation hollow silica was characterized using FTIR and FESEM. A range of 50-300nm particle size obtained from FESEM micrograph. Meanwhile for the electrochemical study, a quasi-reversible system has been obtain via cyclic voltammetry (CV).

  15. Multifunctional mesoporous silica catalyst

    DOEpatents

    Lin, Victor Shang-Yi; Tsai, Chih-Hsiang; Chen, Hung-Ting; Pruski, Marek; Kobayashi, Takeshi

    2015-03-31

    The present invention provides bifunctional silica mesoporous materials, including mesoporous silica nanoparticles ("MSN"), having pores modified with diarylammonium triflate and perfluoroaryl moieties, that are useful for the acid-catalyzed esterification of organic acids with organic alcohols.

  16. Silica extraction from geothermal water

    DOEpatents

    Bourcier, William L; Bruton, Carol J

    2014-09-23

    A method of producing silica from geothermal fluid containing low concentration of the silica of less than 275 ppm includes the steps of treating the geothermal fluid containing the silica by reverse osmosis treatment thereby producing a concentrated fluid containing the silica, seasoning the concentrated fluid thereby producing a slurry having precipitated colloids containing the silica, and separating the silica from the slurry.

  17. In situ ultra-small-angle X-ray scattering study under uniaxial stretching of colloidal crystals prepared by silica nanoparticles bearing hydrogen-bonding polymer grafts

    PubMed Central

    Ishige, Ryohei; Williams, Gregory A.; Higaki, Yuji; Ohta, Noboru; Sato, Masugu; Takahara, Atsushi; Guan, Zhibin

    2016-01-01

    A molded film of single-component polymer-grafted nanoparticles (SPNP), consisting of a spherical silica core and densely grafted polymer chains bearing hydrogen-bonding side groups capable of physical crosslinking, was investigated by in situ ultra-small-angle X-ray scattering (USAXS) measurement during a uniaxial stretching process. Static USAXS revealed that the molded SPNP formed a highly oriented twinned face-centered cubic (f.c.c.) lattice structure with the [11−1] plane aligned nearly parallel to the film surface in the initial state. Structural analysis of in situ USAXS using a model of uniaxial deformation induced by rearrangement of the nanoparticles revealed that the f.c.c. lattice was distorted in the stretching direction in proportion to the macroscopic strain until the strain reached 35%, and subsequently changed into other f.c.c. lattices with different orientations. The lattice distortion and structural transition behavior corresponded well to the elastic and plastic deformation regimes, respectively, observed in the stress–strain curve. The attractive interaction of the hydrogen bond is considered to form only at the top surface of the shell and then plays an effective role in cross-linking between nanoparticles. The rearrangement mechanism of the nanoparticles is well accounted for by a strong repulsive interaction between the densely grafted polymer shells of neighboring particles. PMID:27158507

  18. In situ ultra-small-angle X-ray scattering study under uniaxial stretching of colloidal crystals prepared by silica nanoparticles bearing hydrogen-bonding polymer grafts

    DOE PAGES

    Ishige, Ryohei; Williams, Gregory A.; Higaki, Yuji; ...

    2016-04-19

    A molded film of single-component polymer-grafted nanoparticles (SPNP), consisting of a spherical silica core and densely grafted polymer chains bearing hydrogen-bonding side groups capable of physical crosslinking, was investigated byin situultra-small-angle X-ray scattering (USAXS) measurement during a uniaxial stretching process. Static USAXS revealed that the molded SPNP formed a highly oriented twinned face-centered cubic (f.c.c.) lattice structure with the [11-1] plane aligned nearly parallel to the film surface in the initial state. Structural analysis ofin situUSAXS using a model of uniaxial deformation induced by rearrangement of the nanoparticles revealed that the f.c.c. lattice was distorted in the stretching direction inmore » proportion to the macroscopic strain until the strain reached 35%, and subsequently changed into other f.c.c. lattices with different orientations. The lattice distortion and structural transition behavior corresponded well to the elastic and plastic deformation regimes, respectively, observed in the stress–strain curve. The attractive interaction of the hydrogen bond is considered to form only at the top surface of the shell and then plays an effective role in cross-linking between nanoparticles. The rearrangement mechanism of the nanoparticles is well accounted for by a strong repulsive interaction between the densely grafted polymer shells of neighboring particles.« less

  19. Resolution and isolation of enantiomers of (±)-isoxsuprine using thin silica gel layers impregnated with L-glutamic acid, comparison of separation of its diastereomers prepared with chiral derivatizing reagents having L-amino acids as chiral auxiliaries.

    PubMed

    Bhushan, Ravi; Nagar, Hariom

    2015-03-01

    Thin silica gel layers impregnated with optically pure l-glutamic acid were used for direct resolution of enantiomers of (±)-isoxsuprine in their native form. Three chiral derivatizing reagents, based on DFDNB moiety, were synthesized having l-alanine, l-valine and S-benzyl-l-cysteine as chiral auxiliaries. These were used to prepare diastereomers under microwave irradiation and conventional heating. The diastereomers were separated by reversed-phase high-performance liquid chromatography on a C18 column with detection at 340 nm using gradient elution with mobile phase containing aqueous trifluoroacetic acid and acetonitrile in different compositions and by thin-layer chromatography (TLC) on reversed phase (RP) C18 plates. Diastereomers prepared with enantiomerically pure (+)-isoxsuprine were used as standards for the determination of the elution order of diastereomers of (±)-isoxsuprine. The elution order in the experimental study of RP-TLC and RP-HPLC supported the developed optimized structures of diastereomers based on density functional theory. The limit of detection was 0.1-0.09 µg/mL in TLC while it was in the range of 22-23 pg/mL in HPLC and 11-13 ng/mL in RP-TLC for each enantiomer. The conditions of derivatization and chromatographic separation were optimized. The method was validated for accuracy, precision, limit of detection and limit of quantification.

  20. Preparation of magnetic graphene/mesoporous silica composites with phenyl-functionalized pore-walls as the restricted access matrix solid phase extraction adsorbent for the rapid extraction of parabens from water-based skin toners.

    PubMed

    Feng, Jianan; He, Xinying; Liu, Xiaodan; Sun, Xueni; Li, Yan

    2016-09-23

    In this work, phenyl-functionalized magnetic graphene/mesoporous silica composites (MG-mSiO2-Ph) were prepared and applied as restricted access matrix solid phase extraction (RAM-SPE) adsorbents to determine the parabens in commercially available retail cosmetics. MG-mSiO2-Ph composites were synthesized by a surfactant-mediated co-condensation reaction in which mesoporous silica with phenyl-functionalized pore-walls was coated on a magnetic graphene sheet. The obtained nano-composites were proven to be of sufficient quality for an ideal RAM-SPE adsorbent with a large specific surface area of 369m(2)g(-1), uniform mesopores of 2.8nm, and special phenyl-functionalized pore-walls. Parabens, such as methyl paraben, ethyl paraben and propyl paraben, were extracted from water-based skin toners using one step of the RAM-SPE and were then analysed by a HPLC-DAD system. The SPE conditions were optimized by studying the parameters, such as the adsorbent amount, elution solvent type, adsorption time and desorption time, that influence the extraction efficiency. For each analyte, there were good linearities of approximately 0.10-120μgmL(-1) with determination coefficients (R(2))>0.995. The sensitivity was as low as 0.01-0.025μgmL(-1) for the LOD, and the percent recoveries were 98.37-105.84%. The intra-day and inter-day RSDs were 1.44-6.11% (n=6) and 3.12-11.70% (n=6), respectively. The results indicated that this method with novel RAM-SPE adsorbents is sensitive and convenient. The results also offered an attractive alternative for the extraction and determination of paraben preservatives in a complex matrix, such as cosmetics.

  1. Microporous layer based on SiC for high temperature proton exchange membrane fuel cells

    NASA Astrophysics Data System (ADS)

    Lobato, Justo; Zamora, Héctor; Cañizares, Pablo; Plaza, Jorge; Rodrigo, Manuel Andrés

    2015-08-01

    This work reports the evaluation of Silicon Carbide (SiC) for its application in microporous layers (MPL) of HT-PEMFC electrodes and compares results with those obtained using conventional MPL based on Vulcan XC72. Influence of the support load on the MPL prepared with SiC was evaluated, and the MPL were characterized by XRD, Hg porosimetry and cyclic voltammetries. In addition, a short lifetest was carried out to evaluate performance in accelerated stress conditions. Results demonstrate that SiC is a promising alternative to carbonaceous materials because of its higher electrochemical and thermal stability and the positive effect on mass transfer associated to its different pore size distribution. Ohmic resistance is the most significant challenge to be overcome in further studies.

  2. Hydrolysis of microporous polyamide-6 membranes as substrate for in situ synthesis of oligonucleotides

    NASA Astrophysics Data System (ADS)

    Tang, Jianxin; He, Nongyue; Nie, Libo; Xiao, Pengfeng; Chen, Hong

    2004-02-01

    This article provides a novel method of preparing substrate for in situ synthesis of oligonucleotide by hydrolyzing microporous polyamide-6 membranes in a 0.01 mol/l/NaOH/(H 2O-CH 3OH) mixture medium with refluxing about 36 h. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) demonstrated the emergence of amines (NH 2) on the surface. Optimum hydrolyzing conditions were determined through the ultra-violet (UV) spectra. A pH value of 12 and a hydrolysis time of 36 h are the preferred conditions for the modification. The treated membrane can be applied to in situ synthesis of oligonucleotide and, for example, the oligonucleotide probes of 5 '-AAC CAC CAA ACA CAC-3 ' were successfully synthesized on the hydrolyzed membrane. The single step coupling efficiency determined by ultraviolet (UV) spectra is above 98%.

  3. Microporous polycarbazole with high specific surface area for gas storage and separation.

    PubMed

    Chen, Qi; Luo, Min; Hammershøj, Peter; Zhou, Ding; Han, Ying; Laursen, Bo Wegge; Yan, Chao-Guo; Han, Bao-Hang

    2012-04-11

    Microporous polycarbazole via straightforward carbazole-based oxidative coupling polymerization is reported. The synthesis route exhibits cost-effective advantages, which are essential for scale-up preparation. The Brunauer-Emmett-Teller specific surface area for obtained polymer is up to 2220 m(2) g(-1). Gas (H(2) and CO(2)) adsorption isotherms show that its hydrogen storage can reach to 2.80 wt % (1.0 bar and 77 K) and the uptake capacity for carbon dioxide is up to 21.2 wt % (1.0 bar and 273 K), which show a promising potential for clean energy application and environmental field. Furthermore, the high selectivity toward CO(2) over N(2) and CH(4) makes the obtained polymer possess potential application in gas separation.

  4. Highly microporous-graphene aerogel monolith of unidirectional honeycomb macro-textures

    NASA Astrophysics Data System (ADS)

    Wang, Shuwen; Wang, Zhipeng; Futamura, Ryusuke; Endo, Morinobu; Kaneko, Katsumi

    2017-04-01

    The highly microporous graphene aerogel monolith of unidirectional textures is obtained from reduction and KOH activation of colloidal graphene oxide prepared with an ice-templating route. The free-standing geometry and well-aligned textures of graphene monolith are persevered even after an intensive KOH activation at 973 K, although the frame structure is slightly disordered. The non-overestimated surface area of the KOH activated graphene monolith is 990 m2 g-1. The free-standing graphene aerogel monolith has predominant microporosity with appropriate macroporosity and a low bulk density of 8 ± 0.5 mg cm-3, being one of the lightest materials of the reported porous graphene materials.

  5. Immobilization of silver nanoparticles on silica microspheres

    NASA Astrophysics Data System (ADS)

    Huang, Chih-Kai; Chen, Chia-Yin; Han, Jin-Lin; Chen, Chii-Chang; Jiang, Meng-Dan; Hsu, Jen-Sung; Chan, Chia-Hua; Hsieh, Kuo-Huang

    2010-01-01

    The silver nanoparticles (Ag NPs) have been immobilized onto silica microspheres through the adsorption and subsequent reduction of Ag+ ions on the surfaces of the silica microspheres. The neat silica microspheres that acted as the core materials were prepared through sol-gel processing; their surfaces were then functionalized using 3-mercaptopropyltrimethoxysilane (MPTMS). The major aims of this study were to immobilize differently sized Ag particles onto the silica microspheres and to understand the mechanism of formation of the Ag nano-coatings through the self-assembly/adsorption behavior of Ag NPs/Ag+ ions on the silica spheres. The obtained Ag NP/silica microsphere conglomerates were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and energy-dispersive spectroscopy (EDS). Their electromagnetic wave shielding effectiveness were also tested and studied. The average particle size of the obtained Ag NPs on the silica microsphere was found that could be controllable (from 2.9 to 51.5 nm) by adjusting the ratio of MPTMS/TEOS and the amount of AgNO3.

  6. Cell instructive microporous scaffolds through interface engineering.

    PubMed

    Viswanathan, Priyalakshmi; Chirasatitsin, Somyot; Ngamkham, Kamolchanok; Engler, Adam J; Battaglia, Giuseppe

    2012-12-12

    The design of novel biomaterials for regenerative medicine requires incorporation of well-defined physical and chemical properties that mimic the native extracellular matrix (ECM). Here, we report the synthesis and characterization of porous foams prepared by high internal phase emulsion (HIPE) templating using amphiphilic copolymers that act as surfactants during the HIPE process. We combine different copolymers exploiting oil-water interface confined phase separation to engineer the surface topology of foam pores with nanoscopic domains of cell inert and active chemistries mimicking native matrix. We further demonstrate how proteins and hMSCs adhere in a domain specific manner.

  7. Profiling preparations of recombinant birch pollen allergen Bet v 1a with capillary zone electrophoresis in pentamine modified fused-silica capillaries.

    PubMed

    Punzet, M; Ferreira, F; Briza, P; van Ree, R; Malissa, H; Stutz, H

    2006-07-24

    Three preparation batches of the recombinant birch pollen allergen Bet v 1a have been analyzed by capillary zone electrophoresis (CZE) using a separation electrolyte consisting of 100 mmol L(-1) phosphate at pH 6.50 with 2.0 mmol L(-1) tetraethylenepentamine (TEPA) added. TEPA improved the resolution by wall shielding and selective attachment to allergens, but reduced migration repeatability at concentrations >2.0 mmol L(-1). Heterogeneity of preparations determined by CZE and electrospray ionization-quadrupole-time-of flight-MS were in accordance and revealed chemically modified (carbamylated) allergens in one of the preparations. The method was validated according to the ICH-guidelines. Repeatability of effective electrophoretic mobility (mu(eff)) was <0.55% R.S.D. (n = 5). Migration time corrected peak areas were used for quantification. Limit of quantification (LOQ) was 25 microg mL(-1) for the major isoform Bet v 1a, based on a signal-to-noise ratio of 10, and detector response was linear between LOQ and 0.90 mg mL(-1). Purity of the different rBet v 1a preparations was determined to be between 40 and 92% depending on the manufacturing protocol.

  8. One-Step Synthesis of Microporous Carbon Monoliths Derived from Biomass with High Nitrogen Doping Content for Highly Selective CO2 Capture

    PubMed Central

    Geng, Zhen; Xiao, Qiangfeng; Lv, Hong; Li, Bing; Wu, Haobin; Lu, Yunfeng; Zhang, Cunman

    2016-01-01

    The one-step synthesis method of nitrogen doped microporous carbon monoliths derived from biomass with high-efficiency is developed using a novel ammonia (NH3)-assisted activation process, where NH3 serves as both activating agent and nitrogen source. Both pore forming and nitrogen doping simultaneously proceed during the process, obviously superior to conventional chemical activation. The as-prepared nitrogen-doped active carbons exhibit rich micropores with high surface area and high nitrogen content. Synergetic effects of its high surface area, microporous structure and high nitrogen content, especially rich nitrogen-containing groups for effective CO2 capture (i.e., phenyl amine and pyridine-nitrogen) lead to superior CO2/N2 selectivity up to 82, which is the highest among known nanoporous carbons. In addition, the resulting nitrogen-doped active carbons can be easily regenerated under mild conditions. Considering the outstanding CO2 capture performance, low production cost, simple synthesis procedure and easy scalability, the resulting nitrogen-doped microporous carbon monoliths are promising candidates for selective capture of CO2 in industrial applications. PMID:27488268

  9. One-Step Synthesis of Microporous Carbon Monoliths Derived from Biomass with High Nitrogen Doping Content for Highly Selective CO2 Capture.

    PubMed

    Geng, Zhen; Xiao, Qiangfeng; Lv, Hong; Li, Bing; Wu, Haobin; Lu, Yunfeng; Zhang, Cunman

    2016-08-04

    The one-step synthesis method of nitrogen doped microporous carbon monoliths derived from biomass with high-efficiency is developed using a novel ammonia (NH3)-assisted activation process, where NH3 serves as both activating agent and nitrogen source. Both pore forming and nitrogen doping simultaneously proceed during the process, obviously superior to conventional chemical activation. The as-prepared nitrogen-doped active carbons exhibit rich micropores with high surface area and high nitrogen content. Synergetic effects of its high surface area, microporous structure and high nitrogen content, especially rich nitrogen-containing groups for effective CO2 capture (i.e., phenyl amine and pyridine-nitrogen) lead to superior CO2/N2 selectivity up to 82, which is the highest among known nanoporous carbons. In addition, the resulting nitrogen-doped active carbons can be easily regenerated under mild conditions. Considering the outstanding CO2 capture performance, low production cost, simple synthesis procedure and easy scalability, the resulting nitrogen-doped microporous carbon monoliths are promising candidates for selective capture of CO2 in industrial applications.

  10. One-Step Synthesis of Microporous Carbon Monoliths Derived from Biomass with High Nitrogen Doping Content for Highly Selective CO2 Capture

    NASA Astrophysics Data System (ADS)

    Geng, Zhen; Xiao, Qiangfeng; Lv, Hong; Li, Bing; Wu, Haobin; Lu, Yunfeng; Zhang, Cunman

    2016-08-01

    The one-step synthesis method of nitrogen doped microporous carbon monoliths derived from biomass with high-efficiency is developed using a novel ammonia (NH3)-assisted activation process, where NH3 serves as both activating agent and nitrogen source. Both pore forming and nitrogen doping simultaneously proceed during the process, obviously superior to conventional chemical activation. The as-prepared nitrogen-doped active carbons exhibit rich micropores with high surface area and high nitrogen content. Synergetic effects of its high surface area, microporous structure and high nitrogen content, especially rich nitrogen-containing groups for effective CO2 capture (i.e., phenyl amine and pyridine-nitrogen) lead to superior CO2/N2 selectivity up to 82, which is the highest among known nanoporous carbons. In addition, the resulting nitrogen-doped active carbons can be easily regenerated under mild conditions. Considering the outstanding CO2 capture performance, low production cost, simple synthesis procedure and easy scalability, the resulting nitrogen-doped microporous carbon monoliths are promising candidates for selective capture of CO2 in industrial applications.

  11. Macroscopic Simulation of Deformation in Soft Microporous Composites.

    PubMed

    Evans, Jack D; Coudert, François-Xavier

    2017-03-23

    Soft microporous materials exhibit properties, such as gated adsorption and breathing, which are highly desirable for many applications. These properties are largely studied for single crystals; however, many potential applications expect to construct structured or composite systems, examples of which include monoliths and mixed-matrix membranes. Herein, we use finite element methods to predict the macroscopic mechanical response of composite microporous materials. This implementation connects the microscopic treatment of crystalline structures to the response of a macroscopic sample. Our simulations reveal the bulk modulus of an embedded adsorbent within a composite is affected by the thickness and properties of the encapsulating layer. Subsequently, we employ this methodology to examine mixed-matrix membranes and materials of negative linear compressibility. This application of finite element methods allows for unprecedented insight into the mechanical properties of real-world systems and supports the development of composites containing mechanically anomalous porous materials.

  12. Preparation and identification of multifunctional mesoporous silica nanoparticles for in vitro and in vivo dual-mode imaging, theranostics, and targeted tracking.

    PubMed

    Chan, Ming-Hsien; Lin, Hsiu-Mei

    2015-04-01

    Mesoporous silica nanoparticles (MSNs) can provide a structural foundation for a new generation of nanocarriers with a broad range of functionalities. Multifunctional MSNs can serve as all-in-one diagnostic and therapeutic tools that can be used to simultaneously visualize and treat various diseases, such as cancer. This research study is the first time that two lanthanide-based imaging systems have been combined to incorporate controlled drug release and targeted tracing into a single MSN-based nano-platform for a novel theranostic drug delivery system. Doping lanthanide ions, i.e., europium (Eu) and gadolinium (Gd) ions, into an MSN structure (EuGd-MSNs) imparts fluorescence and magnetism to the nanostructure that can be used to develop magnetic resonance imaging (MRI) and biological fluorescence tools. Current cancer research has revealed that most human cancer cells express a large number of folate receptors on their surface. Grafting folic acid (FA) onto the EuGd-MSN surface (EuGd-FA-MSNs) imparts a targeting function to the MSN because of the specificity of the binding of FA to cell surface receptors. Furthermore, grafting anticancer drugs, such as camptothecin (CPT), onto the surface of these MSNs by forming disulfide bonds (EuGd-SS-CPT-FA-MSNs) enables intracellular controlled drug release. A high concentration of intracellular glutathione cleaves the disulfide bond to release the drug and treat the disease. The results of in vitro and in vivo studies show that the functionalized MSNs can be successfully used as a platform to integrate dual-imaging, targeting, and therapeutic treatment in multifunctional diagnosis drug delivery systems.

  13. An ion-imprinted amino-functionalized silica gel sorbent prepared by hydrothermal assisted surface imprinting technique for selective removal of cadmium (II) from aqueous solution

    NASA Astrophysics Data System (ADS)

    Fan, Hong-Tao; Li, Jing; Li, Zhan-Chao; Sun, Ting

    2012-02-01

    A new ion-imprinted amino-functionalized silica gel sorbent was synthesized by the hydrothermal-assisted surface imprinting technique using Cd2+ as the template, 3-[2-(2-aminoethylamino)ethylamino]propyl-trimethoxysilane (AAAPTS) as the functional monomer, and epichlorohydrin as the cross-linking agent (IIP-AAAPTS/SiO2) for the selective removal of Cd2+ from aqueous solution, and was characterized by FTIR, SEM, nitrogen adsorption and the static adsorption-desorption experiment method. The specific surface area of the IIP-AAAPTS/SiO2 sorbents was found to be 149 m2 g-1. The results showed that the maximum static adsorption capacities of IIP-AAAPTS/SiO2 sorbents by hydrothermal heating method and by the conventional heating method were 57.4 and 31.6 mg g-1, respectively. The IIP-AAAPTS/SiO2 sorbents offered a fast kinetics for the adsorption and desorption of Cd(II). The relative selectivity coefficients of IIP-AAAPTS/SiO2 sorbents for Cd2+/Co2+, Cd2+/Ni2+, Cd2+/Zn2+, Cd2+/Pb2+ and Cd2+/Cu2+ were 30.68, 14.02, 3.00, 3.12 and 6.17, respectively. IIP-AAAPTS/SiO2 sorbents had a substantial binding capacity in the range of pH 4-8 and could be used repeatedly. Equilibrium data fitted perfectly with Langmuir isotherm model compared to Freundlich isotherm model. Kinetic studies indicated that adsorption followed a pseudo-second-order model. Negative values of ΔG° indicated spontaneous adsorption and the degree of spontaneity of the reaction increased with increasing temperature. ΔH° of 26.13 kJ mol-1 due to the adsorption of Cd2+ on the IIP-AAAPTS/SiO2 sorbents indicated that the adsorption was endothermic in the experimental temperature range.

  14. Reverse Micelle Based Synthesis of Microporous Materials in Microgravity

    NASA Technical Reports Server (NTRS)

    Dutta, Prabir K.

    2001-01-01

    Microporous materials include a large group of solids of varying chemical composition as well as porosity. These materials are characterized by channels and cavities of molecular dimensions. The framework structure is made up of interconnecting T-O-T' bonds, where T and T' can be Si, Al, P, Ga, Fe, Co, Zn, B and a host of other elements. Materials with Si-O-Al bonding in the framework are called zeolites and are extensively used in many applications. Ion-exchange properties of these materials are exploited in the consumer and environmental industries. Chemical and petroleum industries use zeolites as catalysts in hydrocarbon transform ations. Synthesis of new microporous frameworks has led to the development of new technologies, and thus considerable effort worldwide is expended in their discovery. Microporous materials are typically made under hydrothermal conditions. Influence of nature of starting reactants, structure directing agents, pH, temperature, and aging all have profound influence on the synthesis process. This is primarily because the most interesting open frameworks are not necessarily the stable structures in the reaction medium. Thus, the discovery of new frameworks is often tied to finding the right composition and synthesis conditions that allow for kinetic stabilization of the structure. This complexity of the synthesis process and limited understanding of it has made it difficult to develop directed is of microporous materials and most advances in this field have been made by trial and error. The basic issues in crystal growth of these materials include: (1) Nature of the nucleation process; (2) Molecular structure and assembly of nuclei; (3) Growth of nuclei into crystals; (4) Morphology control; and (5) Transformation of frameworks into other structures. The NASA-funded research described in this paper focuses on all the above issues and has been described in several publications. We present the highlights of our program, especially with the

  15. Fundamental Studies of Crystal Growth of Microporous Materials

    NASA Technical Reports Server (NTRS)

    Dutta, P.; George, M.; Ramachandran, N.; Schoeman, B.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    Microporous materials are framework structures with well-defined porosity, often of molecular dimensions. Zeolites contain aluminum and silicon atoms in their framework and are the most extensively studied amongst all microporous materials. Framework structures with P, Ga, Fe, Co, Zn, B, Ti and a host of other elements have also been made. Typical synthesis of microporous materials involve mixing the framework elements (or compounds, thereof) in a basic solution, followed by aging in some cases and then heating at elevated temperatures. This process is termed hydrothermal synthesis, and involves complex chemical and physical changes. Because of a limited understanding of this process, most synthesis advancements happen by a trial and error approach. There is considerable interest in understanding the synthesis process at a molecular level with the expectation that eventually new framework structures will be built by design. The basic issues in the microporous materials crystallization process include: (1) Nature of the molecular units responsible for the crystal nuclei formation; (2) Nature of the nuclei and nucleation process; (3) Growth process of the nuclei into crystal; (4) Morphological control and size of the resulting crystal; (5) Surface structure of the resulting crystals; (6) Transformation of frameworks into other frameworks or condensed structures. The NASA-funded research described in this report focuses to varying degrees on all of the above issues and has been described in several publications. Following is the presentation of the highlights of our current research program. The report is divided into five sections: (1) Fundamental aspects of the crystal growth process; (2) Morphological and Surface properties of crystals; (3) Crystal dissolution and transformations; (4) Modeling of Crystal Growth; (5) Relevant Microgravity Experiments.

  16. Development of Self-Decontaminating Textiles With Microporous Membranes

    DTIC Science & Technology

    2002-01-01

    tension forces of the polymer, and a free surface of charged polymer will produce fine jets of liquid that are rapidly drawn toward a grounded target...Liquid Jets of Polymer Solutions in Electrospinning ,” J. Appl. Phys., 9, Part I, 87(2000). 3. Schmidt, K. “Manufacture and Use of Felt Pads Made from...microporous membranes have been developed at the U.S. Army Natick Soldier Center using the process of electrospinning . By electrostatically producing

  17. Microporous calcium phosphate ceramics driving osteogenesis through surface architecture.

    PubMed

    Zhang, Jingwei; Barbieri, Davide; ten Hoopen, Hetty; de Bruijn, Joost D; van Blitterswijk, Clemens A; Yuan, Huipin

    2015-03-01

    The presence of micropores in calcium phosphate (CaP) ceramics has shown its important role in initiating inductive bone formation in ectopic sites. To investigate how microporous CaP ceramics trigger osteoinduction, we optimized two biphasic CaP ceramics (i.e., BCP-R and BCP-S) to have the same chemical composition, equivalent surface area per volume, comparable protein adsorption, similar ion (i.e., calcium and phosphate) exchange and the same surface mineralization potential, but different surface architecture. In particular, BCP-R had a surface roughness (Ra) of 325.4 ± 58.9 nm while for BCP-S it was 231.6 ± 35.7 nm. Ceramic blocks with crossing or noncrossing channels of 250, 500, 1000, and 2000 µm were implanted in paraspinal muscle of dogs for 12 weeks. The percentage of bone volume in the channels was not affected by the type of pores (i.e., crossing vs. closed) or their size, but it was greatly influenced by the ceramic type (i.e., BCP-R vs. BCP-S). Significantly, more bone was formed in the channels of BCP-R than in those of BCP-S. Since the two CaP ceramics differed only in their surface architecture, the results hereby demonstrate that microporous CaP ceramics may induce ectopic osteogenesis through surface architecture.

  18. On the physical adsorption of vapors by microporous carbons

    SciTech Connect

    Bradley, R.H. . Inst. of Surface Science and Technology); Rand, B. . Division of Ceramics)

    1995-01-01

    The physical adsorption of nonpolar and polar vapors by active carbons is discussed in relation to pore structure and pore wall chemistry. For nonpolar vapors the Dubinin-Radushkevich equation is used to derive micropore volumes (W[sub 0]), average adsorption energies (E[sub 0]), and micropore widths (L) for a number of systems. These parameters are used to interpret the adsorption behavior of nitrogen which, because it is a relatively small molecule, is frequently used at 77 K to probe porosity and surface area. Results are presented for three carbons from differing precursors, namely, coal, coconut shells, and polyvinylidene chloride (PVDC) to illustrate the applicability of the technique. For the latter carbon increases in micropore size, induced by activation in carbon dioxide, and reductions in accessible pore volume caused by heat treatment in argon are also characterized and related to structural changes. The approach is then extended to the adsorption of larger hydrogen vapors, where the resulting W[sub 0] values may require correction for molecular packing effects which occur in the lower relative pressure regions of the isotherms, i.e., during the filling of ultramicropores. These packing effects are shown to limit the use of the Polanyi characteristic curve for correlating isotherm data for several vapors, of differing molecular size, by one adsorbent. Data for the adsorption of water, which is a strongly polar liquid, have been interpreted using the Dubinin-Serpinsky equation.

  19. Kinetically forbidden transformations of water molecular assemblies in hydrophobic micropores.

    PubMed

    Ohba, Tomonori; Kaneko, Katsumi

    2011-06-21

    Water adsorption hysteresis is one of the most important phenomena observed during the interaction of water with hydrophobic surfaces. Adsorption hysteresis in micropores has strong relevance to the structure of adsorbed water. We used three typical models (cluster, monolayer, and uniform distribution structure models) to determine the structure of the water molecules adsorbed in hydrophobic slit-shaped carbon micropores. In each model, stabilization energy profiles were calculated for various fractional fillings by using the interaction potential theory. Simultaneously, molecular dynamics (MD) simulations of water adsorbed in the micropore of 1.1 nm pore width, which shows significant adsorption hysteresis, were performed to determine the kinetics of the observed structural transformations. The transformations between monolayer and cluster were slow, that is, kinetically forbidden at the fractional filling of 0.2 and 0.6, whereas the cluster-uniform distribution structure and uniform distribution structure-monolayer transformations were kinetically allowed. The kinetically forbidden transformation resulted in the occurrence of metastable structure of adsorbed water and was responsible for the observed adsorption hysteresis.

  20. Silicon Micropore based Electromechanical Transducer to Differentiate Tumor Cells

    NASA Astrophysics Data System (ADS)

    Ali, Waqas; Raza, Muhammad U.; Khanzada, Raja R.; Kim, Young-Tae; Iqbal, Samir M.

    2015-03-01

    Solid-state micropores have been used before to differentiate cancer cells from normal cells using size-based filtering. Tumor cells differ from normal ones not only in size but also in physical properties like elasticity, shape, motility etc. Tumor cells show different physical attributes depending on the stage and type of cancer. We report a micropore based electromechanical transducer that differentiated cancer cells based on their mechanophysical properties. The device was interfaced with a high-speed patch-clamp measurement system that biased the ionic solution across the silicon-based membrane. The bias resulted in the flow of ionic current. Electrical pulses were generated when cells passed through. Different cells depicted characteristic pulses. Translocation profiles of cells that were either small or were more elastic and flexible caused electrical pulses shorter in widths and amplitudes whereas cells with larger size or lesser elasticity/flexibility showed deeper and wider pulses. Three non-small cell lung cancer (NSCLC) cell lines NCI-H1155, A549 and NCI-H460 were successfully differentiated. NCI-H1155, due to their comparatively smaller size, were found quickest in translocating through. The solid-sate micropore based electromechanical transducer could process the whole blood sample of cancer patient without any pre-processing requirements and is ideal for point-of-care applications. Support Acknowledged from NSF through ECCS-1201878.

  1. Microporous spongy chitosan monoliths doped with graphene oxide as highly effective adsorbent for methyl orange and copper nitrate (Cu(NO3)2) ions.

    PubMed

    Wang, Ying; Liu, Xu; Wang, Hongfang; Xia, Guangmei; Huang, Wei; Song, Rui

    2014-02-15

    In the current study, microporous spongy chitosan monoliths doped with small amount of graphene oxide (CSGO monoliths) with high porosity (96-98%), extraordinary high water absorption (more than 2000%) and low density (0.0436-0.0607 g cm(-3)) were prepared by the freeze-drying method and used as adsorbents for anionic dyes methyl orange (MO) and Cu(2+) ions. The adsorption behavior of the CSGO monoliths and influencing factors such as pH value, graphene oxide (GO) content, concentration of pollutants as well as adsorption kinetics were studied. Specifically, the saturated adsorption capacity for MO is 567.07 mg g(-1), the highest comparing with other publication results, and it is 53.69 mg g(-1) for Cu(2+) ions. Since they are biodegradable, non-toxic, efficient, low-cost and easy to prepare, we believe that these microporous spongy CSGO monoliths will be the promising candidates for water purification.

  2. Determining the sizes of micropores in activated charcoals by the pulsed NMR method

    NASA Astrophysics Data System (ADS)

    Gogelashvili, G. Sh.; Khozina, E. V.; Vartapetyan, R. Sh.; Ladychuk, D. V.; Grunin, Yu. B.

    2011-07-01

    The pulsed NMR method was used to measure the nuclear spin-spin relaxation of protons of water adsorbed in micropores of activated charcoal (AC) samples with different porous structures. A correlation was found between the spin-spin relaxation time of water protons in AC with completely filled micropores and the volume density of water primary adsorption centers in the AC samples. An equation for approximating obtained dependences is proposed that allows us to determine the volume of micropores in AC.

  3. Thermally stable hydrophobicity in electrospun silica/polydimethylsiloxane hybrid fibers

    NASA Astrophysics Data System (ADS)

    Wei, Zhonglin; Li, Jianjun; Wang, Chao; Cao, Jungang; Yao, Yongtao; Lu, Haibao; Li, Yibin; He, Xiaodong

    2017-01-01

    In order to improve practical performances of silica-based inorganic/organic hybrid fibers, silica/polydimethylsiloxane hydrophobic fibers were successfully prepared by electrospinning. Silica sol and polydimethylsiloxane can be mixed homogeneously and become stable precursor solution in dichloromethane, which allows the transformation of silica/polydimethylsiloxane precursor solution into ultrafine fibers. Flame can ignite organic groups in polydimethylsiloxane directly and destroy the hydrophobicity of hybrid fibers, but hydrophobic feature may survive if electrospun hybrid membrane is combined with thin stainless-steel-304 gauze of 150 meshes due to its thermally stable hydrophobicity (>600 °C).

  4. Controlled growth of silica-titania hybrid functional nanoparticles through a multistep microfluidic approach.

    PubMed

    Shiba, K; Sugiyama, T; Takei, T; Yoshikawa, G

    2015-11-11

    Silica/titania-based functional nanoparticles were prepared through controlled nucleation of titania and subsequent encapsulation by silica through a multistep microfluidic approach, which was successfully applied to obtaining aminopropyl-functionalized silica/titania nanoparticles for a highly sensitive humidity sensor.

  5. Electron transfer reactions in microporous solids

    SciTech Connect

    Mallouk, T.E.

    1992-05-01

    We have studied electron transfer quenching of the excited state of Ru(bpy){sub 3}{sup 2+} in aqueous suspensions of zeolites Y, L, and mordenite. The internal pore network of the zeolite is ion-exchanged with methylviologen cations, which quench the excited state of the surface-bound sensitizer. A detailed study of the quenching and charge recombination kinetics, using time-resolved luminescence quenching and transient diffuse reflectance spectroscopies, shows to remarkable effects: first, the excited state quenching is entirely dynamic is large-pore zeolites (L and Y), even when they are prepared as apparently dry'' powders (which still contain significant amounts of internally sited water). Second, a lower limit for the diffusion coefficient of the MV{sup 2+} ion in these zeolites, determined by this technique, is 10{sup {minus}7} cm{sup 2}sec, i.e., only about one order of magnitude slower than a typical ion in liquid water, and 2--3 orders of magnitude faster than charge transfer diffusion of cations in polyelectrolyte films or membranes such as Nafion. Surface sensitization of internally platinized layered oxide semiconductors such as K{sub 4-x}H{sub x}Nb{sub 6}O{sub 17}{center dot}nH{sub 2}O (x {approx} 2.5) yields photocatalysts for the production of H{sub 2} and I{sub 3{minus}} in aqueous iodide solutions. Layered alkali niobates and titanates form a class of zeolitic wide-bandap semiconductors, and are the first examples of photocatalysts that evolve hydrogen from an electrochemically reversible (i.e., non-sacrificial) electron donor with visible light excitation.

  6. High-density gold nanoparticles supported on a [Ru(bpy)(3)](2+)-doped silica/Fe3O4 nanocomposite: facile preparation, magnetically induced immobilization, and applications in ECL detection.

    PubMed

    Guo, Shaojun; Li, Jing; Wang, Erkang

    2008-09-01

    A large-scale process combined sonication with self-assembly techniques for the preparation of high-density gold nanoparticles supported on a [Ru(bpy)(3)](2+)-doped silica/Fe(3)O(4) nanocomposite (GNRSF) is provided. The obtained hybrid nanomaterials containing Fe(3)O(4) spheres have high saturation magnetization, which leads to their effective immobilization on the surface of an ITO electrode through simple manipulation by an external magnetic field (without the need of a special immobilization apparatus). Furthermore, this hybrid nanomaterial film exhibits a good and very stable electrochemiluminescence (ECL) behavior, which gives a linear response for tripropylamine (TPA) concentrations between 5 muM and 0.21 mM, with a detection limit in the micromolar range. The sensitivity of this ECL sensor can be easily controlled by the amount of [Ru(bpy)(3)](2+) immobilized on the hybrid nanomaterials (that is, varying the amount of [Ru(bpy)(3)](2+) during GNRSF synthesis).

  7. Nanoemulsion drug delivery by ketene based polyester synthesized using electron rich carbon/silica composite surface.

    PubMed

    Swarnalatha, S; Selvi, P K; Ganesh Kumar, A; Sekaran, G

    2008-09-01

    A new carrier matrix for nanoemulsion drug delivery was synthesized from glycine as the raw material, using mesoporous/microporous electron rich carbon-silica composite surface (MAC(800)). MAC(800) was prepared from rice husk in two-stage carbonization. The surface area, pore volume, and pore size distribution of MAC(800) were measured, using nitrogen adsorption isotherms at 77K. The unpaired electron density of MAC(800) was measured in electron spin resonance spectroscopy (ESR), using TEMPOL (4-hydroxy-2,2,6,6-tetramethyl piperidine-1-oxyl) as the reference spin probe. Glycine was converted into ketene at the surface of MAC(800), which further underwent radical polymerization to form a low molecular weight ketene polymer (LMKP) of ester structure. The structure and the properties of LMKP were confirmed through (13)C, (1)H and DEPT nuclear magnetic resonance (NMR) spectroscopy, attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and size exclusion chromatography (SEC). The two hydrophilic drugs namely ciprofloxacin hydrochloride (CPH) and gentamicin sulphate (GS) were chosen for the nanoemulsion preparation and characterization. They were characterized for morphology, interaction of drugs with the polymer and their crystallinity, using HR-TEM, DSC and XRD, respectively. The encapsulation efficiency of the LMKP towards the drugs ciprofloxacin hydrochloride and gentamicin sulphate were 26% and 12%, respectively. The dissolution studies of the nanoemulsion were carried out for the pH 6.5, 7.4 and 8.0. The cytocompatibility studies were done for LMKP as well as nanoemulsion using Hep2 epithelial cells.

  8. Silica-Ceria Hybrid Nanostructures

    SciTech Connect

    Munusamy, Prabhakaran; Sanghavi, Shail P.; Nachimuthu, Ponnusamy; Baer, Donald R.; Thevuthasan, Suntharampillai

    2012-04-25

    A new hybrid material system that consists of ceria attached silica nanoparticles has been developed. Because of the versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and versatile properties of silica and antioxidant properties of ceria nanoparticles, this material system is ideally suited for biomedical applications. The silica particles of size ~50nm were synthesized by the Stöber synthesis method and ceria nanoparticles of size ~2-3nm was attached to the silica surface using a hetrocoagulation method. The presence of silanol groups on the surface of silica particles mediated homogenous nucleation of ceria which were attached to silica surface by Si-O-Ce bonding. The formations of silica-ceria hybrid nanostructures were characterized by X-photoelectron spectroscopy (XPS) and high resolution transmission electron microscopy (HRTEM). The HRTEM image confirms the formation of individual crystallites of ceria nanoparticles attached to the silica surface. The XPS analysis indicates that ceria nanoparticles are chemically bonded to surface of silica and possess mixture of +3 and +4 chemical states.

  9. Sonochemical synthesis of silica particles and their size control

    NASA Astrophysics Data System (ADS)

    Kim, Hwa-Min; Lee, Chang-Hyun; Kim, Bonghwan

    2016-09-01

    Using an ultrasound-assisted sol-gel method, we successfully synthesized very uniformly shaped, monodisperse, and size-controlled spherical silica particles from a mixture of ethanol, water, and tetraethyl orthosilicate in the presence of ammonia as catalyst, at room temperature. The diameters of the silica particles were distributed in the range from 40 to 400 nm; their morphology was well characterized by scanning electron microscopy. The silica particle size could be adjusted by choosing suitable concentrations of ammonium hydroxide and water, which in turn determined the nucleation and growth rates of the particles during the reaction. This sonochemical-based silica synthesis offers an alternative way to produce spherical silica particles in a relatively short reaction time. Thus, we suggest that this simple, low-cost, and efficient method of preparing uniform silica particles of various sizes will have practical and wide-ranging industrial applicability.

  10. Silica powders for powder evacuated thermal insulating panel and method

    DOEpatents

    Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

    1994-01-01

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2 /g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

  11. Silica powders for powder evacuated thermal insulating panel and method

    DOEpatents

    Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

    1996-01-01

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2/ g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

  12. Silica powders for powder evacuated thermal insulating panel and method

    DOEpatents

    Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

    1995-01-01

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2/ g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

  13. Silica powders for powder evacuated thermal insulating panel and method

    DOEpatents

    Harris, M.T.; Basaran, O.A.; Kollie, T.G.; Weaver, F.J.

    1996-01-02

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm{sup 3} and an external surface area in the range of about 90 to 600 m{sup 2}/g is described. The silica powders are prepared by reacting a tetraalkyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders. 2 figs.

  14. Preparation of Hollow N-Chloramine-Functionalized Hemispherical Silica Particles with Enhanced Efficacy against Bacteria in the Presence of Organic Load: Synthesis, Characterization, and Antibacterial Activity.

    PubMed

    Rahma, Hakim; Asghari, Sogol; Logsetty, Sarvesh; Gu, Xiaochen; Liu, Song

    2015-06-03

    The fabrication of highly effective antimicrobial materials is an important strategy for coping with the growing concern of bacterial resistance. In this study, N-chloramine-functionalized hollow hemispherical structures were designed and prepared to examine possible enhancement of antimicrobial performance. Antimicrobial testing was carried out on Gram-negative (Escherichia coli) and Gram-positive (Baccilus Cereus) bacteria in the presence and absence of biological medium. The efficacy of the hollow hemispherical particles functionalized with various N-chloramines in killing bacteria was compared among themselves with that of small organic molecules and spherical particles to investigate the effect of the surface charge, chemical structure, and shape of the particles. Results demonstrated that quaternary ammonium salt or amine functions in the chemical structure enhanced the antimicrobial activity of the particles and made the particles more effective than the small molecules in the presence of biological medium. The importance of particle shape in the killing tests was also confirmed.

  15. Preparation of phenyl group-functionalized magnetic mesoporous silica microspheres for fast extraction and analysis of acetaldehyde in mainstream cigarette smoke by gas chromatography-mass spectrometry.

    PubMed

    Huang, Danni; Sha, Yunfei; Zheng, Saijing; Liu, Baizhan; Deng, Chunhui

    2013-10-15

    Acetaldehyde is regarded as a toxic mainstream cigarette smoke constituent, and measurement of acetaldehyde in complex real samples is difficult owing to its high volatility and reactivity. In this work, phenyl group-functionalized magnetic mesoporous microspheres were developed as the solid-phase extraction sorbents for enrichment and analysis of acetaldehyde in mainstream cigarette smoke. The functional magnetic microspheres were first synthesized through a facile one-pot co-condensation approach. The prepared nanomaterials possessed abundant silanol groups in the exterior surface and numerous phenyl groups in the interior pore-walls, as well as a large surface area (273.5m(2)/g), strong superparamagnetism and uniform mesopores (3.3 nm). Acetaldehyde in mainstream cigarette smoke was collected in water and derivatizated with O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine. The formed acetaldehyde oximes were extracted and enriched by the prepared adsorbents via π-π interactions and subsequently analyzed using GC-MS. Extraction conditions such as amounts of sorbents, eluting solvent, adsorption and desorption time were investigated and optimized to achieve the best efficiency. Method validations including linearity, recovery, repeatability, and limit of detection were also studied. It was found that the suggested methodology provided low detection limit of 0.04 mg/mL, good recovery of 88-92%, intra-day and inter-day RSD values of 4.5% and 10.1%, and linear range of 0.25-4 mg/mL (R(2)=0.999). The results indicated that the proposed method based on phenyl-functionalized magnetic mesoporous microspheres was rapid, efficient and convenient for the enrichment and analysis of acetaldehyde in tobacco.

  16. Hierarchical porous silicon carbide with controlled micropores and mesopores for electric double layer capacitors

    NASA Astrophysics Data System (ADS)

    Kim, Myeongjin; Oh, Ilgeun; Kim, Jooheon

    2015-05-01

    Three-dimensional hierarchical micro and mesoporous silicon carbide spheres (MMPSiC) are prepared by the template method and carbonization reaction via the aerosol spray drying method. The mesopores are generated by the self-assembly of the structure-directing agents, whereas the micropores are derived from the partial evaporation of Si atoms during carbonization. To investigate the effect of mesopore size on electrochemical performance, three types of MMPSiC with different mesopore size were fabricated by using three different structure directing agents (cetyltriethylammonium bromide (CTAB), Polyethylene glycol hexadecyl ether (Brij56), and Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (P123)). The MMPSiC electrode prepared with Brij56 exhibits the highest charge storage capacity with a specific capacitance of 253.7 F g-1 at a scan rate of 5 mV s-1 and 87.9% rate performance from 5 to 500 mV s-1 in 1 M Na2SO4 aqueous electrolyte. The outstanding electrochemical performance might be because of the ideal mesopore size, which effectively reduces the resistant pathways for ion diffusion in the pores and provides a large accessible surface area for ion transport/charge storage. These encouraging results demonstrate that the MMPSiC prepared with Brij56 is a promising candidate for high performance electrode materials for supercapacitors.

  17. Silazine to silica

    NASA Technical Reports Server (NTRS)

    Harvey, Gale A.

    1993-01-01

    Thin film silica and/or methyl silicone were detected on most external surfaces of the retrieved LDEF. Both solar ultraviolet radiation and atomic oxygen can convert silicones to silica. Known sources of silicone in or on the LDEF appear inadequate to explain the ubiquitous presence of the silica and silicone films. Hexamethyldisilazane (HMDS) was used as the Challenger tile waterproofing compound for the Challenger/LDEF deployment mission. HMDS is both volatile and chemically reactive at STP. In addition, HMDS releases NH3 which depolymerizes silicone RTV's. Polyurethanes are also depolymerized. Experiments are reported that indicate much of the silicone and silica contamination of LDEF resulted directly or indirectly from HMDS.

  18. Functionalized mesoporous silica materials for molsidomine adsorption: Thermodynamic study

    SciTech Connect

    Alyoshina, Nonna A.; Parfenyuk, Elena V.

    2013-09-15

    A series of unmodified and organically modified mesoporous silica materials was prepared. The unmodified mesoporous silica was synthesized via sol–gel synthesis in the presence of D-glucose as pore-forming agent. The functionalized by phenyl, aminopropyl and mercaptopropyl groups silica materials were prepared via grafting. The fabricated adsorbent materials were characterized by Fourier transform infrared spectroscopy (FTIR) analysis, N{sub 2} adsorption/desorption and elemental analysis methods. Then their adsorption properties for mesoionic dug molsidomine were investigated at 290–313 K and physiological pH value. Thermodynamic parameters of molsidomine adsorption on the synthesized materials have been calculated. The obtained results showed that the adsorption process of molsidomine on the phenyl modified silica is the most quantitatively and energetically favorable. The unmodified and mercaptopropyl modified silica materials exhibit significantly higher adsorption capacities and energies for molsidomine than the aminopropyl modified sample. The effects are discussed from the viewpoint of nature of specific interactions responsible for the adsorption. - Graphical abstract: Comparative analysis of the thermodynamic characteristics of molsidomine adsorption showed that the adsorption process on mesoporous silica materials is controlled by chemical nature of surface functional groups. Molsidomine adsorption on the phenyl modified silica is the most quantitatively and energetically favorable. Taking into account ambiguous nature of mesoionic compounds, it was found that molsidomine is rather aromatic than dipolar. Display Omitted - Highlights: • Unmodified and organically modified mesoporous silica materials were prepared. • Molsidomine adsorption on the silica materials was studied. • Phenyl modified silica shows the highest adsorption capacity and favorable energy. • Molsidomine exhibits the lowest affinity to aminopropyl modified silica.

  19. A fibrinogen-based precision microporous scaffold for tissue engineering.

    PubMed

    Linnes, Michael P; Ratner, Buddy D; Giachelli, Cecilia M

    2007-12-01

    Fibrin has been long used as an effective scaffolding material to grow a variety of cells and tissue constructs. It has been utilized mainly as a hydrogel in varying concentrations to provide an environment in which suspended cells work to rearrange the fibers and lay down their own extracellular matrix. For these fibrin hydrogels to be useful in many tissue-engineering applications, the gels must be cultured for long periods of time in order to increase their mechanical strength to the levels of native tissues. High concentrations of fibrinogen increase the mechanical strength of fibrin hydrogels, but at the same time reduce the ability of cells within the scaffold to spread and survive. We present a method to create a microporous, nanofibriliar fibrin scaffold that has controllable pore size, porosity, and microstructure for applications in tissue engineering. Fibrin has numerous advantages as a scaffolding material as it is normally used by the body as temporary scaffolding for tissue regeneration and healing, and can be autologously sourced. We present here a scaffolding process which enhances the mechanical properties of the fibrin hydrogel by forming it surrounding poly(methyl-methacrylate) beads, then removing the beads with acetone to form an interconnected microporous network. The acetone serves the dual purpose of precipitating and fixing the fibrinogen-based scaffolds as well as adding strength to the network during polymer bead removal. Effects of fibrinogen concentration and time in acetone were examined as well as polymerization with thrombin. A natural crosslinker, genipin, was also used to add strength to the scaffolds, producing a Young's modulus of up to 184+/-5 kPa after 36 h of reaction. Using these methods we were able to produce microporous fibrin scaffolds that support cell growth and have mechanical properties similar to many native tissues.

  20. Interface physics in microporous media : LDRD final report.

    SciTech Connect

    Yaklin, Melissa A.; Knutson, Chad E.; Noble, David R.; Aragon, Alicia R.; Chen, Ken Shuang; Giordano, Nicholas J.; Brooks, Carlton, F.; Pyrak-Nolte, Laura J.; Liu, Yihong

    2008-09-01

    This document contains a summary of the work performed under the LDRD project entitled 'Interface Physics in Microporous Media'. The presence of fluid-fluid interfaces, which can carry non-zero stresses, distinguishes multiphase flows from more readily understood single-phase flows. In this work the physics active at these interfaces has been examined via a combined experimental and computational approach. One of the major difficulties of examining true microporous systems of the type found in filters, membranes, geologic media, etc. is the geometric uncertainty. To help facilitate the examination of transport at the pore-scale without this complication, a significant effort has been made in the area of fabrication of both two-dimensional and three-dimensional micromodels. Using these micromodels, multiphase flow experiments have been performed for liquid-liquid and liquid-gas systems. Laser scanning confocal microscopy has been utilized to provide high resolution, three-dimensional reconstructions as well as time resolved, two-dimensional reconstructions. Computational work has focused on extending lattice Boltzmann (LB) and finite element methods for probing the interface physics at the pore scale. A new LB technique has been developed that provides over 100x speed up for steady flows in complex geometries. A new LB model has been developed that allows for arbitrary density ratios, which has been a significant obstacle in applying LB to air-water flows. A new reduced order model has been developed and implemented in finite element code for examining non-equilibrium wetting in microchannel systems. These advances will enhance Sandia's ability to quantitatively probe the rich interfacial physics present in microporous systems.

  1. Graphene-wrapped sulfur/metal organic framework-derived microporous carbon composite for lithium sulfur batteries

    NASA Astrophysics Data System (ADS)

    Chen, Renjie; Zhao, Teng; Tian, Tian; Cao, Shuai; Coxon, Paul R.; Xi, Kai; Fairen-Jimenez, David; Vasant Kumar, R.; Cheetham, Anthony K.

    2014-12-01

    A three-dimensional hierarchical sandwich-type graphene sheet-sulfur/carbon (GS-S/CZIF8-D) composite for use in a cathode for a lithium sulfur (Li-S) battery has been prepared by an ultrasonic method. The microporous carbon host was prepared by a one-step pyrolysis of Zeolitic Imidazolate Framework-8 (ZIF-8), a typical zinc-containing metal organic framework (MOF), which offers a tunable porous structure into which electro-active sulfur can be diffused. The thin graphene sheet, wrapped around the sulfur/zeolitic imidazolate framework-8 derived carbon (S/CZIF8-D) composite, has excellent electrical conductivity and mechanical flexibility, thus facilitating rapid electron transport and accommodating the changes in volume of the sulfur electrode. Compared with the S/CZIF8-D sample, Li-S batteries with the GS-S/CZIF8-D composite cathode showed enhanced capacity, improved electrochemical stability, and relatively high columbic efficiency by taking advantage of the synergistic effects of the microporous carbon from ZIF-8 and a highly interconnected graphene network. Our results demonstrate that a porous MOF-derived scaffold with a wrapped graphene conductive network structure is a potentially efficient design for a battery electrode that can meet the challenge arising from low conductivity and volume change.

  2. Graphene-wrapped sulfur/metal organic framework-derived microporous carbon composite for lithium sulfur batteries

    SciTech Connect

    Chen, Renjie E-mail: chenrj@bit.edu.cn; Zhao, Teng; Tian, Tian; Fairen-Jimenez, David; Cao, Shuai; Coxon, Paul R.; Xi, Kai E-mail: chenrj@bit.edu.cn; Vasant Kumar, R.; Cheetham, Anthony K.

    2014-12-01

    A three-dimensional hierarchical sandwich-type graphene sheet-sulfur/carbon (GS-S/C{sub ZIF8-D}) composite for use in a cathode for a lithium sulfur (Li-S) battery has been prepared by an ultrasonic method. The microporous carbon host was prepared by a one-step pyrolysis of Zeolitic Imidazolate Framework-8 (ZIF-8), a typical zinc-containing metal organic framework (MOF), which offers a tunable porous structure into which electro-active sulfur can be diffused. The thin graphene sheet, wrapped around the sulfur/zeolitic imidazolate framework-8 derived carbon (S/C{sub ZIF8-D}) composite, has excellent electrical conductivity and mechanical flexibility, thus facilitating rapid electron transport and accommodating the changes in volume of the sulfur electrode. Compared with the S/C{sub ZIF8-D} sample, Li-S batteries with the GS-S/C{sub ZIF8-D} composite cathode showed enhanced capacity, improved electrochemical stability, and relatively high columbic efficiency by taking advantage of the synergistic effects of the microporous carbon from ZIF-8 and a highly interconnected graphene network. Our results demonstrate that a porous MOF-derived scaffold with a wrapped graphene conductive network structure is a potentially efficient design for a battery electrode that can meet the challenge arising from low conductivity and volume change.

  3. Synthesis and properties of porous silica obtained by the template method

    NASA Astrophysics Data System (ADS)

    Kuznetsova, T. F.; Rat'ko, A. I.; Eremenko, S. I.

    2012-10-01

    Micromesoporous samples of SiO2 were synthesized by the sol-gel method using tetraethoxysilane as a starting reagent and 1-5 wt % cetylpyridinium chloride as a template under the conditions of preadsorption of colloid silica by polyethyleneglycol macromolecules. The adsorption and texture of the samples were studied by the low-temperature nitrogen adsorption-desorption technique. Preadsorption of silica sol was shown to affect the adsorption and capillary-condensation properties of silica. The surface area and the volume of mesopores increased at cetylpyridinium concentrations higher than 1 wt %. The micropore volume increased to a maximum. The capillary-condensation hysteresis loop of H4 type transformed into an H3 loop according to the IUPAC classification.

  4. Adsorption and desorption performance of benzene over hierarchically structured carbon-silica aerogel composites.

    PubMed

    Dou, Baojuan; Li, Jinjun; Wang, Yufei; Wang, Hailin; Ma, Chunyan; Hao, Zhengping

    2011-11-30

    Hierarchically structured carbon-silica aerogel (CSA) composites were synthesized from cheap water glass precursors and granulated activated carbon via a post-synthesis surface modification with trimethylchlorosilane (TMCS) and a low-cost ambient pressure drying procedure. The resultant CSA composites possess micro/mesoporous structure and hydrophobic surface. The adsorption and desorption performance of benzene on carbon-silica aerogel composite (CSA-2) under static and dynamic conditions were investigated, comparing with pure silica aerogel (CSA-0) and microporous activated carbon (AC). It was found that CSA-2 has high affinity towards aromatic molecules and fast adsorption kinetics. Excellent performance of dynamic adsorption and desorption observed on CSA-2 is related to its higher adsorption capacity than CSA-0 and less mass transfer resistance than AC, arising from the well-developed microporosity and open foam mesostructure in the CSA composites.

  5. Method for rapidly producing microporous and mesoporous materials

    DOEpatents

    Coronado, Paul R.; Poco, John F.; Hrubesh, Lawrence W.; Hopper, Robert W.

    1997-01-01

    An improved, rapid process is provided for making microporous and mesoporous materials, including aerogels and pre-ceramics. A gel or gel precursor is confined in a sealed vessel to prevent structural expansion of the gel during the heating process. This confinement allows the gelation and drying processes to be greatly accelerated, and significantly reduces the time required to produce a dried aerogel compared to conventional methods. Drying may be performed either by subcritical drying with a pressurized fluid to expel the liquid from the gel pores or by supercritical drying. The rates of heating and decompression are significantly higher than for conventional methods.

  6. Method for rapidly producing microporous and mesoporous materials

    DOEpatents

    Coronado, P.R.; Poco, J.F.; Hrubesh, L.W.; Hopper, R.W.

    1997-11-11

    An improved, rapid process is provided for making microporous and mesoporous materials, including aerogels and pre-ceramics. A gel or gel precursor is confined in a sealed vessel to prevent structural expansion of the gel during the heating process. This confinement allows the gelation and drying processes to be greatly accelerated, and significantly reduces the time required to produce a dried aerogel compared to conventional methods. Drying may be performed either by subcritical drying with a pressurized fluid to expel the liquid from the gel pores or by supercritical drying. The rates of heating and decompression are significantly higher than for conventional methods. 3 figs.

  7. The role of UHMW-PE in microporous PE separators

    SciTech Connect

    Wang, L.C.; Harvey, M.K.; Stein, H.L.; Scheunemann, U.

    1997-12-01

    Microporous PE separators have gained large popularity in the lead acid battery industry, particularly in SLI (Starting, Lighting and Ignition) Automotive Applications. The PE (Polyethylene) in battery separator is actually UHMW-PE (Ultra High Molecular Weight Polyethylene). UHMW-PE has a molecular weight more than ten times that of conventional HDPE (High Density Polyethylene). This paper gives an overview of the UHMW-PE`s contributions to the PE battery separator process, assembly, and performance, in comparison to other conventional separators, such as PVC (Polyvinyl Chloride), cellulose, and glass fiber.

  8. Microporous organic polymers for gas storage and separation applications.

    PubMed

    Chang, Ze; Zhang, Da-Shuai; Chen, Qiang; Bu, Xian-He

    2013-04-21

    Microporous organic polymers (MOPs), an emerging class of functional porous materials featured with the pure organic component have been widely studied in recent years. These materials have potential uses in areas such as storage, separation, and catalysis. In this Perspective, we focused on the gas storage and separation of MOPs. The targeted design and synthesis of MOPs toward the enhancement of gas capacity and selectivity are discussed. Furthermore, special emphasis is given to the post-synthesis modification of MOPs which have been proved to be effective methods to accurately tune the desired properties.

  9. Essential design considerations for microporous implants: preliminary communication.

    PubMed Central

    Cameron, H U

    1981-01-01

    The introduction of microporous metallic implants into which bone can grow to stabilize the implant has necessitated considerable work prior to clinical studies. Ten years of bench and animal testing have resulted in a clinically available prosthesis with a multilayer porous coating with a pore size of 50-300 mu. Initial clinical trials with a 50-100 mu hip prosthesis indicated the necessity to increase the pore size to 300 mu and clinical studies of such prostheses are at present underway. Images Figure 1. PMID:7321013

  10. Interfacial interaction between the epoxidized natural rubber and silica in natural rubber/silica composites

    NASA Astrophysics Data System (ADS)

    Xu, Tiwen; Jia, Zhixin; Luo, Yuanfang; Jia, Demin; Peng, Zheng

    2015-02-01

    The epoxidized natural rubber (ENR) as an interfacial modifier was used to improve the mechanical and dynamical mechanical properties of NR/silica composites. In order to reveal the interaction mechanism between ENR and silica, the ENR/Silica model compound was prepared by using an open mill and the interfacial interaction of ENR with silica was investigated by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), X-ray diffraction (XRD) and stress-strain testing. The results indicated that the ring-opening reaction occurs between the epoxy groups of ENR chains and Si-OH groups on the silica surfaces and the covalent bonds are formed between two phases, which can improve the dispersion of silica in the rubber matrix and enhance the interfacial combination between rubber and silica. The ring-opening reaction occurs not only in vulcanization process but also in mixing process, meanwhile, the latter seems to be more important due to the simultaneous effects of mechanical force and temperature.

  11. Development and characterization of chitosan/silica nanocomposite membranes

    NASA Astrophysics Data System (ADS)

    Kumar, Amit; Gahlot, Swati; Kulshrestha, Vaibhav; Shahi, V. K.

    2014-04-01

    Quaternized Chitosan/silica based composite membranes were prepared for pervaporation dehydration of water-ethanol mixture. Silica content in membrane matrix has been systematically optimized to control the nanostructure of the developed polymer matrix for studying the effects of molecular structure on the swelling, and PV performance. Among prepared membranes, 40% silica composite membrane shows the remarkable results for the water removal from water/ethanol mixture (80% ethanol + 20% water (w/w)). Contact angle measurement support the PV data as nature of CH-3 membrane is more hydrophilic comparative to others. SEM micrographs show the surface uniformity of the membranes.

  12. Wear behavior of light-cured resin composites with bimodal silica nanostructures as fillers.

    PubMed

    Wang, Ruili; Bao, Shuang; Liu, Fengwei; Jiang, Xiaoze; Zhang, Qinghong; Sun, Bin; Zhu, Meifang

    2013-12-01

    To enhance wear behavior of resin composites, bimodal silica nanostructures including silica nanoparticles and silica nanoclusters were prepared and proposed as fillers. The silica nanoclusters, a combination of individually dispersed silica nanoparticles and their agglomerations, with size distribution of 0.07-2.70 μm, were fabricated by the coupling reaction between amino and epoxy functionalized silica nanoparticles, which were obtained by the surface modification of silica nanoparticles (~70 nm) using 3-aminopropyl triethoxysilane (APTES) and 3-glycidoxypropyl trimethoxysilane (GPS) as coupling agents, respectively. Silica nanoparticles and nanoclusters were then silanized with 3-methacryloxypropyl trimethoxysilane (γ-MPS) to prepare composites by mixing with bisphenol A glycerolate dimethacrylate (Bis-GMA) and tri (ethylene glycol) dimethacrylate (TEGDMA). Experimental composites with various filler compositions were prepared and their wear behaviors were assessed in this work. The results suggested that composites with increasing addition of silica nanoparticles in co-fillers possessed lower wear volume and smoother worn surface. Particularly, the composite 53:17 with the optimum weight ratio of silica nanoparticles and silica nanoclusters presented the excellent wear behavior with respect to that of the commercial Esthet-X, although the smallest wear volume was achieved by Z350 XT. The introduction of bimodal silica nanostructures as fillers might provide a new sight for the design of resin composites with significantly improved wear resistance.

  13. Fluorescent single walled carbon nanotube/silica composite materials.

    PubMed

    Satishkumar, B C; Doorn, Stephen K; Baker, Gary A; Dattelbaum, Andrew M

    2008-11-25

    We present a new approach for the preparation of single walled carbon nanotube silica composite materials that retain the intrinsic fluorescence characteristics of the encapsulated nanotubes. Incorporation of isolated nanotubes into optically transparent matrices, such as sol-gel prepared silica, to take advantage of their near-infrared emission properties for applications like sensing has been a challenging task. In general, the alcohol solvents and acidic conditions required for typical sol-gel preparations disrupt the nanotube/surfactant assembly and cause the isolated nanotubes to aggregate leading to degradation of their fluorescence properties. To overcome these issues, we have used a sugar alcohol modified silica precursor molecule, diglycerylsilane, for encapsulation of nanotubes in silica under aqueous conditions and at neutral pH. The silica/nanotube composite materials have been prepared as monoliths, at least 5 mm thick, or as films (<1 mm) and were characterized using fluorescence and Raman spectroscopy. In the present work we have investigated the fluorescence characteristics of the silica encapsulated carbon nanotubes by means of redox doping studies as well as demonstrated their potential for biosensing applications. Such nanotube/silica composite systems may allow for new sensing and imaging applications that are not currently achievable.

  14. Guest-responsive reversible swelling and enhanced fluorescence in a super-absorbent, dynamic microporous polymer.

    PubMed

    Rao, K Venkata; Mohapatra, Sudip; Maji, Tapas Kumar; George, Subi J

    2012-04-10

    A swell idea! The guest-responsive reversible swelling and fluorescence enhancement of a dynamic, microporous polymer network is presented. Guest-induced breathing of hydrophobic pores imparts multi-functional properties, such as super-absorbency, phase-selective swelling of oil from water and encapsulation of C(60) (see figure), to this soft micro-porous organic polymer.

  15. Electrochemical synthesis of polyaniline in the micropores of activated carbon for high-performance electrochemical capacitors.

    PubMed

    Itoi, Hiroyuki; Hayashi, Shinya; Matsufusa, Hidenori; Ohzawa, Yoshimi

    2017-03-14

    Polyaniline (PANI) was synthesized exclusively inside the micropores of activated carbon (AC). This nanosized PANI was smaller than 2 nm in diameter and allowed for fast redox reactions, exhibiting superior pseudocapacitance in terms of power and energy densities over the electric double layer capacitance generated inside the micropores.

  16. NMR characterization of the hydrogen storage properties of microporous materials

    NASA Astrophysics Data System (ADS)

    Anderson, Robert James

    Nuclear magnetic resonance techniques were employed to study properties and characteristics related to hydrogen storage within a variety of carbon nanomaterials. NMR methods were established for studying adsorption at temperatures of 100 and 290 K, and hydrogen pressures up to 10 MPa. A standard interpretation of the NMR spectra of molecular hydrogen in microporous materials was developed. The characterization of three samples are included here: boron-doped graphite, activated PEEK (a polymer), and zeolite-templated carbon. In all of the studies discussed here, each sample necessitated a custom approach to interpreting the data. The chemical shift, a relaxation filter, and low temperature dynamics were needed to uncover a significantly enhanced binding energy in the boron-doped graphite. The key result of the activated PEEK work was that at 100 K, the pressure-dependent behavior of the chemical shift of the micropore spectral component could be directly linked to the dimensions of the pore. The zeolite-templated carbon displayed local paramagnetic behavior within its pores but was diamagnetic in the bulk form. Pressure-dependent chemical shift analysis revealed that the paramagnetic behavior could be related to the numerous edge sites present.

  17. Tailored crystalline microporous materials by post-synthesis modification.

    PubMed

    Valtchev, Valentin; Majano, Gerardo; Mintova, Svetlana; Pérez-Ramírez, Javier

    2013-01-07

    Crystalline microporous solids are an important class of inorganic materials with uses in different areas impacting our everyday lives, namely as catalysts, adsorbents, and ion exchangers. Advancements in synthesis have been invaluable in expanding the classical aluminosilicate zeolites to new unique framework types and compositions, motivating innovative developments. However, the inexhaustible post-synthetic options to tailor zeolite properties have been and will continue to be indispensable to realize emerging and to improve conventional applications. Starting from the routine drying and template removal processes that every zeolite must experience prior to use, a wide spectrum of treatments exists to alter individual or collective characteristics of these materials for optimal performance. This review documents the toolbox of post-synthetic strategies available to tune the properties of zeolitic materials for specific functions. The categorisation is based on the scale at which the alteration is aimed at, including the atomic structure (e.g. the introduction, dislodgment, or replacement of framework atoms), the micropore level (e.g. template removal and functionalisation by inorganic and organic species), and the crystal and particle levels (e.g. the introduction of auxiliary porosity). Through examples in the recent literature, it is shown that the combination of post-synthetic methods enables rational zeolite design, extending the characteristics of these materials way beyond those imposed by the synthesis conditions.

  18. Detritiation of water using microporous hollow-fiber membranes

    SciTech Connect

    Kelso, R.C.; Ahmed, T.; Middlebrooks, E.J.

    1997-03-01

    A novel concept of tritium (HTO) removal with microporous hollow fiber membranes was evaluated in this study. Small-scale laboratory modules were constructed and tested to determine the mass transfer characteristics of the hollow fibers under varying system parameters. Tritiated water is pumped through the fiber lumen and air, saturated with water vapor, is pumped over the exterior of the fibers in a countercurrent mode. The high HTO concentration gradient encourages the HTO to diffuse across the porous membrane wall, and to transfer directly into the saturated air stream. A dimensionless mathematical correlation that predicts the tritium transfer coefficient across the membranes is presented for parallel flow modules. The measured overall mass transfer coefficients in the membrane module are two to three orders of magnitude greater than those of conventional bubble stripping. In additions, factors that influence the mass transfer performance of the membrane modules in practical applications are evaluated. The results indicate that very low concentrations of HTO can be separated from water using microporous hollow fiber membranes. 33 refs., 8 figs., 3 tabs.

  19. Microporous polystyrene particles for selective carbon dioxide capture.

    PubMed

    Kaliva, Maria; Armatas, Gerasimos S; Vamvakaki, Maria

    2012-02-07

    This study presents the synthesis of microporous polystyrene particles and the potential use of these materials in CO(2) capture for biogas purification. Highly cross-linked polystyrene particles are synthesized by the emulsion copolymerization of styrene (St) and divinylbenzene (DVB) in water. The cross-link density of the polymer is varied by altering the St/DVB molar ratio. The size and the morphology of the particles are characterized by scanning and transmission electron microscopy. Following supercritical point drying with carbon dioxide or lyophilization from benzene, the polystyrene nanoparticles exhibit a significant surface area and permanent microporosity. The dried particles comprising 35 mol % St and 65 mol % DVB possess the largest surface area, ∼205 m(2)/g measured by Brunauer-Emmett-Teller and ∼185 m(2)/g measured by the Dubinin-Radushkevich method, and a total pore volume of 1.10 cm(3)/g. Low pressure measurements suggest that the microporous polystyrene particles exhibit a good separation performance of CO(2) over CH(4), with separation factors in the range of ∼7-13 (268 K, CO(2)/CH(4) = 5/95 gas mixture), which renders them attractive candidates for use in gas separation processes.

  20. In vivo iontophoretic delivery of salmon calcitonin across microporated skin.

    PubMed

    Vemulapalli, Viswatej; Bai, Yun; Kalluri, Haripriya; Herwadkar, Anushree; Kim, Hyun; Davis, Shawn P; Friden, Phil M; Banga, Ajay K

    2012-08-01

    The purpose of this study was to determine the effect of microneedle (MN) technology and its combination with iontophoresis (ITP) on the in vivo transdermal delivery of salmon calcitonin (sCT). Maltose MNs (500 µm) were used to porate skin prior to application of the drug, with or without ITP. Micropores created by maltose MNs were characterized by histological sectioning and calcein imaging studies, which indicated uniformity of the created micropores. In vivo studies were performed in hairless rats to assess the degree of enhancement achieved by ITP (0.2 mA/cm² for 1 h), MNs (81 MNs), and their combination. In vivo studies indicate a serum maximal concentration of 0.61 ± 0.42 ng/mL, 1.79 ± 0.72 ng/mL, and 5.51 ± 0.32 ng/mL for ITP, MNs, and combination treatment, respectively. MN treatment alone increased serum concentration 2.5-fold and the combination treatment increased the concentration ninefold as compared with iontophoretic treatment alone. Combination treatment of ITP and MNs resulted in the highest delivery of sCT and therapeutic levels were achieved within 5 min of administration.

  1. Silica, Silicosis, and Autoimmunity

    PubMed Central

    Pollard, Kenneth Michael

    2016-01-01

    Inhalation of dust containing crystalline silica is associated with a number of acute and chronic diseases including systemic autoimmune diseases. Evidence for the link with autoimmune disease comes from epidemiological studies linking occupational exposure to crystalline silica dust with the systemic autoimmune diseases systemic lupus erythematosus, systemic sclerosis, and rheumatoid arthritis. Although little is known regarding the mechanism by which silica exposure leads to systemic autoimmune disease, there is a voluminous literature on silica exposure and silicosis that may help identify immune processes that precede development of autoimmunity. The pathophysiology of silicosis consists of deposition of silica particles in the alveoli of the lung. Ingestion of these particles by macrophages initiates an inflammatory response, which stimulates fibroblasts to proliferate and produce collagen. Silica particles are encased by collagen leading to fibrosis and the nodular lesions characteristic of the disease. The steps in the development of silicosis, including acute and chronic inflammation and fibrosis, have different molecular and cellular requirements, suggesting that silica-induced inflammation and fibrosis may be mechanistically separate. Significantly, it is unclear whether silica-induced inflammation and fibrosis contribute similarly to the development of autoimmunity. Nonetheless, the findings from human and animal model studies are consistent with an autoimmune pathogenesis that begins with activation of the innate immune system leading to proinflammatory cytokine production, pulmonary inflammation leading to activation of adaptive immunity, breaking of tolerance, and autoantibodies and tissue damage. The variable frequency of these immunological features following silica exposure suggests substantial genetic involvement and gene/environment interaction in silica-induced autoimmunity. However, numerous questions remain unanswered. PMID:27014276

  2. Europium (II)-doped microporous zeolite derivatives with enhanced photoluminescence by isolating active luminescence centers.

    PubMed

    Yang, Xuyong; Tiam, Tan Swee; Yu, Xibin; Demir, Hilmi Volkan; Sun, Xiao Wei

    2011-11-01

    Solid-state reaction is the most common method for preparing luminescent materials. However, the luminescent dopants in the hosts tend to aggregate in the high-temperature annealing process, which causes adverse effect in photoluminescence. Herein, we report a novel europium (II)-doped zeolite derivative prepared by a combined ion-exchange and solid-state reaction method, in which the europium (II) ions are isolated to a large extent by the micropores of the zeolite. Excited by a broad ultraviolet band from 250 to 420 nm, a strong blue emission peaking at 450 nm was observed for these Eu-embedded zeolites annealed at 800 °C in a reducing atmosphere. The zeolite host with pores of molecular dimension was found to be an excellent host to isolate and stabilize the Eu(2+) ions. The as-obtained europium (II)-doped zeolite derivative showed an approximately 9 fold enhancement in blue emission compared to that of the general europium (II)-doped aluminosilicates obtained by conventional solid-state reaction, indicating that, by isolating active luminescence centers, it is promising to achieve highly luminescent materials. Also, the strong blue emission with broad UV excitation band suggests a potential candidate of phosphor for ultraviolet excited light-emitting diode.

  3. A microporous silk carbon-ionic liquid composite for the electrochemical sensing of dopamine.

    PubMed

    Wang, Min; Bai, Lu; Zhang, Lingling; Sun, Guangping; Zhang, Xiaowei; Dong, Shaojun

    2016-04-21

    Porous silk carbon (Silk C) was obtained through carbonization and KOH activation of natural silk cocoons. The as-prepared Silk C presented the good characteristics of a large surface area (SBET: 2854.53 m(2) g(-1)) and a high volume of pores (1.54 cm(3) g(-1)) with uniform micropores (2.5 nm) and multiple defects. The metal-free silk carbon-ionic liquid (Silk C-IL) composite, synthesized by modifying Silk C with ionic liquid through non-covalent (π-π) interactions under grinding conditions, was prepared for electrochemical determination of dopamine (DA). The detection limit of DA was 79 nM (S/N = 3) with a linear range from 0.6 μM to 140 μM. Meanwhile, the as-made Silk C-IL/GCE presented good selectivity for DA detection from other possible interferences, such as ascorbic acid, glucose and uric acid. Furthermore, the Silk C-IL/GCE was also successfully used for the detection of DA in fetal bovine serum and dopamine hydrochloride injection samples.

  4. Microporous nano-MgO/diatomite ceramic membrane with high positive surface charge for tetracycline removal.

    PubMed

    Meng, Xian; Liu, Zhimeng; Deng, Cheng; Zhu, Mengfu; Wang, Deyin; Li, Kui; Deng, Yu; Jiang, Mingming

    2016-12-15

    A novel microporous nano-MgO/diatomite ceramic membrane with high positive surface charge was prepared, including synthesis of precursor colloid, dip-coating and thermal decomposition. Combined SEM, EDS, XRD and XPS studies show the nano-MgO is irregularly distributed on the membrane surface or pore walls and forms a positively charged nano coating. And the nano-MgO coating is firmly attached to the diatomite membrane via SiO chemical bond. Thus the nano-MgO/diatomite membrane behaves strong electropositivity with the isoelectric point of 10.8. Preliminary filtration tests indicate that the as-prepared nano-MgO/diatomite membrane could remove approximately 99.7% of tetracycline in water through electrostatic adsorption effect. The desirable electrostatic property enables the nano-MgO/diatomite membrane to be a candidate for removal of organic pollutants from water. And it is convinced that there will be a great application prospect of charged ceramic membrane in water treatment field.

  5. Microporous Ni-doped TiO2 film photocatalyst by plasma electrolytic oxidation.

    PubMed

    Yao, Zhongping; Jia, Fangzhou; Tian, Shujun; Li, ChunXiang; Jiang, Zhaohua; Bai, Xuefeng

    2010-09-01

    Ni-doped TiO2 film catalysts were prepared by a plasma electrolytic oxidation (PEO) method and were mainly characterized by means of SEM, EDS, XRD, XPS, and DRS, respectively. The effects of Ni doping on the structure, composition and optical absorption property of the film catalysts were investigated along with their inherent relationships. The results show that the film catalyst is composed of anatase and rutile TiO2 with microporous structure. Doping Ni changes the phase composition and the lattice parameters (interplanar crystal spacing and cell volume) of the films. The optical absorption range of TiO2 film gradually expands and shifts to the red with increasing dosages. Both direct and indirect transition band gaps of the TiO2 films are deduced consequently. Moreover, the photocatalytic activity of the film catalysts for splitting Na2S+Na2SO3 solution into H2 is enhanced by doping with an appropriate amount of Ni. The as-prepared TiO2 film catalyst doping with 10 g/L of Ni(Ac)2 presents the highest photocatalytic reducing activity.

  6. Application of silica nanoparticles for increased silica availability in maize

    NASA Astrophysics Data System (ADS)

    Suriyaprabha, R.; Karunakaran, G.; Yuvakkumar, R.; Prabu, P.; Rajendran, V.; Kannan, N.

    2013-02-01

    Silica nanoparticles were extracted from rice husk and characterised comprehensively. The synthesised silica powders were amorphous in size with 99.7% purity (20-40 nm). Nanosilica was amended with red soil at 15 kg ha-1 along with micron silica. The influence of nanoscale on silica uptake, accumulation and nutritional variations in maize roots were evaluated through the studies such as root sectioning, elemental analysis and physiological parameters (root length and silica content) and compared with micron silica and control. Nanosilica treated soil reveals enhanced silica uptake and elongated roots which make the plant to resist in stress conditions like drought.

  7. High resolution patterning of silica aerogels

    SciTech Connect

    Bertino, M.F.; Hund, J.F.; Sosa, J.; Zhang, G.; Sotiriou-Leventis, C.; Leventis, N.; Tokuhiro, A.T.; Terry, J.

    2008-10-30

    Three-dimensional metallic structures are fabricated with high spatial resolution in silica aerogels. In our method, silica hydrogels are prepared with a standard base-catalyzed route, and exchanged with an aqueous solution typically containing Ag{sup +} ions (1 M) and 2-propanol (0.2 M). The metal ions are reduced photolytically with a table-top ultraviolet lamp, or radiolytically, with a focused X-ray beam. We fabricated dots and lines as small as 30 x 70 {micro}m, protruding for several mm into the bulk of the materials. The hydrogels are eventually supercritically dried to yield aerogels, without any measurable change in the shape and spatial resolution of the lithographed structures. Transmission electron microscopy shows that illuminated regions are composed by Ag clusters with a size of several {micro}m, separated by thin layers of silica.

  8. Fullerene-silica complexes for medical chemistry

    NASA Astrophysics Data System (ADS)

    Sheka, E. F.

    2007-06-01

    A quantum-chemical study of the interaction of C60 fullerene with nanosized silica was performed. It was demonstrated that a fullerene molecule forms a weakly bound complex with a pyrogenic silica (Aerosil) particle only via the interaction with the silanediol groups of the hydroxyl covering on the particle. By contrast, a fullerene molecule is not bonded to an individual siloxane cycle, and, therefore, fullerosilica gel is formed due to the retention of fullerene molecules in pores of silica gel as a result cooperative action of the siloxane cycles comprising the pore. In both cases, the predicted medico-biological action of medicinal preparations is due to the radical-like and donor-acceptor characteristics of the C60 molecule.

  9. Silica-based cationic bilayers as immunoadjuvants

    PubMed Central

    Lincopan, Nilton; Santana, Mariana RA; Faquim-Mauro, Eliana; da Costa, Maria Helena B; Carmona-Ribeiro, Ana M

    2009-01-01

    Background Silica particles cationized by dioctadecyldimethylammonium bromide (DODAB) bilayer were previously described. This work shows the efficiency of these particulates for antigen adsorption and presentation to the immune system and proves the concept that silica-based cationic bilayers exhibit better performance than alum regarding colloid stability and cellular immune responses for vaccine design. Results Firstly, the silica/DODAB assembly was characterized at 1 mM NaCl, pH 6.3 or 5 mM Tris.HCl, pH 7.4 and 0.1 mg/ml silica over a range of DODAB concentrations (0.001–1 mM) by means of dynamic light scattering for particle sizing and zeta-potential analysis. 0.05 mM DODAB is enough to produce cationic bilayer-covered particles with good colloid stability. Secondly, conditions for maximal adsorption of bovine serum albumin (BSA) or a recombinant, heat-shock protein from Mycobacterium leprae (18 kDa-hsp) onto DODAB-covered or onto bare silica were determined. At maximal antigen adsorption, cellular immune responses in vivo from delayed-type hypersensitivity reactions determined by foot-pad swelling tests (DTH) and cytokines analysis evidenced the superior performance of the silica/DODAB adjuvant as compared to alum or antigens alone whereas humoral response from IgG in serum was equal to the one elicited by alum as adjuvant. Conclusion Cationized silica is a biocompatible, inexpensive, easily prepared and possibly general immunoadjuvant for antigen presentation which displays higher colloid stability than alum, better performance regarding cellular immune responses and employs very low, micromolar doses of cationic and toxic synthetic lipid. PMID:19152701

  10. Synthesis and properties of water-soluble core-shell-shell silica-CdSe/CdS-silica nanoparticles.

    PubMed

    Lin, Yang-Wei; Liu, Chi-Wei; Chang, Huan-Tsung

    2006-04-01

    This paper describes the synthesis of highly water-soluble and fluorescent core-shell-shell silica-CdSe/CdS-silica nanoparticles (CSS silica-QDs-silica NPs). We used cadmium nitrate and 1,1-dimethyl-2-selenourea precursors to synthesize CdSe quantum dots (QDs) in aqueous solution under simultaneous illumination with a diode-pumped solid state green laser and a Xe-Hg lamp. After passivation of the CdSe QDs with CdS, the CdSe/CdS QDs were then conjugated covalently to (3-mercaptopropyl)trimethoxysilane (MPS); we call these nanoparticles "MPS-QDs". We mixed the MPS-QDs with tetraethoxysilane (TEOS), ethanol, and NH3. By controlling the concentrations of the reagents, the stirring speed, and the reaction time, we synthesized CSS silica-QDs-silica NPs having sizes ranging from 75 to 190 nm. The incubation time for preparing the MPS-QDs and their concentrations are important parameters in determining the morphologies of the CSS silica-QDs-silica NPs. When we mixed 50 nM MPS-QDs, 1.1 mM TEOS, and 78 mM NH3 and reacted them at a stirring speed of 750 rpm, we obtained 85-nm-diameter CSS silica-QDs-silica NPs having a QD shell thickness of about 20 nm. The CSS silica-QDs-silica NPs provide a strong photoluminescence intensity (quantum yield 88%) and exhibit enhanced stability both photochemically and in high-conductivity media (e.g., 1.0 M NaCl).

  11. Direct formation of S-nitroso silica nanoparticles from a single silica source.

    PubMed

    Chou, Hung-Chang; Chiu, Shih-Jiuan; Liu, Ying-Ling; Hu, Teh-Min

    2014-01-28

    Nitric oxide (NO) is a ubiquitous molecule in the body. Because of its multiple pathophysiologic roles, the potential for treating various diseases by the exogenous administration of NO has been under intensive investigation. However, the unstable, radical nature of NO poses a major challenge to the effective delivery of NO. Previously, silica nanoparticles synthesized by the traditional method have been developed into NO-carrying systems. In the present study, for the first time NO-carrying silica nanoparticles were prepared from a single silica precursor using a simple nanoprecipitation method. (3-Mercaptopropyl)-trimethoxysilane (MPTMS) was used as the sole silane source, which was subjected to acid-catalyzed S-nitrosation and condensation reactions in a one-pot organic phase. S-Nitroso silica nanoparticles (SNO-SiNPs) were then produced by injecting a smaller quantity of the organic phase into a larger amount of water without surfactants. Various preparation parameters were tested to obtain optimized conditions. Moreover, a phase diagram demonstrating the ouzo effect was constructed. The prepared SNO-SiNPs were spherical particles with a tunable size in the range of 100-400 nm. The nanoparticles in aqueous dispersions exhibited high colloid stability, possibly resulting from highly negatively charged surfaces. The result of solid-state (29)Si NMR shows the predominance of T(2) and T(3) silicon structures, suggesting that nanoparticles were formed from polycondensed silica species. In conclusion, NO-loaded silica nanoparticles have been directly prepared from a single silane precursor using a surfactant-free, low-energy, one-step nanoprecipitation approach. The method precludes the need for the initial formation of bare particles and subsequent functionalization steps.

  12. Synthetic zeolites and other microporous oxide molecular sieves.

    PubMed

    Sherman, J D

    1999-03-30

    Use of synthetic zeolites and other microporous oxides since 1950 has improved insulated windows, automobile air-conditioning, refrigerators, air brakes on trucks, laundry detergents, etc. Their large internal pore volumes, molecular-size pores, regularity of crystal structures, and the diverse framework chemical compositions allow "tailoring" of structure and properties. Thus, highly active and selective catalysts as well as adsorbents and ion exchangers with high capacities and selectivities were developed. In the petroleum refining and petrochemical industries, zeolites have made possible cheaper and lead-free gasoline, higher performance and lower-cost synthetic fibers and plastics, and many improvements in process efficiency and quality and in performance. Zeolites also help protect the environment by improving energy efficiency, reducing automobile exhaust and other emissions, cleaning up hazardous wastes (including the Three Mile Island nuclear power plant and other radioactive wastes), and, as specially tailored desiccants, facilitating the substitution of new refrigerants for the ozone-depleting chlorofluorocarbons banned by the Montreal Protocol.

  13. Functionalizing Microporous Membranes for Protein Purification and Protein Digestion.

    PubMed

    Dong, Jinlan; Bruening, Merlin L

    2015-01-01

    This review examines advances in the functionalization of microporous membranes for protein purification and the development of protease-containing membranes for controlled protein digestion prior to mass spectrometry analysis. Recent studies confirm that membranes are superior to bead-based columns for rapid protein capture, presumably because convective mass transport in membrane pores rapidly brings proteins to binding sites. Modification of porous membranes with functional polymeric films or TiO₂ nanoparticles yields materials that selectively capture species ranging from phosphopeptides to His-tagged proteins, and protein-binding capacities often exceed those of commercial beads. Thin membranes also provide a convenient framework for creating enzyme-containing reactors that afford control over residence times. With millisecond residence times, reactors with immobilized proteases limit protein digestion to increase sequence coverage in mass spectrometry analysis and facilitate elucidation of protein structures. This review emphasizes the advantages of membrane-based techniques and concludes with some challenges for their practical application.

  14. Functionalizing Microporous Membranes for Protein Purification and Protein Digestion

    NASA Astrophysics Data System (ADS)

    Dong, Jinlan; Bruening, Merlin L.

    2015-07-01

    This review examines advances in the functionalization of microporous membranes for protein purification and the development of protease-containing membranes for controlled protein digestion prior to mass spectrometry analysis. Recent studies confirm that membranes are superior to bead-based columns for rapid protein capture, presumably because convective mass transport in membrane pores rapidly brings proteins to binding sites. Modification of porous membranes with functional polymeric films or TiO2 nanoparticles yields materials that selectively capture species ranging from phosphopeptides to His-tagged proteins, and protein-binding capacities often exceed those of commercial beads. Thin membranes also provide a convenient framework for creating enzyme-containing reactors that afford control over residence times. With millisecond residence times, reactors with immobilized proteases limit protein digestion to increase sequence coverage in mass spectrometry analysis and facilitate elucidation of protein structures. This review emphasizes the advantages of membrane-based techniques and concludes with some challenges for their practical application.

  15. Magnetic modification of microporous carbon for dye adsorption.

    PubMed

    Kyzas, George Z; Deliyanni, Eleni A; Lazaridis, Nikolaos K

    2014-09-15

    In this study, impregnation of microporous activated carbon with magnetite was achieved by co-precipitation of iron salts onto activated carbon. The evaluation of the adsorption ability of this material was examined using the anionic dye Reactive Black 5 as model dye pollutant (adsorbate). The effect of pH, ionic strength, contact time and initial dye concentration were also studied. It was found that high pH and high ionic strength favor the adsorption of Reactive Black 5. The adsorption kinetics and isotherms were well fitted by the fractal BS model and Langmuir model, respectively. The impregnation with magnetite decreases the adsorption capacity of activated carbon. Thermal re-activation of dye-loaded activated carbons was also succeeded. The characterization of the magnetic carbons was investigated by various techniques (SEM/EDAX, VSM, BET, FTIR, XRD, DTG) revealing many possible interactions in the carbon-dye system.

  16. Selective gas sensitivity of a microporous barrier-equipped chemoresistor

    NASA Astrophysics Data System (ADS)

    Nemati, Kianoosh; Rahbarpour, Saeedeh

    2011-08-01

    A slab of chemically passive microporous ceramic material is attached to the gas sensitive surface of a chemoresistor. When exposed to analyte contaminated air, analyte molecules diffuse through the slab before affecting the sensor. We compared the transient responses of the barrier-equipped sensor with those of a bare device and resulted in the information regarding the rate process of the analyte's diffusion through the barrier. Rooted in the molecular diffusion equation and the Langmuir model of gas adsorption, a nonlinear partial differential equation was derived to describe the diffusion-physisorption of the analyte in the porous medium. The fitting parameters of the model to the experimental results were utilized as features for analyte identification. These features were used for the classification of different volatile organic substances. Our fabricated sample could recognize methanol, ethanol, 2-propanol and 1-butanol vapors in a wide concentration range in air.

  17. Reactive Infiltration of Silicon Melt Through Microporous Amorphous Carbon Preforms

    NASA Technical Reports Server (NTRS)

    Sangsuwan, P.; Tewari, S. N.; Gatica, J. E.; Singh, M.; Dickerson, R.

    1999-01-01

    The kinetics of unidirectional capillary infiltration of silicon melt into microporous carbon preforms have been investigated as a function of the pore morphology and melt temperature. The infiltrated specimens showed alternating bands of dark and bright regions, which corresponded to the unreacted free carbon and free silicon regions, respectively. The decrease in the infiltration front velocity for increasing infiltration distances, is in qualitative agreement with the closed-form solution of capillarity driven fluid flow through constant cross section cylindrical pores. However, drastic changes in the thermal response and infiltration front morphologies were observed for minute differences in the preforms microstructure. This suggests the need for a dynamic percolation model that would account for the exothermic nature of the silicon-carbon chemical reaction and the associated pore closing phenomenon.

  18. A Three-Dimensional Microporous Metal-Metalloporphyrin Framework

    SciTech Connect

    Guo, Zhiyong; Yan, Dan; Wang, Hailong; Tesfagaber, Daniel; Li, Xinle; Chen, Yusheng; Huang, Wenyu; Chen, Banglin

    2015-01-14

    A new porphyrin-based microporous MOF, {Mn(II)0.5[Mn(II)4Cl(Mn(III)Cl-ttzpp)2(H2O)4]}·(DEF)20·(CH3OH)18·(H2O)12 (UTSA-57), has been constructed from {5,10,15,20-tetrakis[4-(2,3,4,5-tetrazolyl)phenyl]porphyrinato} manganese(III) chloride as the metalloligand. The MOF adopts the rare scu topology with one-dimensional square nanotube-like channels of about 20 Å. UTSA-57a exhibits permanent porosity and displays moderately high performance for C2H2/CH4 separation at room temperature.

  19. Hydrophobic conjugated microporous polymers for sorption of human serum albumin

    NASA Astrophysics Data System (ADS)

    Zheng, Chunli; Du, Miaomiao; Feng, Shanshan; Sun, Hanxue; Li, An; He, Chi; Zhang, TianCheng; Wang, Qiaorui; Wei, Wei

    2016-02-01

    This paper investigated the sorption of human serum albumin (HSA) from water by three kinds of conjugated microporous polymers (CMPs) with surface hydrophobicity and intrinsic porosity. It was found that the three CMPs captured HSA with fast sorption kinetics and good working capacity. Equilibrium was obtained at 80 min for all the tests, and the maximum sorption quantity (qm) ranged from 0.07 to 0.14 mg/mg. With the increase in the particle external surface area of the CMPs, a greater extent of HSA sorption was achieved. Moreover, promoting the dispersion of CMPs in HSA aqueous solution was also beneficial to the extraction. Attenuated Total Reflection Fourier Transform Infrared spectroscopy verified the interactions between the CMPs and the Nsbnd H, Cdbnd O, and Csbnd N groups of HSA. This paper might provide fundamental guidance for the practical application of CMPs to proteins separation and recovery.

  20. Synthetic Zeolites and Other Microporous Oxide Molecular Sieves

    NASA Astrophysics Data System (ADS)

    Sherman, John D.

    1999-03-01

    Use of synthetic zeolites and other microporous oxides since 1950 has improved insulated windows, automobile air-conditioning, refrigerators, air brakes on trucks, laundry detergents, etc. Their large internal pore volumes, molecular-size pores, regularity of crystal structures, and the diverse framework chemical compositions allow "tailoring" of structure and properties. Thus, highly active and selective catalysts as well as adsorbents and ion exchangers with high capacities and selectivities were developed. In the petroleum refining and petrochemical industries, zeolites have made possible cheaper and lead-free gasoline, higher performance and lower-cost synthetic fibers and plastics, and many improvements in process efficiency and quality and in performance. Zeolites also help protect the environment by improving energy efficiency, reducing automobile exhaust and other emissions, cleaning up hazardous wastes (including the Three Mile Island nuclear power plant and other radioactive wastes), and, as specially tailored desiccants, facilitating the substitution of new refrigerants for the ozone-depleting chlorofluorocarbons banned by the Montreal Protocol.