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Sample records for microporous silica prepared

  1. Microporous silica prepared by organic templating: Relationship between the molecular template and pore structure

    SciTech Connect

    Lu, Y.; Brinker, C.J. |; Cao, G.; Kale, R.P.; Prabakar, S.; Lopez, G.P.

    1999-05-01

    Microporous silica materials with a controlled pore size and a narrow pore size distribution have been prepared by sol-gel processing using an organic-templating approach. Microporous networks were formed by pyrolytic removal of organic ligands (methacryloxypropyl groups) from organic/inorganic hybrid materials synthesized by copolymerization of 3-methacryloxypropylsilane (MPS) and tetraethoxysilane (TEOS). Molecular simulations and experimental measurements were conducted to examine the relationship between the microstructural characteristics of the porous silica (e.g., pore size, total pore volume, and pore connectivity) and the size and amount of organic template ligands added. Adsorption measurements suggest that the final porosity of the microporous silica is due to both primary pores (those present in the hybrid material prior to pyrolysis) and secondary pores (those created by pyrolytic removal of organic templates). Primary pores were inaccessible to N{sub 2} at 77 K but accessible to CO{sub 2} at 195 K; secondary pores were accessible to both N{sub 2} (at 77 K) and CO{sub 2} (at 195 K) in adsorption measurements. Primary porosity decreases with the amount of organic ligands added because of the enhanced densification of MPS/TEOS hybrid materials as the mole fraction of trifunctional MPS moieties increases. Pore volumes measured by nitrogen adsorption experiments at 77 K suggest that the secondary (template-derived) porosity exhibits a percolation behavior as the template concentration is increased. Gas permeation experiments indicate that the secondary pores are approximately 5 {angstrom} in diameter, consistent with predictions based on molecular simulations.

  2. Microstructure investigation on micropore formation in microporous silica materials prepared via a catalytic sol-gel process by small angle X-ray scattering.

    PubMed

    Shimizu, Wataru; Hokka, Junsuke; Sato, Takaaki; Usami, Hisanao; Murakami, Yasushi

    2011-08-01

    The so-called sol-gel technique has been shown to be a template-free, efficient way to create functional porous silica materials having uniform micropores. This appears to be closely linked with a postulation that the formation of weakly branched polymer-like aggregates in a precursor solution is a key to the uniform micropore generation. However, how such a polymer-like structure can precisely be controlled, and further, how the generated low-fractal dimension solution structure is imprinted on the solid silica materials still remain elusive. Here we present fabrication of microporous silica from tetramethyl orthosilicate (TMOS) using a recently developed catalytic sol-gel process based on a nonionic hydroxyacetone (HA) catalyst. Small angle X-ray scattering (SAXS), nitrogen adsorption porosimetry, and transmission electron microscope (TEM) allowed us to observe the whole structural evolution, ranging from polymer-like aggregates in the precursor solution to agglomeration with heat treatment and microporous morphology of silica powders after drying and hydrolysis. Using the HA catalyst with short chain monohydric alcohols (methanol or ethanol) in the precursor solution, polymer-like aggregates having microscopic correlation length (or mesh-size) < 2 nm and low fractal dimensions ∼2, which is identical to that of an ideal coil polymer, can selectively be synthesized, yielding the uniform micropores with diameters <2 nm in the solid materials. In contrast, the absence of HA or substitution of 1-propanol led to considerably different scattering behavior reflecting the particle-like aggregate formation in the precursor solution, which resulted in the formation of mesopores (diameter >2 nm) in the solid product due to apertures between the particle-like aggregates. The data demonstrate that the extremely fine porous silica architecture comes essentially from a gaussian polymer-like nature of the silica aggregates in the precursor having the microscopic mesh-size and

  3. Controlling the porosity of microporous silica by sol-gel processing using an organic template approach

    SciTech Connect

    Lu, Y.; Cao, G.Z.; Kale, R.P.; Delattre, L.; Lopez, G.P.; Brinker, C.J. |

    1996-12-31

    The authors use an organic template approach to prepare microporous silica with controlled pore size and narrow pore size distributions. This was accomplished by fabricating relatively dense hybrid silica matrices incorporating organic template ligands by sol-gel synthesis and then removing the organic ligands to create a microporous silica network. Comparison of computer simulation results and experimental data indicated that using this fugitive template approach, pore volume can be controlled by the amount of organic template added to the system, and pore size can be controlled by the size of the organic ligands.

  4. Controlled release of chlorhexidine from amorphous microporous silica.

    PubMed

    Verraedt, E; Pendela, M; Adams, E; Hoogmartens, J; Martens, J A

    2010-02-25

    A new system for the controlled release of the antiseptic chlorhexidine is presented. Amorphous microporous silica (AMS) excipient material was synthesized via an acid catalyzed sol-gel method and shaped as powder or coating. Chlorhexidine diacetate was introduced into the pores of the AMS silica via the incipient wetness impregnation method. This silica reservoir maintained a slow release of chlorhexidine over more than 7days. Chlorhexidine release was controlled by configurational diffusion in the AMS pores having free diameters of less than 1nm. The release of chlorhexidine was fine tuned by adapting particle size and pore diameter. Controlled release of chlorhexidine from an AMS coating on silicon wafer was demonstrated. PMID:19804804

  5. Tadalafil inclusion in microporous silica as effective dissolution enhancer: optimization of loading procedure and molecular state characterization.

    PubMed

    Mehanna, Mohammed M; Motawaa, Adel M; Samaha, Magda W

    2011-05-01

    Tadalafil is an efficient drug used to treat erectile dysfunction characterized by poor water solubility, which has a negative influence on its bioavailability. Utilization of microporous silica represents an effective and facile technology to increase the dissolution rate of poorly soluble drugs. Our strategy involved directly introducing tadalafil as guest molecule into microporous silica as host material by incipient wetness impregnation method. To optimize tadalafil inclusion, response surface methodology (RSM) using 3(3) factorial design was utilized. Furthermore, to investigate the molecular state of tadalafil, Fourier-transform infrared spectroscopy, differential scanning calorimetery, thermal gravimetrical analysis, nitrogen adsorption, and powder X-ray diffraction (PXRD) were carried out. The results obtained pointed out that the quantity of microporous silica was the predominant factor that increased the loading efficiency. For the optimized formula, the loading efficiency was 42.50 wt %. Adsorption-desorption experiments indicated that tadalafil has been introduced into the micropores. Powder XRD and differential scanning calorimetry analyses revealed that tadalafil is arranged in amorphous form. In addition, the dissolution rate of tadalafil from the microporous silica was faster than that of free drug. Amorphous tadalafil occluded in microporous silica did not crystallize over 3 months. These findings contributed in opening a new strategy concerning the utilization of porous silica for the dissolution rate enhancement. PMID:21374616

  6. A new microporous polymorph of silica isomorphous to zeolite MCM-22

    SciTech Connect

    Camblor, M.A.; Corell, C.; Corma, A.

    1996-10-01

    A zeolite-like silica polymorph was prepared and given the descriptor, ITQ-1. The synthesis of this silica and high Si/Al aluminosilicates is described. The structure of the these materials was studied by X-ray diffraction and NMR.

  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+. PMID:27612695

  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. Determination of phenolic compounds in air by using cyclodextrin-silica hybrid microporous composite samplers.

    PubMed

    Mauri-Aucejo, Adela R; Ponce-Català, Patricia; Belenguer-Sapiña, Carolina; Amorós, Pedro

    2015-03-01

    An analytical method for the determination of phenolic compounds in air samples based on the use of cyclodextrin-silica hybrid microporous composite samplers is proposed. The method allows the determination of phenol, guaiacol, cresol isomers, eugenol, 4-ethylphenol and 4-ethylguaiacol in workplaces according to the Norm UNE-EN 1076:2009 for active sampling. Therefore, the proposed method offers an alternative for the assessment of the occupational exposure to phenol and cresol isomers. The detection limits of the proposed method are lower than those for the NIOSH Method 2546. Storage time of samples almost reaches 44 days. Recovery values for phenol, guaiacol, o-cresol, m-cresol, p-cresol, 4-ethylguaiacol, eugenol and 4-ethylphenol are 109%, 99%, 102%, 94%, 94%, 91%, 95% and 102%, respectively with a coefficient of variation below 6%. The method has been applied to the assessment of exposure in different areas of a farm and regarding the quantification of these compounds in the vapors generated by burning incense sticks and an essential oil marketed as air fresheners. The acquired results are comparable with those provided from a reference method for a 95% of confidence level. The possible use of these samplers for the sampling of other toxic compounds such as phthalates is evaluated by qualitative analysis of extracts from incense sticks and essential oil samples.

  10. An activated microporous carbon prepared from phenol-melamine-formaldehyde resin for lithium ion battery anode

    SciTech Connect

    Zhu, Yinhai; Xiang, Xiaoxia; Liu, Enhui; Wu, Yuhu; Xie, Hui; Wu, Zhilian; Tian, Yingying

    2012-08-15

    Highlights: ► Microporous carbon was prepared by chemical activation of phenol-melamine-formaldehyde resin. ► Activation leads to high surface area, well-developed micropores. ► Micropores lead to strong intercalation between carbon and lithium ion. ► Large surface area promotes to improve the lithium storage capacity. -- Abstract: Microporous carbon anode materials were prepared from phenol-melamine-formaldehyde resin by ZnCl{sub 2} and KOH activation. The physicochemical properties of the obtained carbon materials were characterized by scanning electron microscope, X-ray diffraction, Brunauer–Emmett–Teller, and elemental analysis. The electrochemical properties of the microporous carbon as anode materials in lithium ion secondary batteries were evaluated. At a current density of 100 mA g{sup −1}, the carbon without activation shows a first discharge capacity of 515 mAh g{sup −1}. After activation, the capacity improved obviously. The first discharge capacity of the carbon prepared by ZnCl{sub 2} and KOH activation was 1010 and 2085 mAh g{sup −1}, respectively. The reversible capacity of the carbon prepared by KOH activation was still as high as 717 mAh g{sup −1} after 20 cycles, which was much better than that activated by ZnCl{sub 2}. These results demonstrated that it may be a promising candidate as an anode material for lithium ion secondary batteries.

  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)

    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.

  13. 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.

  14. Effect of embedded metal compound on porosity of silica colloids prepared by spray reaction of silicon tetrachloride.

    PubMed

    Isobe, Hiroshi; Hattori, Yoshiyuki; Hayano, Tomoe; Kanoh, Hirofumi; Yamamoto, Kohzoh; Kaneko, Katsumi

    2006-03-15

    Attempts to prepare macroporous silica particles and metal-compound-nanoparticle-embedded silica microspheres were carried out using reactions between silicon tetrachloride and ultrasonic generating microdroplets including metal (Na, K, Al, Ni, Ti, Pt) compounds. Samples were collected by dry and wet processes. In the case of using nickel and aluminum compounds, acid-treated samples were also prepared. The obtained samples were characterized by scanning electron microscopy, X-ray fluorescence spectroscopy, powder X-ray diffractometry, mercury porosimetry, and the nitrogen adsorption method. The macroporous silica particles were prepared by removing the salt crystals, such as NaCl and KCl, formed in the silica frame. For acid-resistant metals, platinum- and titanium-compound nanoparticles are easily embedded in silica microspheres using these metal-compound solutions. For acid-soluble metals, aluminum- and nickel-compound-nanoparticle-embedded silicas were prepared by applying neutralization of the collection water. Micropores and mesopores were produced in wet-process samples. Acid treatment induced the increase of micropore volumes. PMID:16246356

  15. 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%. PMID:19569094

  16. Controlled release of chlorhexidine antiseptic from microporous amorphous silica applied in open porosity of an implant surface.

    PubMed

    Verraedt, Els; Braem, Annabel; Chaudhari, Amol; Thevissen, Karin; Adams, Erwin; Van Mellaert, Lieve; Cammue, Bruno P A; Duyck, Joke; Anné, Jozef; Vleugels, Jef; Martens, Johan A

    2011-10-31

    Amorphous microporous silica (AMS) serving as a reservoir for controlled release of a bioactive agent was applied in the open porosity of a titanium coating on a Ti-6Al-4V metal substrate. The pores of the AMS emptied by calcination were loaded with chlorhexidine diacetate (CHX) via incipient wetness impregnation with CHX solution, followed by solvent evaporation. Using this CHX loaded AMS system on titanium substrate sustained release of CHX into physiological medium was obtained over a 10 day-period. CHX released from the AMS coating was demonstrated to be effective in killing planktonic cultures of the human pathogens Candida albicans and Staphylococcus epidermidis. This surface modification of titanium bodies with AMS controlled release functionality for a bioactive compound potentially can be applied on dental and orthopaedic implants to abate implant-associated microbial infection. PMID:21798323

  17. 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  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. 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.

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

    DOE PAGESBeta

    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. Immobilization of Cross-Linked Phenylalanine Ammonia Lyase Aggregates in Microporous Silica Gel

    PubMed Central

    Cui, Jian Dong; Li, Lian Lian; Bian, Hong Jie

    2013-01-01

    A separable and highly-stable enzyme system was developed by adsorption of phenylalanine ammonia lyase (PAL) from Rhodotorula glutinis in amino-functionalized macroporous silica gel and subsequent enzyme crosslinking. This resulted in the formation of cross-linked enzyme aggregates (PAL-CLEAs) into macroporous silica gel (MSG-CLEAs). The effect of adsorptive conditions, type of aggregating agent, its concentration as well as that of cross-linking agent was studied. MSG-CLEAs production was most effective using ammonium sulfate (40%-saturation), followed by cross-linking for 1 h with 1.5% (v/v) glutaraldehyde. The resulting MSG-CLEAs extended the optimal temperature and pH range compared to free PAL and PAL-CLEAs. Moreover, MSG-CLEAs exhibited the excellent stability of the enzyme against various deactivating conditions such as temperature and denaturants, and showed higher storage stability compared to the free PAL and the conventional PAL-CLEAs. Such as, after 6 h incubation at 60°C, the MSG-CLEAs still retained more than 47% of the initial activity whereas PAL-CLEAs only retained 7% of the initial activity. Especially, the MSG-CLEAs exhibited good reusability due to its suitable size and active properties. These results indicated that PAL-CLEAs on MSG might be used as a feasible and efficient solution for improving properties of immobilized enzyme in industrial application. PMID:24260425

  3. 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.

  4. Preparation and characterization of SiO{sub 2}/TiO{sub 2} composite microspheres with microporous SiO{sub 2} core/mesoporous TiO{sub 2} shell

    SciTech Connect

    Zhao Li; Yu Jiaguo . E-mail: jiaguoyu@yahoo.com; Cheng Bei

    2005-06-15

    SiO{sub 2}/TiO{sub 2} composite microspheres with microporous SiO{sub 2} core/mesoporous TiO{sub 2} shell structures were prepared by hydrolysis of titanium tetrabutylorthotitanate (TTBT) in the presence of microporous silica microspheres using hydroxypropyl cellulose (HPC) as a surface esterification agent and porous template, and then dried and calcined at different temperatures. The as-prepared products were characterized with differential thermal analysis and thermogravimetric (DTA/TG), scanning electron microscopy (SEM), X-ray diffraction (XRD), nitrogen adsorption. The results showed that composite particles were about 1.8{mu}m in diameter, and had a spherical morphology and a narrow size distribution. Uniform mesoporous titania coatings on the surfaces of microporous silica microspheres could be obtained by adjusting the HPC concentration to an optimal concentration of about 3.2mmolL{sup -1}. The anatase and rutile phase in the SiO{sub 2}/TiO{sub 2} composite microspheres began to form at 700 and 900 deg. C, respectively. At 700 deg. C, the specific surface area and pore volume of the SiO{sub 2}/TiO{sub 2} composite microspheres were 552 and 0.652mLg{sup -1}, respectively. However, at 900 deg. C, the specific surface area and pore volume significantly decreased due to the phase transformation from anatase to rutile.

  5. 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.

  6. Preparation and Characterization of Silica-Enoxil Nanobiocomposites

    NASA Astrophysics Data System (ADS)

    Kuzema, Pavlo O.; Laguta, Iryna V.; Stavinskaya, Oksana N.; Kazakova, Olga A.; Borysenko, Mykola V.; Lupaşcu, Tudor

    2016-02-01

    Silica-Enoxil nanobiocomposites with 13 %w of Enoxil were prepared either by mechanical mixing of corresponding powders or by sorptive modification of fumed silica powder with aqueous Enoxil solution under fluidized bed conditions. The interaction of fumed silica with Enoxil and the properties of silica-Enoxil composites have been investigated using IR spectroscopy, thermogravimetric analysis, and quantum chemistry methods, as well as by means of water absorption, Enoxil desorption, and 2,2-diphenyl-1-picrylhydrazyl (DPPH) test. It has been shown that the main biomolecules of Enoxil composition interact with silica involving their hydroxyl groups and surface silanol groups. The water absorption of silica-Enoxil nanocomposites was found to be less than that for the individual components. The Enoxil biomolecules are readily and completely desorbed from silica surface into water, and the antioxidant activity of desorbed Enoxil is practically the same as that for the just dissolved one.

  7. Preparation of uniform-sized agarose beads by microporous membrane emulsification technique.

    PubMed

    Zhou, Qing-Zhu; Wang, Lian-Yan; Ma, Guang-Hui; Su, Zhi-Guo

    2007-07-01

    Uniform-sized agarose beads were prepared by membrane emulsification technique in this study. Agarose was dissolved in boiling water (containing 0.9% sodium chloride) and used as water phase. A mixture of liquid paraffin and petroleum ether containing 4 wt% of hexaglycerin penta ester (PO-500) emulsifier was used as oil phase. At 55 degrees C, the water phase permeated through uniform pores of microporous membrane into the oil phase by a pressure of nitrogen gas to form uniform W/O emulsion. Then the emulsion was cooled down to room temperature under gentle agitation to form gel beads. The effect of oil phase, emulsifier, especially temperature on the uniformity of the beads were investigated and interpreted from interfacial tension between water phase and oil phase. Under optimized condition, the coefficient variation (C.V.) showing the size distribution of the beads was under 15%. This was the first report to prepare uniform agarose beads by membrane emulsification, and to investigate the effect of temperature on the size distribution of the droplets and beads. The beads with different size can be prepared by using membranes with different pore size, and the result showed that there was a linear relationship between the average diameter of beads and pore size of the membranes; beads with diameter from 15 to 60 microm were able to obtain in this study.

  8. Facile preparation and ultra-microporous structure of melamine-resorcinol-formaldehyde polymeric microspheres.

    PubMed

    Zhou, Huanhuan; Xu, Sheng; Su, Haiping; Wang, Mei; Qiao, Wenming; Ling, Licheng; Long, Donghui

    2013-05-01

    A facile hydrothermal method was developed to synthesize nitrogen-rich phenolic microspheres with a tunable ultra-microporous structure for CO(2) adsorption. The results highlighted that chemical composition and ultramicroporous size, much more than surface area, dictated the CO(2) uptake in a microporous organic polymer.

  9. 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…

  10. 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.

  11. 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

  12. 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.

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

    PubMed

    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 f 2 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

  14. 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

  15. 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.

  16. Janus Silica Hollow Spheres Prepared via Interfacial Biosilicification.

    PubMed

    Sheng, Li; Chen, Hong; Fu, Wenxin; Li, Zhibo

    2015-11-10

    A poly(ethylene glycol)-b-poly(L-lysine)-b-poly(styrene) (PEG-PLL-PS) triblock copolymer, which contains a cationic PLL block as the middle block, is synthesized via a combination of ring-opening polymerization (ROP) and atom-transfer radical polymerization (ATRP). The PEG-PLL-PS (ELS) triblock is employed as a macromolecular surfactant to form a stable oil-in-water (O/W) emulsion, which is subsequently used as the template to prepare Janus silica hollow spheres (JHS) via a one-pot biosilicification reaction. For the emulsion template, the middle PLL block assembles at the O/W interface and directs the biomimetic silica synthesis in the presence of phosphate buffer and silicic acid precursors. This biosilicification process takes place only in the intermediate layer between water and the organic interior phase, leading to the formation of silica JHSs with hydrophobic PS chains tethered to the inner surface and PEG attached to the outer surface. The three-layer JHSs, namely, PEG/silica-polylysine/PS composites, were verified by electron microscopy. Upon further breaking these JHSs into species, polymer-grafted Janus silica nanoplates (JPLs) can be obtained. Our studies provide an efficient one-step method for preparing hybrid silica Janus structures within minutes.

  17. 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.

  18. Bio-electrochemical characterization of air-cathode microbial fuel cells with microporous polyethylene/silica membrane as separator.

    PubMed

    Kircheva, Nina; Outin, Jonathan; Perrier, Gérard; Ramousse, Julien; Merlin, Gérard; Lyautey, Emilie

    2015-12-01

    The aim of this work was to study the behavior over time of a separator made of a low-cost and non-selective microporous polyethylene membrane (RhinoHide®) in an air-cathode microbial fuel cell with a reticulated vitreous carbon foam bioanode. Performances of the microporous polyethylene membrane (RhinoHide®) were compared with Nafion®-117 as a cationic exchange membrane. A non-parametric test (Mann-Whitney) done on the different sets of coulombic or energy efficiency data showed no significant difference between the two types of tested membrane (p<0.05). Volumetric power densities were ranging from 30 to 90 W·m(-3) of RVC foam for both membranes. Similar amounts of biomass were observed on both sides of the polyethylene membrane illustrating bacterial permeability of this type of separator. A monospecific denitrifying population on cathodic side of RhinoHide® membrane has been identified. Electrochemical impedance spectroscopy (EIS) was used at OCV conditions to characterize electrochemical behavior of MFCs by equivalent electrical circuit fitted on both Nyquist and Bode plots. Resistances and pseudo-capacitances from EIS analyses do not differ in such a way that the nature of the membrane could be considered as responsible.

  19. 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.

  20. 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. PMID:22905559

  1. 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.

  2. Preparation of a unique microporous structure via two step phase separation in the course of drying a ternary polymer solution.

    PubMed

    Kim, Jae-Kyung; Taki, Kentaro; Ohshima, Masahiro

    2007-11-20

    A unique porous polymeric film was prepared by drying a ternary polymer solution: a polystyrene (PS), polyethylene glycol (PEG), and toluene solution. Highly ordered micropores, ranging from 5 to 12 mum in diameter, were formed on the film surface, and the rim of each micropore was surrounded by a ring of PEG. The effects of the weight ratio of the polymer blend and molecular weight of the polymer (PEG) on the porous structure were investigated. Based on in situ visual observation and light scattering measurements, the formation mechanism of the porous structure was speculated to be a two step phase separation: the phase separation into PEG-rich and PEG-poor (i.e., PS-rich) phases occurred first at the surface area of the ternary solutions, where polymers were condensed due to solvent evaporation. The PEG-rich phase became droplets and had an ordered structure on the surface. The PEG-poor phase became a matrix where PS and solvent coexisted as a single phase solution. Secondary phase separation then followed in the PEG droplets, which was induced by further solvent evaporation, and formed into solvent-rich and PEG-rich domains within the droplets. Solvent evaporation and secondary phase separation created a cavity structure in each PEG droplet structured on the film surface.

  3. 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.

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

    PubMed

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

    2014-07-02

    Two-dimensional (2D) porous carbon AC-SPN-3 possessing of amazing high micropore volume ratio of 83% and large surface area of about 1069 m(2) 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.

  5. 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

  6. 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

  7. Method for preparing high activity silica supported hydrotreating catalysts

    SciTech Connect

    Thompson, M.S.

    1986-03-04

    A method is described for preparing a silica supported hydrotreating catalyst containing from about 10-25%w molybdenum and from about 1-5%w nickel and/or cobalt as hydrogenation metals. The method consists of: (a) reacting a mixture of MoCl/sub 5/ and a compound selected from the group consisting of Ni(H/sub 2/O)/sub 6/Cl/sub 2/, Co(H/sub 2/O)/sub 6/Cl/sub 2/ and mixutres in amounts to provide a desired catalytic metals concentration of the support in the presence of a solubilizing amount of acetonitrile; (b) heating the mixture to between about 25/sup 0/ and 80/sup 0/C until most of the metal compounds have reacted and/or dissolved; (c) removing any undissolved solids from the solution; (d) impregnating the dried silica support with the hydrogenation metals-containing solution in one or more steps; and (e) drying the impregnated silica support at elevated temperature.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. Preparation of monodisperse porous silica particles using poly(glycidyl methacrylate) microspheres as a template.

    PubMed

    Grama, S; Horák, D

    2015-01-01

    Monodisperse macroporous poly(glycidyl methacrylate) (PGMA) microspheres were used as a template for preparing porous silica particles. The starting polymer microspheres that were 9.3 microm in size were synthesized by multistep swelling polymerization using a modified Ugelstad technique. Subsequently, silica (SiO2) was deposited on the surface and inside the PGMA microspheres to produce poly(glycidyl methacrylate)-silica hybrid particles (PGMA-SiO2). Upon calcination of the PGMA-SiO2 microspheres, porous silica particles were formed. The morphology, particle size, polydispersity and inner structure of the silica microspheres were investigated by scanning and transmission electron microscopy. Thermogravimetric analysis and dynamic adsorption of nitrogen determined the amount of silica formed and its specific surface area. Compared with the starting PGMA microspheres, the size of the porous silica particles decreased by up to 30%. These porous silica microspheres are promising for chromatography and biomedical applications. PMID:26447591

  14. Preparation of monodisperse porous silica particles using poly(glycidyl methacrylate) microspheres as a template.

    PubMed

    Grama, S; Horák, D

    2015-01-01

    Monodisperse macroporous poly(glycidyl methacrylate) (PGMA) microspheres were used as a template for preparing porous silica particles. The starting polymer microspheres that were 9.3 microm in size were synthesized by multistep swelling polymerization using a modified Ugelstad technique. Subsequently, silica (SiO2) was deposited on the surface and inside the PGMA microspheres to produce poly(glycidyl methacrylate)-silica hybrid particles (PGMA-SiO2). Upon calcination of the PGMA-SiO2 microspheres, porous silica particles were formed. The morphology, particle size, polydispersity and inner structure of the silica microspheres were investigated by scanning and transmission electron microscopy. Thermogravimetric analysis and dynamic adsorption of nitrogen determined the amount of silica formed and its specific surface area. Compared with the starting PGMA microspheres, the size of the porous silica particles decreased by up to 30%. These porous silica microspheres are promising for chromatography and biomedical applications.

  15. 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.

  16. 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.

  17. Preparation of novel silica-coated alginate gel beads for efficient encapsulation of yeast alcohol dehydrogenase.

    PubMed

    Xu, Song-Wei; Lu, Yang; Li, Jian; Zhang, Yu-Fei; Jiang, Zhong-Yi

    2007-01-01

    Biomimetic formation has undoubtedly inspired the preparation of novel organic-inorganic hybrid composites. In this study, silica-coated alginate gel beads were prepared by coating the surface of alginate gel beads with silica film derived from tetramethoxysilane (TMOS). The composition and structure of the silica film were characterized by FT-IR and SEM equipped with EDX. The swelling behavior of silica-coated alginate gel beads was studied to be more stable against swelling than that of alginate gel beads. The results showed that silica-coated alginate gel beads exhibited appropriate diffusion property. The effective diffusion coefficient (D(e)) of NADH in silica-coated alginate beads was 1.76 x 10(-10) m2/s, while the effective diffusion coefficient in alginate beads was 1.84 x 10(-10) m2/s. The model enzyme yeast alcohol dehydrogenase (YADH) was encapsulated in silica-coated alginate and pure alginate beads, respectively. Enzyme leakage of YADH in alginate gel beads was determined to be 32%, while the enzyme leakage in silica-coated alginate gel beads was as low as 11%. Furthermore, the relative activity of YADH in alginate gel beads decreased almost to zero after 10 recycles, while the relative activity of YADH in silica-coated alginate gel beads was 81.3%. The recycling stability of YADH in silica-coated alginate gel beads was found to be increased significantly mainly due to the effective inhibition of enzyme leakage by compact silica film.

  18. 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.

  19. Preparation of concentrated colloids of gold core-silica shell nanoparticles for biomedical applications.

    PubMed

    Park, Yeon-Su

    2012-01-01

    Encapsulation of gold nanoparticles within a silica shell is highly beneficial to the preparation of highly concentrated gold nanoparticles that can strongly absorb X-ray and hence be used as an X-ray contrast agent. This chapter describes a method for preparing highly concentrated colloidal gold nanoparticles suitable for an X-ray contrast agent application. It describes specific details of procedures for preparing spherical gold nanoparticles, forming thin silica shell on each gold nanoparticle, and enriching the silica-encapsulated gold nanoparticles.

  20. Facile preparation of silica-supported Ti catalysts effective for the epoxidation of cyclooctene using Ti-bridged silsesquioxanes.

    PubMed

    Wada, Kenji; Sakugawa, Shuko; Inoue, Masashi

    2012-08-18

    When used as additives, silicas strongly promoted the epoxidation of cyclooctene by (t)BuOOH in the presence of Ti-silsesquioxane (Ti-POSS), where Ti species were found to be bound to the silica surface. Based on this observation, highly-active silica-supported Ti catalysts were prepared by the thermal treatment of mixtures of Ti-POSS and silica.

  1. Hollow Microporous Organic Capsules

    PubMed Central

    Li, Buyi; Yang, Xinjia; Xia, Lingling; Majeed, Muhammad Irfan; Tan, Bien

    2013-01-01

    Fabrication of hollow microporous organic capsules (HMOCs) could be very useful because of their hollow and porous morphology, which combines the advantages of both microporous organic polymers and non-porous nanocapsules. They can be used as storage materials or reaction chambers while supplying the necessary path for the design of controlled uptake/release systems. Herein, the synthesis of HMOCs with high surface area through facile emulsion polymerization and hypercrosslinking reactions, is described. Due to their tailored porous structure, these capsules possessed high drug loading efficiency, zero-order drug release kinetics and are also demonstrated to be used as nanoscale reactors for the prepareation of nanoparticles (NPs) without any external stabilizer. Moreover, owing to their intrinsic biocompatibility and fluorescence, these capsules exhibit promising prospect for biomedical applications. PMID:23820511

  2. Preparation and characterization of silica nanoparticulate polyacrylonitrile composite and porous nanofibers

    NASA Astrophysics Data System (ADS)

    Ji, Liwen; Saquing, Carl; Khan, Saad A.; Zhang, Xiangwu

    2008-02-01

    In this study, polyacrylonitrile (PAN) composite nanofibers containing different amounts of silica nanoparticulates have been obtained via electrospinning. The surface morphology, thermal properties and crystal structure of PAN/silica nanofibers are characterized using attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, wide-angle x-ray diffraction (WAXD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and differential scanning calorimetry (DSC). The results indicate that the addition of silica nanoparticulates affects the structure and properties of the nanofibers. In addition to PAN/silica composite nanofibers, porous PAN nanofibers have been prepared by selective removal of the silica component from PAN/silica composite nanofibers using hydrofluoric (HF) acid. ATR-FTIR and thermal gravimetric analysis (TGA) experiments validate the removal of silica nanoparticulates by HF acid, whereas SEM and TEM results reveal that the porous nanofibers obtained from composite fibers with higher silica contents exhibited more nonuniform surface morphology. The Brunauer-Emmett-Teller (BET) surface area of porous PAN nanofibers made from PAN/silica (5 wt%) composite precursors is higher than that of pure nonporous PAN nanofibers.

  3. Preparation of silica sphere with porous structure in supercritical carbon dioxide.

    PubMed

    Chatterjee, Maya; Chatterjee, Abhijit; Ikushima, Yutaka; Kawanami, Hajime; Ishizaka, Takayuki; Sato, Masahiro; Suzuki, Toshishige; Yokoyama, Toshirou

    2010-08-01

    Silica sphere with porous structure has been synthesized in supercritical carbon dioxide. The structure originates from a delicate CO(2) trapping phenomenon intended for void formation in the inorganic framework. Silicate polymerization and subsequent removal of CO(2) by depressurization leaves the porous architecture. The key factor to obtain stable porous spherical structure was CO(2) pressure. Different characterization techniques such as X-ray diffraction, scanning and transmission electron microscopy and N(2) adsorption-desorption isotherm were used to determine the framework structure, morphology and porosity of the material. Microscopic visualization of calcined material suggested that the spherical structure was consisted of macroporous windows of diameter approximately 100 nm and the space between macropores presents a wormhole like mesoporous/microporous structure. The pore diameter of the mesoporous structure has been calculated as approximately 3 nm. X-ray diffraction and N(2) adsorption isotherm analysis confirmed the presence of micropores and also the macropores. In addition, the resulting material possess high thermal and hydrothermal stability associated with fully SiO(4) cross-linking. The spherical structure with different types of porosity was successfully obtained without using any molding agent.

  4. Preparation and Characterization of Silica/Polyamide-imide Nanocomposite Thin Films

    NASA Astrophysics Data System (ADS)

    Ma, Xiaokun; Lee, Nam-Hee; Oh, Hyo-Jin; Hwang, Jong-Sun; Kim, Sun-Jae

    2010-11-01

    The functional silica/polyamide-imide composite films were prepared via simple ultrasonic blending, after the silica nanoparticles were modified by cationic surfactant—cetyltrimethyl ammonium bromide (CTAB). The composite films were characterized by scanning electron microscope (SEM), thermo gravimetric analysis (TGA) and thermomechanical analysis (TMA). CTAB-modified silica nanoparticles were well dispersed in the polyamide-imide matrix, and the amount of silica nanoparticles to PAI was investigated to be from 2 to 10 wt%. Especially, the coefficients of thermal expansion (CET) continuously decreased with the amount of silica particles increasing. The high thermal stability and low coefficient of thermal expansion showed that the nanocomposite films can be widely used in the enamel wire industry.

  5. Acidic and Hydrophobic Microporous Clays Pillared with Mixed Metal Oxide Nano-Sols

    NASA Astrophysics Data System (ADS)

    Han, Yang-Su; Yamanaka, Shoji; Choy, Jin-Ho

    1999-04-01

    Silica-metal oxide sol pillared clays have been synthesized from montmorillonite by exchanging interlamellar (Na+) ions with silica sol particles modified with polyhydroxy metal cations. Though the silica sol particle itself is negatively charged in the pH range used in present experiment, 1.5-2.7, the ion-exchange-type intercalation of the silica sol into montmorillonite was realized by modifying the surface charge of the sol particles from negative to positive. The positively charged silica sol particles were prepared by titrating metal aqueous solutions (Mz+=Fe3+, Al3+, Cr3+, and Zr4+) with NaOH in the presence of silica sol particles, which were easily intercalated inbetween the silicate layers of clay. On pillaring of oxide sols and subsequent calcining at 400°C, new porous materials were obtained with high BET surface areas of 320-720 m2/g, pore volumes of 0.24-0.50 ml/g, and basal spacings in the range 40-60 Å. Furthermore, their thermal stability could be remarkably improved up to 700°C. According to the adsorption measurements of nitrogen and solvent vapors, the micropores in the samples of size 9-13 Å dominate due to the multilayer stacking of interlayer sol particles inbetween silicate layers. Temperature-programmed desorption (TPD) spectra of ammonia revealed that the microporous samples are weakly acidic, but with different strengths, depending on the doped metal species.

  6. 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.

  7. Preparation, purification, and characterization of aminopropyl-functionalized silica sol.

    PubMed

    Pálmai, Marcell; Nagy, Lívia Naszályi; Mihály, Judith; Varga, Zoltán; Tárkányi, Gábor; Mizsei, Réka; Szigyártó, Imola Csilla; Kiss, Teréz; Kremmer, Tibor; Bóta, Attila

    2013-01-15

    A new, simple, and "green" method was developed for the surface modification of 20 nm diameter Stöber silica particles with 3-aminopropyl(diethoxy)methylsilane in ethanol. The bulk polycondensation of the reagent was inhibited and the stability of the sol preserved by adding a small amount of glacial acetic acid after appropriate reaction time. Centrifugation, ultrafiltration, and dialysis were compared in order to choose a convenient purification technique that allows the separation of unreacted silylating agent from the nanoparticles without destabilizing the sol. The exchange of the solvent to acidic water during the purification yielded a stable colloid, as well. Structural and morphological analysis of the obtained aminopropyl silica was performed using transmission electron microscopy (TEM), dynamic light scattering (DLS) and zeta potential measurements, Fourier-transform infrared (FTIR), (13)C and (29)Si MAS nuclear magnetic resonance (NMR) spectroscopies, as well as small angle X-ray scattering (SAXS). Our investigations revealed that the silica nanoparticle surfaces were partially covered with aminopropyl groups, and multilayer adsorption followed by polycondensation of the silylating reagent was successfully avoided. The resulting stable aminopropyl silica sol (ethanolic or aqueous) is suitable for biomedical uses due to its purity. PMID:23068887

  8. Preparation of Nanowire Silica Inside Self-Assembled Sodium Bis(2-ethylhexyl) Sulfosuccinate (AOT) Gels.

    PubMed

    Lai, Wei-Chi; Hong, Li-Tzuen

    2016-09-22

    In conventional sol-gel methods, gel formation occurs due to aggregation of particles into irregular shapes of larger size. In this study, we conducted hydrolysis-condensation reactions of tetraethyl orthosilicate (TEOS) within water-laden channels inside the space created by self-assembled AOT molecules to prepare regular and nanosized silica in self-assembled sodium bis(2-ethylhexyl) sulfosuccinate (AOT) gels. The AOT gels were obtained by adding small amounts of water to organic solvents containing high concentrations of AOT. Adding silica significantly influenced the rheological properties and microstructures of these AOT/silica gels. Rheological studies showed that the storage modulus G' and loss modulus G″ of the AOT gel systems became very close and even crossed, indicating that the gel is "weak"; however, for the AOT/silica gel systems, the rheological data demonstrated that G' is greater than G″ at all frequencies, indicative of a real gel with a G' of approximately 10(5) pa. Small-angle X-ray scattering (SAXS) results showed that the gels initially had a hexagonal close-packed cylindrical structure with long-range order and transitioned to nonclose-packed cylindrical structures without long-range order as the silica formed. The cylinder is expected to comprise stacks of silica molecules surrounded by AOT molecules, and the radius of the cylinder is close to the sum of the length of one AOT molecule and half the size of one silica molecule. The rheological and SAXS data show that silica in the AOT/silica systems grew in the axial direction due to the confinement of these cylindrical structures, leading to nanowire silica structures. After removal of the AOT components, the nanowire silica was approximately 5-10 nm in diameter, as observed using transmission electron microscopy (TEM). PMID:27602986

  9. Preparation of Nanowire Silica Inside Self-Assembled Sodium Bis(2-ethylhexyl) Sulfosuccinate (AOT) Gels.

    PubMed

    Lai, Wei-Chi; Hong, Li-Tzuen

    2016-09-22

    In conventional sol-gel methods, gel formation occurs due to aggregation of particles into irregular shapes of larger size. In this study, we conducted hydrolysis-condensation reactions of tetraethyl orthosilicate (TEOS) within water-laden channels inside the space created by self-assembled AOT molecules to prepare regular and nanosized silica in self-assembled sodium bis(2-ethylhexyl) sulfosuccinate (AOT) gels. The AOT gels were obtained by adding small amounts of water to organic solvents containing high concentrations of AOT. Adding silica significantly influenced the rheological properties and microstructures of these AOT/silica gels. Rheological studies showed that the storage modulus G' and loss modulus G″ of the AOT gel systems became very close and even crossed, indicating that the gel is "weak"; however, for the AOT/silica gel systems, the rheological data demonstrated that G' is greater than G″ at all frequencies, indicative of a real gel with a G' of approximately 10(5) pa. Small-angle X-ray scattering (SAXS) results showed that the gels initially had a hexagonal close-packed cylindrical structure with long-range order and transitioned to nonclose-packed cylindrical structures without long-range order as the silica formed. The cylinder is expected to comprise stacks of silica molecules surrounded by AOT molecules, and the radius of the cylinder is close to the sum of the length of one AOT molecule and half the size of one silica molecule. The rheological and SAXS data show that silica in the AOT/silica systems grew in the axial direction due to the confinement of these cylindrical structures, leading to nanowire silica structures. After removal of the AOT components, the nanowire silica was approximately 5-10 nm in diameter, as observed using transmission electron microscopy (TEM).

  10. Thermal Insulation Composite Prepared from Carbon Foam and Silica Aerogel Under Ambient Pressure

    NASA Astrophysics Data System (ADS)

    Liu, Heguang; Li, Tiehu; Shi, Yachun; Zhao, Xing

    2015-10-01

    Carbon foam/silica aerogel composite as a promising thermal insulation material was prepared under ambient pressure successfully in the present work. Carbon foam was prepared by pretreatment, foaming, and carbonization process, while silica aerogel was synthesized by sol-gel method. The microstructure, morphology characteristics, compression strength, and thermal properties of composite were characterized by infrared spectroscopy, x-ray diffraction, scanning electron microscope, universal testing machine, and laser flash thermal detector, respectively. Results showed that silica aerogel was successfully synthesized in the surface foam cells of carbon foam due to the closed cell structure of carbon foam. Moreover, the compressive strength of the carbon foam was not affected by the silica aerogel in the cell structure of carbon foam, while its thermal insulation property at room temperature was improved.

  11. [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. PMID:27319171

  12. Effect of nanoparticle coating on the thermal conductivity of microporous thermal insulations.

    PubMed

    Lee, Dong-Bok; Kwon, Hyuk-Chon; Kim, Yun-Il; Park, Sung; Lee, Jae Chun; Misture, Scott

    2010-05-01

    Microporous thermal insulations were prepared from mixtures of nano-sized fumed silica, micron-sized fibers and opacifier particles. Those micron-sized particles were dry coated with nano-sized fumed silica particles by mechanical process using a compressive-shear type mill. The effect of nanoparticle coating on the thermal conductivity of the insulation media was investigated using a hot-wire method. Effect of nanoparticle coating was found to be more pronounced for the insulation composed of fumed silica and fiber than for the one composed of fumed silica, fiber and an opacifier. By adding 15% SiC or TiO2 opacifier, the thermal conductivity of the insulation samples could be lowered to 0.08 Wm(-1) K(-1) at temperature range of 805 approximately 817 degrees C. The temperature dependent thermal conductivity of the sample containing glass fiber did not exhibit any remarkable changes compared to the one containing ceramic fiber.

  13. 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. PMID:24830747

  14. Micro-PIXE and micro-RBS characterization of micropores in porous silicon prepared using microwave-assisted hydrofluoric acid etching.

    PubMed

    Ahmad, Muthanna; Grime, Geoffrey W

    2013-04-01

    Porous silicon (PS) has been prepared using a microwave-assisted hydrofluoric acid (HF) etching method from a silicon wafer pre-implanted with 5 MeV Cu ions. The use of microbeam proton-induced X-ray emission (micro-PIXE) and microbeam Rutherford backscattering techniques reveals for the first time the capability of these techniques for studying the formation of micropores. The porous structures observed from micro-PIXE imaging results are compared to scanning electron microscope images. It was observed that the implanted copper accumulates in the same location as the pores and that at high implanted dose the pores form large-scale patterns of lines and concentric circles. This is the first work demonstrating the use of microwave-assisted HF etching in the formation of PS.

  15. Preparation of silica-encapsulated ZnSe nanocrystals by mixed surfactant microemulsions.

    PubMed

    Liu, Kang; Ma, Sung Jin; Kim, Ji Hyeon; Choi, Hyung Wook; Kim, Kyung Hwan; Park, Sang Joon

    2013-11-01

    Silica-encapsulated ZnSe nanocrystals (NCs) have been prepared by employing sodium (2-ethylhexyl)sulfonate (AOT)/water/cyclohexane microemulsions containing ZnSe quantum dots with polyoxyethylenenonylphenylether (NP5)/water/cyclohexane microemulsions containing tetraethylorthosilicate (TEOS). Size tunable silica nanoparticles were achieved by using various water-to-surfactant ratios, W ([H2O]/[surfactant]). In order to characterize as-synthesized nanocrystals, photoluminescence (PL) spectroscopy, UV-visible spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR) were employed. Cubic zinc blende quantum dots (QDs) (2.5 nm in diameter) were successfully encapsulated by silica nanoparticles (14.3-28.9 nm in diameter). The enhanced photoluminescence efficiency about 10% has been observed when compared with the results from the similar work using AOT microemulsions. The entire size of the silica-encapsulated nanocrystals increased with increasing W, then decreased slightly when free water exists in the core of the NP5/AOT microemulsion. On the other hand, the ZnSe NCs in the silica did not change their size during the synthesis. In addition, the possible mechanisms for growth of silica particles and the kinetics of silica particles formation were discussed. PMID:24245247

  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. PMID:26695263

  17. 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.

  18. 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.

  19. Nanocomposites with fumed silica/poly(vinyl pyrrolidone) prepared at a low content of solvents

    NASA Astrophysics Data System (ADS)

    Gun'ko, V. M.; Voronin, E. F.; Nosach, L. V.; Pakhlov, E. M.; Voronina, O. E.; Guzenko, N. V.; Kazakova, O. A.; Leboda, R.; Skubiszewska-Zięba, J.

    2006-12-01

    Highly disperse nanocomposites with fumed silica/poly(vinyl pyrrolidone) (PVP) prepared using different methods were studied by infrared spectroscopy, adsorption, and quantum chemistry methods. Low amounts of water or ethanol (30 wt.% with respect to the silica content) promote appropriate distribution of PVP on silica particles. The use of ethanol leads to a smaller loss of the specific surface area ( SBET) than in the case of water used as a solvent. On PVP distribution on a silica surface, treatment of the system in a pseudo-liquid state reactor (PLSR) provides slightly better results (a lower loss in SBET) in comparison with mechanochemical activation (MCA) in a ball mill at the PVP monolayer coverage. An increase in the activation time to 6-9 h leads to an increase in the |Δ SBET/ SBET| value to 0.29-0.35 for both treatment methods.

  20. 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.

  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. PMID:21780498

  2. Facile route for preparation of silver nanoparticle-coated precipitated silica

    NASA Astrophysics Data System (ADS)

    Quang, Dang Viet; Sarawade, Pradip B.; Hilonga, Askwar; Park, Sung Dae; Kim, Jong-Kil; Kim, Hee Taik

    2011-02-01

    In this research, a facile route was used to prepare silver nanoparticle-coated precipitated silica using sodium silicate, a cheap precursor. Precipitated silica (PS) was synthesized by dropping 8% H2SO4 into a mixed solution of sodium silicate 24% (Na2O·3.4SiO2) and NaCl 4%; under constant stirring. The precipitated silica was then modified by simultaneous addition of 3-aminopropyltriethoxysilane (3-APTES) and 8% H2SO4. The resulting material was aged at 80 °C for 1 h to produce amino-functionalized precipitated silica (AFPS). Silver nanoparticle-coated precipitated silica (Ag-NPS) was synthesized by adding silver nitrate (AgNO3). The synthesis procedure also involved mixing for 2 h and dropping 0.05 M sodium borohydride (NaBH4). The final products, namely, PS, AFPS, and Ag-NPS were characterized using BET analyzer, FE-SEM, TEM and XRD. Silver nanoparticles with an average size ranging from 18 to 25 nm were found mostly coated on the exterior layer of the precipitated silica. The synthesis method reported in this work is facile and might be used for large-scale industrial production of inexpensive Ag-NPS.

  3. Facile large scale preparation and electromagnetic properties of silica-nickel-carbon composite shelly hollow microspheres.

    PubMed

    An, Zhenguo; Zhang, Jingjie

    2016-02-21

    Silica-nickel-carbon composite microspheres with shelly hollow structures and tunable electromagnetic properties were prepared in large scale through a three-step route. Micron-sized precursor microspheres were prepared firstly by spray drying of water glass. Then a subsequent acid leaching with diluted hydrochloric acid was carried out to eliminate the Na2O in the precursor microspheres to get single shell silica hollow microspheres (SHMs). Afterwards, Ni-C composite shells were assembled on the surface of the previously formed SHMs through a calcination route in an inert atmosphere to form silica-nickel-carbon composite shelly hollow microspheres (CSHMs) through decomposition of the reactants and carbon thermal reduction. By properly tuning the calcination conditions, silica-nickel CSHMs with gradients in composition can also be prepared. The electromagnetic properties of the CSHMs were studied and the results demonstrate that they present ferromagnetic and microwave absorbing properties related to the shell composition. The DSHPs thus obtained may have some promising applications in the fields of low-density magnetic materials and microwave absorbers. This work provides a new strategy to fabricate shelly hollow particles, which can be expected to be extended to the controlled preparation of similar structures with various compositions. PMID:26726765

  4. Surfactant-free small Ni nanoparticles trapped on silica nanoparticles prepared by pulsed laser ablation in liquid

    NASA Astrophysics Data System (ADS)

    Mafuné, Fumitaka; Okamoto, Takumi; Ito, Miho

    2014-01-01

    Small Ni nanoparticles supported on silica nanoparticles were formed by pulsed laser ablation in liquid. Water dispersing surfactant-free silica particles was used here as a solvent, and a bulk Ni metal plate as a target. The nanoparticles formed by laser ablation in water were readily stabilized by the silica particles, whereas Ni nanoparticles prepared in water without silica were found to be precipitated a few hours after aggregation into 5-30 nm particles. The nanoparticles were characterized by TEM, dark-field STEM and optical absorption spectroscopy, which indicated that small 1-3 nm Ni nanoparticles were adsorbed on the surface of silica.

  5. Preparation and CO{sub 2} adsorption properties of aminopropyl-functionalized mesoporous silica microspheres

    SciTech Connect

    Araki, S.; Doi, H.; Sano, Y.; Tanaka, S.; Miyake, Y.

    2009-11-15

    Aminopropyl-functionalized mesoporous silica microspheres (AF-MSM) were synthesized by a simple one-step modified Stober method. Dodecylamine (DDA) was used as the catalyst for the hydrolysis and condensation of the silica source and as the molecular template to prepare the ordered mesopores. The mesoporous silica surfaces were modified to aminopropyl groups by the co-condensation of tetraethoxysilane (TEOS) with 3-aminopropyltriethoxysilane (APTES), up to a maximum of 20 mol.% APTES content in the silica source. The particle size, Brunauer-Emmet-Teller (BET) specific surface area, and mesoporous regularity decreased with increasing APTES content. It is believed that this result is caused by a decreasing amount of DDA incorporated into AF-MSM with increasing APTES content. It was also confirmed that the spherical shape and the mesostructure were maintained even if 20 mol.% of APTES was added to the silica source. Moreover, AF-MSM was applied to the CO{sub 2} adsorbent. The breakthrough time of the CO{sub 2} and CO{sub 2} adsorption capacities increased with increasing APTES content. The adsorption capacity of CO{sub 2} for AF-MSM, prepared at 20 mol.% APTES, was 0.54 mmol g{sup -1}. Carbon dioxide adsorbed onto AF-MSM was completely desorbed by heating in a N{sub 2} purge at 423 K for 30 min.

  6. A novel method of preparing metallic Janus silica particles using supercritical carbon dioxide.

    PubMed

    Yang, Qiuyan; de Vries, Marcel H; Picchioni, Francesco; Loos, Katja

    2013-11-01

    In this study, we demonstrate a novel fabrication method to prepare metallic Janus silica particles by embedding nanosized silica particles on a spherical polystyrene (PS) substrate in supercritical carbon dioxide (sc CO2), followed by labelling with gold nanoparticles on the exposed part of the silica colloids. To this end, three main types of Janus particles displaying two distinct surfaces are produced by recovering silica from the polystyrene template. Embedment of particles into the PS template in sc CO2 allows for precise control of the degree of embedding of particles and subsequent modification of the partially exposed particle surface. The embedding degree, as well as the final Janus balance, can be varied over a wide range through control of pressure, temperature, or treatment time of sc CO2. Hierarchical PS-silica composites and embedment are evaluated by scanning electron microscopy (SEM). Partial surface modification with gold nanoparticles is investigated by transmission electron microscopy (TEM). With this method various functionalized Janus particles with tuneable properties can be prepared by adjusting various surface modifiers and polymer substrates in the future. PMID:24056955

  7. 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.

  8. 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.%.

  9. 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

  10. 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.

  11. 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. PMID:26691852

  12. 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.

  13. 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).

  14. Preparation and characterization of poly (ethylene glycol)-coated Stoeber silica nanoparticles for biomedical applications

    NASA Astrophysics Data System (ADS)

    Kopelman, Raoul; Xu, Hao; Yan, Fei; Monson, Eric E.; Tang, Wei; Schneider, Randy; Philbert, Martin A.

    2002-06-01

    Monodisperse, spherical, polyethylene glycol (PEG)-coated silica nanoparticles have been prepared in the size range of 50-350 nm, and their size distribution were characterized by SEM and multi-angle static light scattering experiments. The chemical binding of PEG to the silica nanoparticles was confirmed by IR spectroscopy. The biocompatibility of these PEGylated nanoparticles was also studied by non-specific protein binding tests and in-vivo toxicology studies in live animals. These silica nanoparticles, as a matrix for encapsulation of certain reagents, have been used for the fabrication of intracellular sensors and have potential for applications to in vivo diagnosis, analysis and measurements, due to their small physical size and their biocompatibility, both stemming from the specialized PEG coating.

  15. Porous polylactic acid-silica hybrids: preparation, characterization, and study of mesenchymal stem cell osteogenic differentiation.

    PubMed

    Pandis, Christos; Trujillo, Sara; Matos, Joana; Madeira, Sara; Ródenas-Rochina, Joaquín; Kripotou, Sotiria; Kyritsis, Apostolos; Mano, João F; Gómez Ribelles, José Luis

    2015-02-01

    A novel approach to reinforce polymer porous membranes is presented. In the prepared hybrid materials, the inorganic phase of silica is synthesized in-situ and inside the pores of aminolyzed polylactic acid (PLA) membranes by sol-gel reactions using tetraethylorthosilicate (TEOS) and glycidoxypropyltrimethoxysilane (GPTMS) as precursors. The hybrid materials present a porous structure with a silica layer covering the walls of the pores while GPTMS serves also as coupling agent between the organic and inorganic phase. The adjustment of silica precursors ratio allows the modulation of the thermomechanical properties. Culture of mesenchymal stem cells on these supports in osteogenic medium shows the expression of characteristic osteoblastic markers and the mineralization of the extracellular matrix. PMID:25303745

  16. Porous polylactic acid-silica hybrids: preparation, characterization, and study of mesenchymal stem cell osteogenic differentiation.

    PubMed

    Pandis, Christos; Trujillo, Sara; Matos, Joana; Madeira, Sara; Ródenas-Rochina, Joaquín; Kripotou, Sotiria; Kyritsis, Apostolos; Mano, João F; Gómez Ribelles, José Luis

    2015-02-01

    A novel approach to reinforce polymer porous membranes is presented. In the prepared hybrid materials, the inorganic phase of silica is synthesized in-situ and inside the pores of aminolyzed polylactic acid (PLA) membranes by sol-gel reactions using tetraethylorthosilicate (TEOS) and glycidoxypropyltrimethoxysilane (GPTMS) as precursors. The hybrid materials present a porous structure with a silica layer covering the walls of the pores while GPTMS serves also as coupling agent between the organic and inorganic phase. The adjustment of silica precursors ratio allows the modulation of the thermomechanical properties. Culture of mesenchymal stem cells on these supports in osteogenic medium shows the expression of characteristic osteoblastic markers and the mineralization of the extracellular matrix.

  17. 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). PMID:25622518

  18. Preparation of fluorescent mesoporous hollow silica-fullerene nanoparticles via selective etching for combined chemotherapy and photodynamic therapy

    NASA Astrophysics Data System (ADS)

    Yang, Yannan; Yu, Meihua; Song, Hao; Wang, Yue; Yu, Chengzhong

    2015-07-01

    Well-dispersed mesoporous hollow silica-fullerene nanoparticles with particle sizes of ~50 nm have been successfully prepared by incorporating fullerene molecules into the silica framework followed by a selective etching method. The fabricated fluorescent silica-fullerene composite with high porosity demonstrates excellent performance in combined chemo/photodynamic therapy.Well-dispersed mesoporous hollow silica-fullerene nanoparticles with particle sizes of ~50 nm have been successfully prepared by incorporating fullerene molecules into the silica framework followed by a selective etching method. The fabricated fluorescent silica-fullerene composite with high porosity demonstrates excellent performance in combined chemo/photodynamic therapy. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr02769a

  19. Preparation and characterization of chemically functionalized silica-coated magnetic nanoparticles as a DNA separator.

    PubMed

    Kang, Kiho; Choi, Jinsub; Nam, Joong Hee; Lee, Sang Cheon; Kim, Kyung Ja; Lee, Sang-Won; Chang, Jeong Ho

    2009-01-15

    The work describes a simple and convenient process for highly efficient and direct DNA separation with functionalized silica-coated magnetic nanoparticles. Iron oxide magnetic nanoparticles and silica-coated magnetic nanoparticles were prepared uniformly, and the silica coating thickness could be easily controlled in a range from 10 to 50 nm by changing the concentration of silica precursor (TEOS) including controlled magnetic strength and particle size. A change in the surface modification on the nanoparticles was introduced by aminosilanization to enhance the selective DNA separation resulting from electrostatic interaction. The efficiency of the DNA separation was explored via the function of the amino-group numbers, particle size, the amount of the nanoparticles used, and the concentration of NaCl salt. The DNA adsorption yields were high in terms of the amount of triamino-functionalized nanoparticles used, and the average particle size was 25 nm. The adsorption efficiency of aminofunctionalized nanoparticles was the 4-5 times (80-100%) higher compared to silica-coated nanoparticles only (10-20%). DNA desorption efficiency showed an optimum level of over 0.7 M of the NaCl concentration. To elucidate the agglomeration of nanoparticles after electrostatic DNA binding, the Guinier plots were calculated from small-angle X-ray diffractions in a comparison of the results of energy diffraction TEM and confocal laser scanning microscopy. Additionally, the direct separation of human genomic DNA was achieved from human saliva and whole blood with high efficiency.

  20. Preparation, characterization, and in vivo evaluation of tanshinone IIA solid dispersions with silica nanoparticles

    PubMed Central

    Jiang, Yan-rong; Zhang, Zhen-hai; Liu, Qi-yuan; Hu, Shao-ying; Chen, Xiao-yun; Jia, Xiao-bin

    2013-01-01

    We prepared solid dispersions (SDs) of tanshinone IIA (TSIIA) with silica nanoparticles, which function as dispersing carriers, using a spray-drying method and evaluated their in vitro dissolution and in vivo performance. The extent of TSIIA dissolution in the silica nanoparticles/TSIIA system (weight ratio, 5:1) was approximately 92% higher than that of the pure drug after 60 minutes. However, increasing the content of silica nanoparticles from 5:1 to 7:1 in this system did not significantly increase the rate or extent of TSIIA dissolution. The physicochemical properties of SDs were investigated using scanning electron microscopy, differential scanning calorimetry, X-ray powder diffraction, and Fourier transforms infrared spectroscopy. Studying the stability of the SDs of TSIIA revealed that the drug content of the formulation and dissolution behavior was unchanged under the applied storage conditions. In vivo tests showed that SDs of the silica nanoparticles/TSIIA had a significantly larger area under the concentration-time curve, which was 1.27 times more than that of TSIIA (P < 0.01). Additionally, the values of maximum plasma concentration and the time to reach maximum plasma concentration of the SDs were higher than those of TSIIA and the physical mixing system. Based on these results, we conclude that the silica nanoparticle based SDs achieved complete dissolution, increased absorption rate, maintained drug stability, and showed improved oral bioavailability compared to TSIIA alone. PMID:23836971

  1. 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.

  2. 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.

  3. 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. PMID:27561496

  4. 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.

  5. 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.

  6. Use of Silica Sol Step Gradients to Prepare Bundle Sheath and Mesophyll Chloroplasts from Panicum maximum.

    PubMed

    Walbot, V

    1977-07-01

    The first method for the direct separation of mesophyll and bundle sheath chloroplasts from whole tissue homogenates of a C(4) plant is described. Centrifugation of mixed chloroplast preparations from Panicum maximum through low viscosity silica sol gradients effectively separates large, starch-containing chloroplasts from smaller plastids. The large chloroplasts are judged to be bundle sheath chloroplasts on the basis of microscopic appearance, the presence of starch grains, the protein complement displayed on sodium dodecyl sulfate acrylamide gels, and the exclusive localization of ribulose bisphosphate carboxylase activity in these plastids. As a measure of intactness both the large (bundle sheath) and small (mesophyll) chloroplasts contain glyceralde-hyde-3-phosphate NADP-dependent dehydrogenase activity that is greatly enhanced by plastid lysis and both chloroplast preparations are impermeable to deoxyribonuclease. Chloroplast enzyme activities are inhibited by silica sol due to the Mg(2+) chelating activity of this reagent. However, well washed chloroplasts separated on silica gradients had enzyme activities similar to reported values in which silica sol gradients were not used. PMID:16660019

  7. 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.

  8. Preparation of Composite Coating on AZ91D Magnesium Alloy by Silica Sol-Micro Oxidation

    NASA Astrophysics Data System (ADS)

    Shao, Zhongcai; Zhang, Feifei; Zhao, Ruiqiang; Shen, Xiaoyi

    2016-03-01

    Composite coating was prepared on AZ91D magnesium alloy with a new method which combined silica sol with micro-arc oxidation (MAO). The MAO coating was prepared on the basis of MAO solution, and then coated by sol-gel process. The composite coating was obtained after second MAO treatment. Scanning electron microscopy coupled with X-ray diffraction (XRD), energy spectrum analysis and electrochemical testing was applied to characterize the properties of MAO coating and composite coating. The experimental test results indicated that the Si element derived from SiO2 gel particle embedded into the MAO coating by second MAO treatment. The surface of composite coating became dense and the holes were smaller with silica sol sealing process. The corrosion resistance of composite coating was improved than the MAO coating.

  9. 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.

  10. 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.

  11. 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.

  12. 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. PMID:27455659

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. Preparation of bicontinuous mesoporous silica and organosilica materials containing gold nanoparticles by co-synthesis method

    SciTech Connect

    Lee, Byunghwan; Zhu, Haoguo; Zhang, Zongtao; Overbury, Steven {Steve} H; Dai, Sheng

    2004-01-01

    Catalytic activities of gold strongly depend on its particle size. It is necessary to have homogeneous distributions of small gold nanoparticles with diameters between 2 and 5 nm for excellent catalytic activities. In this study, gold-containing mesoporous silica materials were prepared by a co-synthesis method. The essence of this sol-gel co-synthesis method is to combine together neutral surfactant template synthesis of mesoporous silica materials with the introduction of metal ions via bifunctional silane ligands, so that the formation of mesostructures and metal-ion doping occur simultaneously. The formation of gold nanoparticles with size less than 5 nm inside mesoporous materials (HMS, MSU, and PMO) has been achieved by this co-synthesis sol-gel process. In addition, the effects of post-treatments, such as calcination and reduction, on pore structures and nanoparticle size distributions were also investigated.

  18. [Preparation and anti-cancer activity in vitro of curcumin loaded mesoporous silica nanoparticle].

    PubMed

    He, Li-li; Gu, Jian

    2015-11-01

    This paper is to prepare curcumin (Cur) loaded mesoporous silica nanoparticle (Cur-MSN), evaluate its release behavior and anti-cancer activity in vitro. Mesoporous silica nanoparticle (MSN) was prepared by polymerization method and Cur-MSN was obtained using solvent evaporation method and impregnation centrifugation method. The preparation method was optimized using entrapment efficiency (EE) and loading efficiency (LE) as indexes. Cur-MSN was characterized with scanning electron microscope and its particle size and zeta potential were determined. Finally, in vitro release behavior in 0.2% SDS solution and its cell-killing effect on HeLa cells were also evaluated. The Cur-MSN prepared with process optimization method was round and uniform and exhibited typical mesoporous characterization. The mean particle size and Zeta potential of Cur-MSN were 75.8 nm and -30.1 mV, respectively. EE and LE of three batches of Cur-MSN were (72.55 ± 2.01)% and (16.21 ± 1.12)%, respectively. In vitro release behavior of Cur-MSN showed a sustained release profile with 83.5% cumulative release within 96 h. The killing effect of Cur-MSN on HeLa cells was dose-dependent with IC50 of 19.40 mg x L(-1), which was similar to that of Cur. PMID:27071254

  19. 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

  20. Infrared spectroscopy analysis of the local atomic structure in silica prepared by sol-gel

    NASA Astrophysics Data System (ADS)

    Martínez, J. R.; Ruiz, F.; Vorobiev, Y. V.; Pérez-Robles, F.; González-Hernández, J.

    1998-11-01

    Infrared spectroscopy has been used to analyze the structural changes in samples prepared by the sol-gel method. Silica gels were prepared from alcoholic solutions of tetraethylorthosilicate (TEOS) with different H2O/TEOS molar ratios. The IR spectra of these gels, in the Si-O bond stretching region, shows that their structure strongly depends on the H2O/TEOS ratio. The relative change in intensity of the Si-O stretching modes, in samples prepared using different H2O/TEOS ratios, are interpreted in terms of different degrees of structural disorder. According to our infrared absorption data, a decrease in the H2O/TEOS ratio from about 7, the SiO2 structure evolves from a three-dimensional network toward a chainlike structure.

  1. 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

    2013-04-01

    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.

  2. 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

    2013-04-01

    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. PMID:23434082

  3. 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.

  4. 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.

  5. 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.

  6. 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. PMID:25892637

  7. Rubber products prepared from silica modified by radiation-induced admicellar polymerization

    NASA Astrophysics Data System (ADS)

    Pongprayoon, Thirawudh; Yooprasert, Narissara; Suwanmala, Phiriyatorn; Hemvichian, Kasinee

    2012-05-01

    Unmodified silica, silica modified with Si69, silica modified by thermal admicellar polymerization and silica modified by radiation-induced admicellar polymerization were applied as rubber reinforcement. Mechanical properties of these different rubber formulae were subsequently tested. The results revealed that the mechanical properties of rubber reinforced with silica modified by admicellar polymerization were superior to those reinforced with unmodified silica or silica modified with Si69. As for the silica modified by admicellar polymerization, cetyltrimethyl ammonium bromide (CTAB) proved to be the most effective surfactant, compared to dodecyltrimethyl ammonium bromide (DTAB) and tetradecyltrimethyl ammonium bromide (TTAB).

  8. [Preparation of procion brilliant blue-doped silica nanorods and their recognition properties for proteins].

    PubMed

    Deng, Qiliang; Chen, Yang; Wu, Jianhua; Li, Yanli; Liu, Chunjing; Song, Weijing

    2011-09-01

    Protein enrichment and separation is one of the pivotal preliminary steps of proteomics studies, which is important to medical diagnosis and treatment. In this study, procion brilliant blue-doped silica nanorod was prepared via self-assembly sol-gel technology without any additional template. Procion brilliant blue was covalently linked to 3-aminopropyltriethyloxy silane in ethanol. Tetraethylorthosilane (TEOS) was then added into the mixture, subsequently hydrolyzed and co-condensed for 3 h under stirring. The resulted nanorods were isolated by centrifugation, re-dispersed in deionized water, and centrifuged again. This wash process was repeated three times. Finally, the nanorods were dried under vacuum. Procion brilliant blue acted simultaneously as a self-assembly template during the preparation process, and subsequently as recognition probe for proteins. Scanning electron microscopy (SEM) image showed that the nanotubes were 2-16 microm in length and 200-500 nm in diameter. The obtained nanorods were further characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSA), separately. All these results indicated that procion brilliant blue were successfully doped into silica nanorods. The recognition property of nanorods for bovine serum albumin (BSA) was investigated under static condition. The resulted nanorods showed high binding capacity (57.6 mg/g) for BSA and fast adsorption equilibrium (within 60 min). The nanorods were also evaluated with four typical proteins, hemoglobin, trypsin, lysozyme and pepsin, with different relative molecular masses and isoelectric points. The results indicated that the prepared nanorods exhibited the highest binding capacity for trypsin (87.5 mg/g) and the least binding for hemoglobin (Hb, 3.0 mg/g). This easy preparation protocol and excellent recognition property make the prepared materials a bright future in proteomics research. PMID:22233075

  9. 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

  10. 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

  11. Ordered micro/mesoporous composite prepared as thin films.

    PubMed

    Petkov, N; Hölzl, M; Metzger, T H; Mintova, S; Bein, T

    2005-03-17

    A new synthesis method for preparation of thin films and powders consisting of zeolite beta nanocrystals embedded in ordered mesoporous silica matrix is described. The final structures possessing bimodal porosity, i.e., high degree of mesophase order and spatially defined microporous zeolite nanocrystals are obtained via simultaneous solvent evaporation of preformed silica/surfactant/ethanol/nanosized zeolite beta assemblies. The films were characterized with grazing-incident diffraction (GID), nitrogen sorption based on gravimetric measurements with quartz crystal microbalance (QCM) devices, and transmission electron microscopy (TEM). It is shown that the incorporation of beta nanocrystals in the mesoporous silica matrix and the mesophase order itself can be controlled through the variation of the fractional amounts of the zeolite nanoparticles and silica/surfactant solutions. The HR-TEM measurements showed that the nanosized Beta microporous crystals are separated and at the same time connected through an ordered mesostructured matrix.

  12. Preparation of silica films on Ru(0001): A LEEM/PEEM study

    NASA Astrophysics Data System (ADS)

    Klemm, H. W.; Peschel, G.; Madej, E.; Fuhrich, A.; Timm, M.; Menzel, D.; Schmidt, Th.; Freund, H.-J.

    2016-01-01

    We use an aberration corrected spectro-microscope, the low energy electron microscope/photoelectron emission microscope (LEEM/PEEM) SMART, to follow the preparation and structure of a bilayer silica film on Ru(0001) as a function of temperature and oxidation conditions. This allows us to analyze the growth process at different length scales in order to judge on the overall quality and the morphology of the film. It is found that the film growth occurs in a crystalline and a vitreous phase as previously discovered using scanning tunneling microscopy. However, the present experiment allows an analysis on the sub-micron level to gain insight into the growth process at a mesoscopic scale. We find that the fully oxidized film can be prepared but that this film contains holes. These are unavoidable and are important to consider, if one wants to use the films for ensemble averaging experiments to investigate migration and reaction of molecules between the silica film and the Ru(0001) substrate.

  13. 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.

  14. 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. PMID:27321060

  15. 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

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. 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. PMID:26353492

  1. 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.

  2. Scalable preparation of ultrathin silica-coated Ag nanoparticles for SERS application.

    PubMed

    Hu, Yanjie; Shi, Yunli; Jiang, Hao; Huang, Guangjian; Li, Chunzhong

    2013-11-13

    Silica-coated Ag nanoparticles (Ag@SiO2 NPs) have been successfully prepared by a scalable flame spray pyrolysis (FSP) technique with production rate up to 4 g/h in laboratory-scale. The ultrathin SiO2 shell, with a thickness 1 nm, not only effectively avoids the intersintering of Ag nanoparticles core at the high temperature, but also serves as a protective layer of the SERS-active nanostructure. The silica-coated Ag nanoparticles form agglomerates in the large temperature gradient zone, which with several nanometers gaps from each other but not contact. Such an intriguing feature can result in more Raman hot-spots generated at the gaps among Ag core active sites, which will beneficial for the whole SERS substrate enhancement. The results demonstrate that a maximum enhancement factor can reach ~10(5) with a detectable concentration as low as 10(-10) M for rhodamine 6G (R6G) molecules, indicating that the as-obtained unique nanostructure will be a promising candidate for SERS applications. PMID:24117322

  3. Silica-coated iron nanocubes: preparation, characterization and application in microwave absorption.

    PubMed

    Ni, Xiaomin; Zheng, Zhong; Hu, Xiang; Xiao, Xiukun

    2010-01-01

    Novel cubic nanocapsules consisting of metallic iron core and amorphous silica shell were fabricated through a simple chemical reduction route followed by a Stöber process. Thus-prepared Fe@SiO(2) nanocubes were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray photoelectron spectrometer (XPS), Fourier transform infrared spectrometer (FTIR), thermogravimetry-differential thermal analysis (TG-DTA), vibrating sample magnetometer (VSM) and scalar network analysis (SNA). Comparing with that of pure iron counterparts, silica-coated iron nanocubes exhibited improved magnetic properties, oxidation resistance and microwave absorption performance. A reflection loss (RL) exceeding -12 dB was obtained in the frequency range of 8-14 GHz for an absorber thickness of 2 mm, with an optimal RL of -18.2 dB at 9 GHz. Mechanism of the improved microwave absorption properties of the Fe@SiO(2) composite was discussed based on their magnetic properties and electromagnetic theory.

  4. 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.

  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. 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.

  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. PMID:23754795

  8. Preparation, characterization and FE-simulation of the reinforcement of polycaprolactone with PEGylated silica nanoparticles

    NASA Astrophysics Data System (ADS)

    Moussaif, N.; Viejo, I.; Bielsa, J. M.; Crespo, C.; Irusta, S.; Yagüe, C.; Meier, J. G.

    2012-09-01

    We recently published the preparation and characterization of polycaprolactone (PCL) nanocomposites with a 45% increased modulus reinforced with only 4 wt% PEGylated silica (polyethylene-glycol/SiO2) nanoparticles obtained by melt-extrusion [1]. The achieved reinforcement is related to an excellent dispersion of the nanoparticles due to the polyethylene-glycol graft of the nanoparticles which was obtained by a simple one-pot synthesis. X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (FTIR) analyses identified the location of the PEG at the PCL/silica interface. However, the extension of the interface could not be resolved. In an attempt to describe the effect of the interface on the reinforcement we applied several analytical micromechanical models. Models considering core-shell systems fitted the experimental data well and gave estimations of the modulus and extension of the interphase. However, different sets of parameters gave equally good representations. In an alternative approach, 3D representative volume elements (RVE) of the composite with spherical nanoparticles including the shell were built-up from the morphological data to carry out computational micromechanics based on finite elements (FE). The interphase was modeled in the RVE. Both approaches demonstrated the need of an interphase extension of roughly twice the radius of the particle. The FEM approach estimates the interface-modulus much higher than the analytical models.

  9. 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

    2016-01-01

    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. PMID:27153055

  10. Preparation of silica aerogels using CTAB/SDS as template and their efficient adsorption

    NASA Astrophysics Data System (ADS)

    Wa, Li; Fengyun, Li; Fanlu, Zhuo; Mengjing, Cao; Qiang, Cai; Jue, Huang; Weijun, Zhang; Mingwei, Mu

    2015-10-01

    Silica aerogels have been successfully synthesized using cationic cetyltrimethylammonium bromide (CTAB) and anionic sodium dodecyl sulfate (SDS) as template. This study provides a novel approach to synthesize silica aerogels. The molar ratio of surfactant mixture was CTAB/SDS = 1.00. The obtained silica aerogels exhibit very low apparent density (0.044 g cm-3) and high specific surface area (856 m2 g-1). Surfactant packing parameter theory is used to explain the possible formation mechanism of the silica aerogels using mixed surfactant template. In addition, the adsorption capacity of Rhodamine B on the as-synthesized silica aerogels is as higher as that on the commercial silica aerogels.

  11. 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.

  12. 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. PMID:27548279

  13. Microporous glassy fillers for dental composites.

    PubMed

    Mabie, C P; Menis, D L

    1978-07-01

    A microporous filler giving greatly improved finish ability, systemic nontoxic X-ray opacification, low thermal expansion (27.2 x 10(-6)/degrees C), and satisfactory translucencies has been developed for dental composite resin restorations. These fillers are prepared from frits obtained by the low-temperature calcination of gelled inorganic sols followed by a pulsed high-temperature treatment. Composites prepared from these fillers are within the range of commercial products with regard to strength and setting contraction.

  14. Binding behaviour of molecularly imprinted polymers prepared by a hierarchical approach in mesoporous silica beads of varying porosity.

    PubMed

    Baggiani, Claudio; Baravalle, Patrizia; Giovannoli, Cristina; Anfossi, Laura; Passini, Cinzia; Giraudi, Gianfranco

    2011-04-01

    One of the most interesting methods for preparing molecularly imprinted polymers with controlled morphology consists in filling the pores of silica beads with an imprinting mixture, polymerizing it and dissolving the support, leaving porous imprinted beads that are the "negative image" of the silica beads. The main advantage of such an approach consists in the easy preparation of spherical imprinted polymeric particles with narrow diameter and pore size distribution, particularly indicated for chromatographic applications. In this approach it has been shown that the resulting morphology of polymeric beads depends essentially on the porosity and surface properties of the silica beads that act as microreactors for the thermopolymerization process. Anyway, it is not yet clear if the porosity of the silica beads influences the binding properties of the resulting imprinted beads. In this paper, we report the effect of different porosities of the starting mesoporous silica beads on the resulting binding properties of imprinted polymers with molecular recognition properties towards the fungicide carbendazim. The morphological properties of the imprinted beads prepared through this hierarchical approach were measured by nitrogen adsorption porosimetry and compared with a reference imprinted material prepared by bulk polymerization. The chromatographic behaviour of HPLC columns packed with the imprinted materials were examined by eluting increasing amounts of carbendazim and extracting the binding parameters through a peak profiling approach. The experimental results obtained show that the resulting binding properties of the imprinted beads are strongly affected by the polymerization approach used but not by the initial porosity of the silica beads, with the sole exception of the binding site density, which appears to be inversely proportional to them. PMID:21349526

  15. 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. PMID:27155234

  16. 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. PMID:24857463

  17. Room-temperature preparation and characterization of poly (ethylene glycol)-coated silica nanoparticles for biomedical applications.

    PubMed

    Xu, Hao; Yan, Fei; Monson, Eric E; Kopelman, Raoul

    2003-09-15

    Monodisperse, spherical, polyethylene glycol (PEG)-coated silica nanoparticles have been prepared at room temperature and characterized for the purpose of biomedical applications. The particles were synthesized by the hydrolysis of tetramethyl orthosilicate (TMOS) in alcohol media under catalysis by ammonia, and their size can range from about 50-350 nm in diameter. We studied the particle size and size distribution using a scanning electron microscope (SEM) and an asymmetric field-flow fractionation (AFFF) multiangle static light-scattering instrument. The chemical and/or physical binding of PEG to the silica nanoparticles was studied by infrared spectroscopy, and the weight percentage of PEG attached to the particles was quantified. The PEG-coated silica nanoparticles showed enhanced colloidal stability when redispersed into aqueous solutions from the dried state as a result of the steric stabilization function of the PEG polymer grafted on the surface of particles. A nonspecific protein-binding test was also carried out to show that the PEG coating can help reduce the protein adsorption onto the surface of the particles, relating to the biocompatibility of these PEG-coated particles. Also, the inclusion of magnetic nanoparticles into the silica particles was shown as an example of the possible applications of PEG-coated silica particles. These silica nanoparticles, as a matrix for encapsulation of certain reagents, have potential for applications to in vivo diagnosis, analysis, and measurements inside intact biologic systems.

  18. 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.

  19. 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.

  20. 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. PMID:27427624

  1. Preparation and Characterization of Rifampin Loaded Mesoporous Silica Nanoparticles as a Potential System for Pulmonary Drug Delivery

    PubMed Central

    Mohseni, Meysam; Gilani, Kambiz; Mortazavi, Seyed Alireza

    2015-01-01

    The goal of this research is to determine the feasibility of loading rifampin into mesoporous silica nanoparticles. Rifampin was selected as a model lipophilic molecule since it is a well-documented and much used anti tuberculosis drug. The mesoporous silica nanoparticles were prepared by using tetraethyl ortho silicate and cetyltrimethyl ammonium bromide (as surfactant). The prepared nanoparticles were characterized in terms of their particle size measurement and porosimetry. The results showed that the particle size is 218 ± 46 nm (mean ± SD) and surface area is 816 m2g-1. In order to load rifampin within the mesopores, adsorption experiments using three different solvents (methanol, water and dimethyl sulfoxide) were carried out. The loading procedure resulted in a significant improvement in the amount of rifampin loaded into mesoporous silica nanoparticles and methanol was found to be a suitable solvent, providing a drug entrapment efficiency of 52 %. Rifampin loaded nanoparticles underwent different in-vitro tests including, SEM and drug release. The in-vitro drug release was investigated using buffer phosphate (pH=7.4). Regarding the drug release study, a biphasic pattern of release was observed. The drug-loaded mesoporous silica nanoparticles were capable of releasing 95% of their drug content after 24 h, following a faster release in the first four hours. The prepared rifampin loaded nanoparticles seem to have potential for use as a pulmonary drug delivery. PMID:25561909

  2. Blue-Emitting Small Silica Particles Incorporating ZnSe-Based Nanocrystals Prepared by Reverse Micelle Method

    PubMed Central

    Ando, Masanori; Li, Chunliang; Yang, Ping; Murase, Norio

    2007-01-01

    ZnSe-based nanocrystals (ca. 4-5 nm in diameter) emitting in blue region (ca. 445 nm) were incorporated in spherical small silica particles (20–40 nm in diameter) by a reverse micelle method. During the preparation, alkaline solution was used to deposit the hydrolyzed alkoxide on the surface of nanocrystals. It was crucially important for this solution to include Zn2+ ions and surfactant molecules (thioglycolic acid) to preserve the spectral properties of the final silica particles. This is because these substances in the solution prevent the surface of nanocrystals from deterioration by dissolution during processing. The resultant silica particles have an emission efficiency of 16% with maintaining the photoluminescent spectral width and peak wavelength of the initial colloidal solution. PMID:18350119

  3. 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.

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

    DOEpatents

    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. 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.

  6. The preparation of polypyrrole surfaces in the presence of mesoporous silica nanoparticles and their biomedical applications

    NASA Astrophysics Data System (ADS)

    Cho, Youngnam; Ben Borgens, Richard

    2010-05-01

    The deposition of carboxylic acid-terminated conducting polymer into two- or three-dimensional structures made up of colloidal particles has been successfully completed. This was accomplished using electrochemical deposition of ordered arrays of mesoporous silica nanoparticles (MSNs) as a template. Subsequent removal of the template yielded a porous polypyrrole surface. The co-polymerization of pyrrole with carboxylic acid-terminated pyrrole derivatives overcame the limitations of a lack of reactive functional groups—by facilitating the direct coupling of the film with biomolecules or drugs on the surface. Such Ppy films were characterized by several techniques: (1) scanning electron microscope (SEM) to evaluate surface topography, (2) x-ray photoelectron spectroscopy (XPS) to assess the chemical composition of the films, (3) four-point probe to measure the conductivity, and cyclic voltammogram to observe surface electroactivity. To assay the biological effectiveness of this preparation, we used phase-contrast light microscopy to compare neurite outgrowth from PC 12 cells grown on Ppy films in the presence and absence of electrical stimulation. These electrically functional, biocompatible composites show promise as novel neural implants that would deliver specific biologically active molecules in a highly localized manner to damaged or otherwise vulnerable cells such as found in the nervous system.

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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

  12. 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.

  13. 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. PMID:26075264

  14. Covalent conjugation of avidin with dye-doped silica nanopaticles and preparation of high density avidin nanoparticles as photostable bioprobes.

    PubMed

    Chen, Ze-Zhong; Cai, Li; Dong, Xiao-Min; Tang, Hong-Wu; Pang, Dai-Wen

    2012-01-01

    Progress in biomedical imaging depends on the development of bioprobes with a high sensitivity and stability. Fluorescent silica nanoparticles (NPs) covalent conjugation of avidin has been proposed for cancer cells imaging by fluorescence microscopy. Uniform silica NPs were prepared using water-in-oil (W/O) microemulsion methods and primary amine groups were introduced onto the surface of the NPs by condensation of tetraethyl orthosilicate (TEOS). Optically stable organic dyes, tris(2,2'-bipyridyl) dichlororuthenium(II) hexahydrate (Rubpy), were doped inside the silica NPs. The amine functions were transferred to carboxyl groups coupled with a linker elongation. Avidin was immobilized at the surface of the NPs by covalent binding to the carboxyl linkers. The binding capacity of the avidin-covered NPs for ligand biotin was quantified by titration with biotin(5-fluorescein) conjugate to 1.25 biotin binding sites/100 nm(2). We used biotinylated antibody and cell recognition by fluorescence microscopy imaging technique. The lung carcinoma cells were identified easily with high efficiency using these antibody-coated NPs. By comparison with fluorescein isothiocyanate (FITC), dye-doped silica NPs display dramatically increased stability of fluorescence as well as photostability, as compared to the common organic dye, when under continuous irradiation.

  15. 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.

  16. On-line automated sample preparation for liquid chromatography using parallel supported liquid membrane extraction and microporous membrane liquid-liquid extraction.

    PubMed

    Sandahl, Margareta; Mathiasson, Lennart; Jönsson, Jan Ake

    2002-10-25

    An automated system was developed for analysis of non-polar and polar ionisable compounds at trace levels in natural water. Sample work-up was performed in a flow system using two parallel membrane extraction units. This system was connected on-line to a reversed-phase HPLC system for final determination. One of the membrane units was used for supported liquid membrane (SLM) extraction, which is suitable for ionisable or permanently charged compounds. The other unit was used for microporous membrane liquid-liquid extraction (MMLLE) suitable for uncharged compounds. The fungicide thiophanate methyl and its polar metabolites carbendazim and 2-aminobenzimidazole were used as model compounds. The whole system was controlled by means of four syringe pumps. While extracting one part of the sample using the SLM technique. the extract from the MMLLE extraction was analysed and vice versa. This gave a total analysis time of 63 min for each sample resulting in a sample throughput of 22 samples per 24 h.

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

    PubMed

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

    2014-05-01

    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. PMID:24562100

  18. 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

  19. Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

    PubMed Central

    Lovingood, Derek D.; Owens, Jeffrey R.; Seeber, Michael; Kornev, Konstantin G.; Luzinov, Igor

    2013-01-01

    Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan δ solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials' morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by Stöber's methods, which have smooth surfaces. PMID:24379052

  20. 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).

  1. Preparative separation and purification of epigallocatechin gallate from green tea extracts using a silica adsorbent containing β-cyclodextrin.

    PubMed

    Lai, Shih-Ming; Gu, Jhe-Yu; Huang, Bing-Hao; Chang, Chieh-Ming J; Lee, Wen-Lung

    2012-03-01

    A silica adsorbent containing β-cyclodextrin (β-CD) has been developed and used for the separation and purification of epigallocatechin gallate (EGCG) from the green tea extracts. The batch adsorption experiments demonstrated that, the β-CD bonded silica adsorbent possessed excellent adsorption equilibrium capacity (> 55 mg/g adsorbent) and adsorption ratio (>95%) for EGCG compared to the other tea catechins and caffeine. The excellent adsorption capacity and selectivity for EGCG are attributed to the specific interactions between β-CD and EGCG. The preparative separation and purification performance of EGCG on the β-CD bonded silica column (220 mm L × 15 mm i.d., 40-63 μm) was then evaluated. The column was operated in the polar organic mode using methanol/acetonitrile/acetic acid as the mobile phase and eluted under a three-step gradient elution program. The sample was dissolved in acetonitrile and loaded on a preparative scale of about 0.8 mg/g adsorbent. Under the optimal chromatographic conditions, the target compound, EGCG, being the most retained species, was obtained at a purity of about 90% with a recovery of about 90%. The productivity of EGCG was about 6 mg per injection, which can be further increased by scaling-up the chromatographic system. PMID:22336694

  2. [Preparation and chromatographic performance of a eugenol-bonded silica gel stationary phase for high performance liquid chromatography].

    PubMed

    Xu, Lili; Zhong, Minghua; Chen, Xiaojing

    2015-05-01

    A eugenol-bonded silica gel stationary phase (EGSP) for high performance liquid chromatography ( HPLC) has been synthesized by the solid-liquid successive reaction method. The preparation process included two steps: firstly, γ-glycidoxypropyltrimethoxy-silane (KH-560) was covalently attached to the surface of spherical silica gel. Then the bonded silica gel continued to react with eugenol ligand, which was a plant active component, and obtained EGSP. The structure of EGSP was characterized by elemental analysis, thermogravimetric analysis and Fourier transform infrared spectroscopy. Using naphthalene as a probe, the column efficiency was tested under the mobile phase of acetonitrile-water (35:65, v/v) at a flow rate of 0.8 mL/min. The chromatographic properties and the retention mechanism of EGSP were evaluated by using neutral, basic and acidic analytes as solute probes. Meanwhile, the comparative study with C18 column and phenyl column was also carried out under the same chromatographic conditions. The result showed that the eugenol ligand was successfully bonded to the surface of silica gel with a 0.28 mmol/g of bonded amount, and the theoretical plate number of EGSP column was about 24 707 N/m. The EGSP appeared to be a kind of excellent reversed-phase stationary phase with suitable hydrophobicity and various synergistic sites. The eugenol ligand bonded on silica gel could first provide π-π interaction sites for different analytes because of its benzene ring and alkenyl. In addition, the methoxy groups of eugenol were responsible for dipole-dipole and hydrogen-bonding interactions between the ligand and solutes in the effective separation process. Comparing with traditional C18 column and phenyl column, EGSP has an advantage in the fast separation of polar compounds under simple experimental conditions. PMID:26387202

  3. [Preparation and chromatographic performance of a eugenol-bonded silica gel stationary phase for high performance liquid chromatography].

    PubMed

    Xu, Lili; Zhong, Minghua; Chen, Xiaojing

    2015-05-01

    A eugenol-bonded silica gel stationary phase (EGSP) for high performance liquid chromatography ( HPLC) has been synthesized by the solid-liquid successive reaction method. The preparation process included two steps: firstly, γ-glycidoxypropyltrimethoxy-silane (KH-560) was covalently attached to the surface of spherical silica gel. Then the bonded silica gel continued to react with eugenol ligand, which was a plant active component, and obtained EGSP. The structure of EGSP was characterized by elemental analysis, thermogravimetric analysis and Fourier transform infrared spectroscopy. Using naphthalene as a probe, the column efficiency was tested under the mobile phase of acetonitrile-water (35:65, v/v) at a flow rate of 0.8 mL/min. The chromatographic properties and the retention mechanism of EGSP were evaluated by using neutral, basic and acidic analytes as solute probes. Meanwhile, the comparative study with C18 column and phenyl column was also carried out under the same chromatographic conditions. The result showed that the eugenol ligand was successfully bonded to the surface of silica gel with a 0.28 mmol/g of bonded amount, and the theoretical plate number of EGSP column was about 24 707 N/m. The EGSP appeared to be a kind of excellent reversed-phase stationary phase with suitable hydrophobicity and various synergistic sites. The eugenol ligand bonded on silica gel could first provide π-π interaction sites for different analytes because of its benzene ring and alkenyl. In addition, the methoxy groups of eugenol were responsible for dipole-dipole and hydrogen-bonding interactions between the ligand and solutes in the effective separation process. Comparing with traditional C18 column and phenyl column, EGSP has an advantage in the fast separation of polar compounds under simple experimental conditions.

  4. SBA-15 mesoporous silica free-standing thin films containing copper ions bounded via propyl phosphonate units - preparation and characterization

    NASA Astrophysics Data System (ADS)

    Laskowski, Lukasz; Laskowska, Magdalena; Jelonkiewicz, Jerzy; Dulski, Mateusz; Wojtyniak, Marcin; Fitta, Magdalena; Balanda, Maria

    2016-09-01

    The SBA-15 silica thin films containing copper ions anchored inside channels via propyl phosphonate groups are investigated. Such materials were prepared in the form of thin films, with hexagonally arranged pores, laying rectilinear to the substrate surface. However, in the case of our thin films, their free standing form allowed for additional research possibilities, that are not obtainable for typical thin films on a substrate. The structural properties of the samples were investigated by X-ray reflectometry, atomic force microscopy (AFM) and transmission electron microscopy (TEM). The molecular structure was examined by Raman spectroscopy supported by numerical simulations. Magnetic measurements (SQUID magnetometry and EPR spectroscopy) showed weak antiferromagnetic interactions between active units inside silica channels. Consequently, the pores arrangement was determined and the process of copper ions anchoring by propyl phosphonate groups was verified in unambiguous way. Moreover, the type of interactions between magnetic atoms was determined.

  5. 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.

  6. 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.

  7. 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.

  8. Water-Dispersible, Responsive, and Carbonizable Hairy Microporous Polymeric Nanospheres.

    PubMed

    Mai, Weicong; Sun, Bin; Chen, Luyi; Xu, Fei; Liu, Hao; Liang, Yeru; Fu, Ruowen; Wu, Dingcai; Matyjaszewski, Krzysztof

    2015-10-21

    Multifunctionalization of microporous polymers is highly desirable but remains a significant challenge, considering that the current microporous polymers are generally hydrophobic and nonresponsive to different environmental stimuli and difficult to be carbonized without damage of their well-defined nanomorphology. Herein, we demonstrate a facile and versatile method to fabricate water-dispersible, pH/temperature responsive and readily carbonizable hairy microporous polymeric nanospheres based on combination of the hyper-cross-linking chemistry with the surface-initiated atom transfer radical polymerization (SI-ATRP). The hyper-cross-linking creates a highly microporous core, whereas the SI-ATRP provides diverse functionalities by surface grafting of hairy functional blocks. The as-prepared materials present multifunctional properties, including sensitive response to pH/temperature, high adsorption capacity toward adsorbates from aqueous solution, and valuable transformation into well-defined microporous carbon nanospheres because of hybrid of carbonizable core and thermo-decomposable protection shell. We hope this strategy could promote the development of both functional microporous polymers and advanced hairy nanoparticles for multipurpose applications.

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

    PubMed Central

    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. PMID:25313299

  10. 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.

  11. The formation of an ordered microporous aluminum-based material mediated by phthalic acid.

    PubMed

    Zhang, Wei; Cai, Jian-Hua; Huang, Pei-Pei; Hu, Lin-Lin; Cao, An-Min; Wan, Li-Jun

    2016-06-28

    By using phthalic acid as a soft template, we showed that it was possible to prepare a microporous aluminum-based material when the precipitation of Al(3+) was properly controlled. We also identified that this microporous aluminum-based material could be promising for the removal of fluoride ions in water treatment. PMID:27263661

  12. 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

  13. Preparation, characterization, and optical properties of gold, silver, and gold-silver alloy nanoshells having silica cores.

    PubMed

    Kim, Jun-Hyun; Bryan, William W; Lee, T Randall

    2008-10-01

    This report describes the structural and optical properties of a series of spherical shell/core nanoparticles in which the shell is comprised of a thin layer of gold, silver, or gold-silver alloy, and the core is comprised of a monodispersed silica nanoparticle. The silica core particles were prepared using the Stöber method, functionalized with terminal amine groups, and then seeded with small gold nanoparticles (approximately 2 nm in diameter). The gold-seeded silica particles were coated with a layer of gold, silver, or gold-silver alloy via solution-phase reduction of an appropriate metal ion or mixture of metal ions. The size, morphology, and elemental composition of the composite nanoparticles were characterized by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, thermal gravimetric analysis (TGA), dynamic light scattering (DLS), and transmission electron microscopy (TEM). The optical properties of the nanoparticles were analyzed by UV-vis spectroscopy, which showed strong absorptions ranging from 400 nm into the near-IR region, where the position of the plasmon band reflected not only the thickness of the metal shell, but also the nature of the metal comprising the shell. Importantly, the results demonstrate a new strategy for tuning the position of the plasmon resonance without having to vary the core diameter or the shell thickness. PMID:18788760

  14. 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. PMID:10578506

  15. Preparation of high-performance polymer electrolyte nanocomposites through nanoscale silica particle dispersion

    NASA Astrophysics Data System (ADS)

    Lee, Chang Hyun; Park, Ho Bum; Park, Chi Hoon; Lee, So Young; Kim, Ju Young; McGrath, James E.; Lee, Young Moo

    Nano-level dispersion with a minimum amount of non-porous and surface-functionalized nanoparticles is a key to tune physically a common polymer material with poor durability to a powerful material with excellent stability even under harsh fuel cell conditions. Surfactants composed of hydrophobic cores and hydrophilic outer shells are used to assist a homogenous distribution of surface-treated (hydrophilic and hydrophobic) silica nanoparticles. In particular, their effect on nanoparticle dispersion is conspicuous in polymer electrolyte nanocomposites containing hydrophilic surface-treated silica. The hydrophilic silica acts as an additional proton conductor in the acid electrolyte medium, leading to improved proton conductivity without any negative side-effects on the mechanical and chemical durability of the membrane material. The well-distributed hydrophilic silica nanoparticles are beneficial in preventing methanol permeation via compact polymer packing and in strengthening the membrane stability under hot aqueous conditions. Finally, the efficacy of the nano-level dispersion is electrochemically verified in terms of high single-cell performance and further extended life time as a result of a synergistic effect of improved proton conductivity, reduced methanol permeability and excellent hydrolytic durability.

  16. 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. PMID:27612823

  17. 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.

  18. 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.

  19. 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.

  20. Preparation of chlorocholine chloride/urea deep eutectic solvent-modified silica and an examination of the ion exchange properties of modified silica as a Lewis adduct.

    PubMed

    Tang, Baokun; Park, Ha Eun; Row, Kyung Ho

    2014-07-01

    Chlorocholine chloride/urea (ClChCl-urea), a deep eutectic solvent (DES), was applied successfully to the modification of silica. The resulting modified silica was characterized by Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller analysis, and elemental analysis. Based on the ClChCl-urea modification of silica, the ClChCl-urea-modified silica is a Lewis adduct with ion exchange properties, and ferulic acid was adsorbed on the ClChCl-urea-modified silica via an ion exchange process. The adsorbed percentage of ferulic acid increased with the increasing amount of modified silica, and a high adsorbed percentage of 89% could be obtained by the ion exchange process. The Freundlich isotherm used to describe the adsorption of ferulic acid on the modified silica by ion exchange showed a good correlation (R(2) = 0.93). Based on the characterization of the structure and the analysis of the ion exchange property of the ClChCl-urea-modified silica, the modified silica as a potential medium can be applied in some analytical technologies such as solid phase extraction, chromatography, and so on.

  1. Preparation of chlorocholine chloride/urea deep eutectic solvent-modified silica and an examination of the ion exchange properties of modified silica as a Lewis adduct.

    PubMed

    Tang, Baokun; Park, Ha Eun; Row, Kyung Ho

    2014-07-01

    Chlorocholine chloride/urea (ClChCl-urea), a deep eutectic solvent (DES), was applied successfully to the modification of silica. The resulting modified silica was characterized by Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller analysis, and elemental analysis. Based on the ClChCl-urea modification of silica, the ClChCl-urea-modified silica is a Lewis adduct with ion exchange properties, and ferulic acid was adsorbed on the ClChCl-urea-modified silica via an ion exchange process. The adsorbed percentage of ferulic acid increased with the increasing amount of modified silica, and a high adsorbed percentage of 89% could be obtained by the ion exchange process. The Freundlich isotherm used to describe the adsorption of ferulic acid on the modified silica by ion exchange showed a good correlation (R(2) = 0.93). Based on the characterization of the structure and the analysis of the ion exchange property of the ClChCl-urea-modified silica, the modified silica as a potential medium can be applied in some analytical technologies such as solid phase extraction, chromatography, and so on. PMID:24748453

  2. Denitrification incorporating microporous membranes

    SciTech Connect

    Reising, A.R.; Schroeder, E.D.

    1996-07-01

    A microbial system for removal of nitrate from drinking water in which the denitrification reactions are physically separated from the water being treated by a microporous membrane was studied. The experimental system was composed of two equal-volume cells separated by a 0.02 {mu}m pore size polytetrafluoroethylene membrane. No pressure difference existed across the membrane, and nitrate ions were transported through the membrane by diffusion. Results of experiments with biofilm denitrification and suspended-culture systems are presented. Deoxygenation by N{sub 2} stripping and by SO{sub 3}{sup {minus}2} produced equivalent results. Removal rates with the suspended culture systems were greater than those with biofilms. Effective membrane diffusivities calculated for suspended-culture systems were approximately the same as for sterile systems, indicating that resistance to transport was not changed by the addition of the suspended microbial culture. The methanol requirement observed in the experiments was 1.4 g total organic carbon (TOC) per g NO{sub 3}{sup {minus}}-N removed. Removal rates followed first-order pseudotransport controlled models for both the biofilm and suspended-culture systems. A prototype continuous-flow system is presented.

  3. Preparation and characterization of mesoporous silicas modified with chiral selectors as stationary phase for high-performance liquid chromatography.

    PubMed

    Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

    2014-01-15

    New hybrid materials were prepared as novel chiral stationary phases (CSPs) for high-performance liquid chromatography (HPLC). Pure mesoporous silica (SM) and ethylene-bridged periodic mesostructured organosilica (PMO) were functionalized, by a post-synthesis method, with derivates of erythromycin and vancomycin. N2 adsorption-desorption measurements, XRD, FT-IR, MAS NMR, SEM, TEM and elemental analysis were used to characterize the physico-chemical properties of these mesostructured materials, before and after the modification process. The synthesized particles had non-symmetrical 3-D wormhole-like mesostructure, spherical morphology, and a mean pore diameter between 53 and 59 Å. CSPs prepared were tested for the separation of four chiral β-blockers (atenolol, metoprolol, pindolol and propranolol) in normal phase (NP) and polar organic phase (PO) elution modes. Much stronger chiral interaction was observed in vancomycin-modified silicas. Results obtained in these preliminary studies will permit in future works to improve the synthesis route in order to design mesoporous materials with better performance as a chiral stationary phase for HPLC.

  4. Superhydrophobic Surfaces with Very Low Hysteresis Prepared by Aggregation of Silica Nanoparticles During In Situ Urea-Formaldehyde Polymerization.

    PubMed

    Diwan, Anubhav; Jensen, David S; Gupta, Vipul; Johnson, Brian I; Evans, Delwyn; Telford, Clive; Linford, Matthew R

    2015-12-01

    We present a new method for the preparation of superhydrophobic materials by in situ aggregation of silica nanoparticles on a surface during a urea-formaldehyde (UF) polymerization. This is a one-step process in which a two-tier topography is obtained. The polymerization is carried out for 30, 60, 120, 180, and 240 min on silicon shards. Silicon surfaces are sintered to remove the polymer. SEM and AFM show both an increase in the area covered by the nanoparticles and their aggregation with increasing polymerization time. Chemical vapor deposition of a fluorinated silane in the presence of a basic catalyst gives these surfaces hydrophobicity. Deposition of this low surface energy silane is confirmed by the F 1s signal in XPS. The surfaces show advancing water contact angles in excess of 160 degrees with very low hysteresis (< 7) after 120 min and 60 min polymerization times for 7 nm and 14 nm silica, respectively. Depositions are successfully demonstrated on glass substrates after they are primed with a UF polymer layer. Superhydrophobic surfaces can also be prepared on unsintered substrates.

  5. 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.

  6. 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.

  7. Catalyzed oxidative degradation of methyl orange over Au catalyst prepared by ionic liquid-polymer modified silica

    NASA Astrophysics Data System (ADS)

    Wang, Y.; Guo, J. S.

    2015-07-01

    A new type of hybrid material was prepared by grafting an ionic liquid monomer, 1-(p-vinylbenzyl)-3-methylimidazolium chloride, on the surface of the porous silica which was synthesized via sodium silicate hydrolysis. The as-synthesized products were characterized by scanning electron microscope, nitrogen physisorption experiment, thermogravimetric analysis and Fourier transform infrared spectra. A catalyst with Au was prepared using the hybrid material as carrier. The experimental results show that the catalyst exhibits a better catalytic effect of hydrogen peroxide on the degradation of methyl orange. The reason may be that the metal component of the catalyst facilitated the dissociation of hydrogen peroxide to produce abundant highly active free radicals which can rapidly ruin the structure of methyl orange molecules in water. Finally, a probable catalytic degradation mechanism based on diffusion was discussed.

  8. 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.

  9. Preparation of phosphorus-containing silica glass microspheres for radiotherapy of cancer by ion implantation.

    PubMed

    Kawashita, M; Miyaji, F; Kokubo, T; Suzuki, Y; Kajiyama, K

    1999-08-01

    A chemically durable glass microsphere containing a large amount of phosphorus is useful for in situ irradiation of cancers, since they can be activated to be a beta-emitter with a half-life of 14.3 d by neutron bombardment. When the activated microspheres are injected to the tumors, they can irradiate the tumors directly with beta-rays without irradiating neighboring normal tissues. In the present study, P+ ion was implanted into silica glass microspheres of 25 microm in average diameter at 50 keV with nominal doses of 2.5 x 10(16) and 3.35 x 10(1)6 cm(-2). The glass microspheres were put into a stainless container and the container was continuously shaken during the ion implantation so that P+ ion was implanted into them uniformly. The implanted phosphorus was localized in deep regions of the glass microsphere with the maximum concentration at about 50 nm depth without distributing up to the surface even for a nominal dose of 3.35 x 10(16) cm(-2). Both samples released phosphorus and silicon into water at 95 degrees C for 7 d. On the basis of the previous study on P+-implanted silica glass plates, the silica glass microspheres containing more phosphorus which is desired for actual treatment could be obtained, without losing high chemical durability, if P+ ion would be implanted at higher energy than 50 keV to be localized in deeper region.

  10. 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.

  11. Microporous carbon derived from polyaniline base as anode material for lithium ion secondary battery

    SciTech Connect

    Xiang, Xiaoxia; Liu, Enhui; Huang, Zhengzheng; Shen, Haijie; Tian, Yingying; Xiao, Chengyi; Yang, Jingjing; Mao, Zhaohui

    2011-08-15

    Highlights: {yields} Nitrogen-containing microporous carbon was prepared from polyaniline base by K{sub 2}CO{sub 3} activation, and used as anode material for lithium ion secondary battery. {yields} K{sub 2}CO{sub 3} activation promotes the formation of amorphous and microporous structure. {yields} High nitrogen content, and large surface area with micropores lead to strong intercalation between carbon and lithium ion, and thus improve the lithium storage capacity. -- Abstract: Microporous carbon with large surface area was prepared from polyaniline base using K{sub 2}CO{sub 3} as an activating agent. The physicochemical properties of the carbon were characterized by scanning electron microscope, X-ray diffraction, Brunauer-Emmett-Teller, elemental analyses and X-ray photoelectron spectroscopy measurement. The electrochemical properties of the microporous carbon as anode material in lithium ion secondary battery were evaluated. The first discharge capacity of the microporous carbon was 1108 mAh g{sup -1}, whose first charge capacity was 624 mAh g{sup -1}, with a coulombic efficiency of 56.3%. After 20 cycling tests, the microporous carbon retains a reversible capacity of 603 mAh g{sup -1} at a current density of 100 mA g{sup -1}. These results clearly demonstrated the potential role of microporous carbon as anode for high capacity lithium ion secondary battery.

  12. A highly crystalline microporous hybrid organic-inorganic aluminosilicate resembling the AFI-type zeolite.

    PubMed

    Bellussi, Giuseppe; Millini, Roberto; Montanari, Erica; Carati, Angela; Rizzo, Caterina; Parker, Wallace O; Cruciani, Giuseppe; de Angelis, Alberto; Bonoldi, Lucia; Zanardi, Stefano

    2012-07-28

    ECS-14, a crystalline microporous hybrid organic-inorganic aluminosilicate, has been synthesized by using 1,4-bis-(triethoxysilyl)-benzene (BTEB) as a source of silica. Its structure contains a system of linear channels with 12-membered ring openings, running along the [001] direction, resembling the pore architecture of the AFI framework type. PMID:22717682

  13. New insight into mesoporous silica for nano metal-organic framework.

    PubMed

    Kondo, Atsushi; Takanashi, Shinji; Maeda, Kazuyuki

    2012-10-15

    A micropore- and mesopore-integrated material was synthesized by using a mesoporous silica and a metal-organic framework (MOF). The composite was composed of nano MOF crystals and mesoporous silica showing high porosity based on the intrinsic micropores of MOF and mesopores of mesoporous silica and additional pore spaces that should be from the void between nano MOF crystals. The composite shows higher adsorption rate of ethanol at 303 K than that of the bulk MOF.

  14. Preparation of Biotubes with vascular cells component by in vivo incubation using adipose-derived stromal cell-exuding multi-microporous molds.

    PubMed

    Iwai, Ryosuke; Tsujinaka, Takahiro; Nakayama, Yasuhide

    2015-12-01

    Biotubes, prepared using in-body tissue architecture (IBTA) technology, have adequate mechanical properties and excellent biocompatibility for vascular grafts. However, they have thin walls, lack vascular constructing cells, and are composed of subcutaneous connective tissues consisting mainly of collagen and fibroblasts. This study aimed to prepare Biotubes with a vascular-like structure including an endothelial cell lining and a smooth muscle cell by IBTA using adipose-derived vascular stromal cell (ADSCs)-exuding specially designed multiporous tubes (outer diameter 5 mm, length 24 mm, pore size 500 μm, pore number 180, cell number/tube >3.0 × 10(6)). ADSCs were separated from rat subcutaneous fat, suspended in a Matrigel™ solution at 4 °C, and then filled into the tubes. After the tubes were embedded into dorsal subcutaneous pouches of the same rats for 2 weeks, robust Biotubes with a wall thickness of >600 μm were formed surrounding the tubes. The luminal layer of the obtained Biotubes was dominated by the cells positive for an endothelial marker. Almost the entire intima, with a thickness of about 400 μm, was occupied with cells positive for a smooth muscle marker. Both cells were derived from ADSCs. Biotube walls were constructed by fusing ADSC-derived vascular constructing cells exuded from the tubes and fibroblasts and collagen from the surrounding connective tissue. A robust Biotubes with vascular cells component, were formed after only 2 weeks of subcutaneous incubation of ADSCs-exuding multiporous tubes.

  15. Critical roles of cationic surfactants in the preparation of colloidal mesostructured silica nanoparticles: control of mesostructure, particle size, and dispersion.

    PubMed

    Yamada, Hironori; Urata, Chihiro; Higashitamori, Sayuri; Aoyama, Yuko; Yamauchi, Yusuke; Kuroda, Kazuyuki

    2014-03-12

    Mesoporous silica nanoparticles are promising materials for various applications, such as drug delivery and catalysis, but the functional roles of surfactants in the formation and preparation of mesostructured silica nanoparticles (MSN-as) remain to be seen. It was confirmed that the molar ratio of cationic surfactants to Si of alkoxysilanes (Surf/Si) can affect the degree of mesostructure formation (i.e., whether the mesochannels formed inside the nanoparticles actually pass through the outer surface of the particles), the particle diameter, and the dispersibility of MSN-as. Wormhole-like mesostructures formed with low Surf/Si ratios; however, the mesopores did not pass through the outer surface of the particles completely. At high Surf/Si ratios, the mesostructures extended. The particle diameter was 100 nm or larger at low Surf/Si ratios, and the primary particle diameter decreased as the Surf/Si ratio increased. This was because the surfactants enhanced the dispersity of the alkoxysilanes in water and the hydrolysis rate of the alkoxysilanes became faster, leading to an increased nucleation as compared to the particle growth. Moreover, primary particles aggregated at low Surf/Si ratios because of the hydrophobic interactions among the surfactants that were not involved in the mesostructure formation but were adsorbed onto the nanoparticles. At high Surf/Si ratios, the surfactant micelles were adsorbed on the surface of primary particles (admicelles), resulting in the dispersion of the particles due to electrostatic repulsion. In particular, molar ratios of 0.13 or higher were quite effective for the preparation of highly dispersed MSN-as. Surfactants played important roles in the mesostructure formation, decreasing the particle diameters, and the dispersibility of the particles. All of these factors were considerably affected by the Surf/Si ratio. The results suggested novel opportunities to control various colloidal mesostructured nanoparticles from the

  16. 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.

  17. 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.

  18. PS-b-PEO/Silica Films with Regular and Reverse Mesostructures of Large Characteristic Length Scales Prepared by Solvent Evaporation-Induced Self-Assembly

    SciTech Connect

    YU,KUI; BRINKER,C. JEFFREY; HURD,ALAN J.; EISENBERG,ADI

    2000-11-22

    Since the discovery of surfactant-templated silica by Mobil scientists in 1992, mesostructured silica has been synthesized in various forms including thin films, powders, particles, and fibers. In general, mesostructured silica has potential applications, such as in separation, catalysis, sensors, and fluidic microsystems. In respect to these potential applications, mesostructured silica in the form of thin films is perhaps one of the most promising candidates. The preparation of mesostructured silica films through preferential solvent evaporation-induced self-assembly (EISA) has recently received much attention in the laboratories. However, no amphiphile/silica films with reverse mesophases have ever been made through this EISA procedure. Furthermore, templates employed to date have been either surfactants or poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) triblock copolymers, such as pluronic P-123, both of which are water-soluble and alcohol-soluble. Due to their relatively low molecular weight, the templated silica films with mesoscopic order have been limited to relatively small characteristic length scales. In the present communication, the authors report a novel synthetic method to prepare mesostructured amphiphilic/silica films with regular and reverse mesophases of large characteristic length scales. This method involves evaporation-induced self-assembly (EISA) of amphiphilic polystyrene-block-poly(ethylene oxide) (PS-b-PEO) diblock copolymers. In the present study, the PS-b-PEO diblocks are denoted as, for example, PS(215)-b-PEO(100), showing that this particular sample contains 215 S repeat units and 100 EO repeat units. This PS(215)-b-PEO(100) diblock possesses high molecular weight and does not directly mix with water or alcohol. To the authors knowledge, no studies have reported the use of water-insoluble and alcohol-insoluble amphiphilic diblocks as structure-directing agents in the synthesis of mesostructured silica films through

  19. [Preparation and chromatographic performance of a silica-bonded (4-cyclopentadienyl benzoic acid-iron-toluene) hexafluorophosphoric acid stationary phase].

    PubMed

    Cao, Aijuan; Li, Xiaole; Qiao, Lijun; Zhou, Xiaohua; Yu, Ajuan; Zhang, Shusheng; Wu, Yangjie

    2016-02-01

    Based on the unique molecular structure of ferrocene and its potential as a new liquid chromatography separation medium, a new silica-bonded (4-cyclopentadienyl benzoic acid-iron-toluene) hexafluorophosphoric acid stationary phase was prepared. The structure of this new material was characterized by infrared spectroscopy, elemental analysis, thermogravimetric analysis et al. The chromatographic performance and retention mechanism of this new stationary phase were evaluated using different solute probes, including polycyclic aromatic hydrocarbons (PAHs), positional isomers of naphthylamine, positional isomers of nitro-aniline, nitroimidazoles, organic phosphorus et al. It could provide various action sites for different solutes in normal-phase chromatography such as π electron transfer, π-π electron interactions, dipole-dipole interactions, and electrostatic interactions with the substrates. And the possible separation mechanisms are discussed. PMID:27382719

  20. 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.

  1. [Preparation of 1 µm non-porous C18 silica gel stationary phase for chiral-pressurized capillary electrochromatography].

    PubMed

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

    2015-03-01

    Non-porous C18 silica gel stationary phase (1 µm) was prepared and applied to chiral separation in pressurized capillary electrochromatography (pCEC) for the enantioseparation of various basic compounds. The non-porous silica particles (1 µm) were synthesized using modified St6ber method. C18 stationary phase (1 µm) was prepared by immobilization of chloro-dimethyl-octadecylsilane. Using carboxymethyl-β-cyclodextrin (CM-β-CD) as the chiral additive, the pCEC conditions including the content of acetonitrile (ACN), concentration of buffer, pH, the concentration of chiral additive and flow rate as well as applied voltage were investigated to obtain the optimal pCEC conditions for the separation of four basic chiral compounds. The column provided an efficiency of up to 190,000 plates/m. Bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, and esmolol hydrochloride were baseline separated under the conditions of 5 mmol/L ammonium acetate buffer at pH 4. 0 with 20% (v/ v) acetonitrile, and 15 mmol/L CM-β-CD as the chiral additive. The applied voltage was 2 kV and flow rate was 0.03 mL/min with splitting ratio of 300:1. The resolution were 1.55, 2.82, 1. 69, 1. 70 for bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, esmolol hydrochloride, respectively. The C18 coverage was improved by repeating silylation method. The synthesized 1 µm C18 packings have better mechanical strength and longer service life because of the special, non-porous structure. The column used in pCEC mode showed better separation of the racemates and a higher rate compared with those used in the capillary liquid chromatography (cLC) mode. This study provided an alternative way for the method of pCEC enantioseparation with chiral additives in the mobile phase and demonstrated the feasibility of micron particle stationary phase in chiral separation. PMID:26182460

  2. Preparation and time-gated luminescence bioimaging applications of long wavelength-excited silica-encapsulated europium nanoparticles

    NASA Astrophysics Data System (ADS)

    Tian, Lu; Dai, Zhichao; Zhang, Lin; Zhang, Ruoyu; Ye, Zhiqiang; Wu, Jing; Jin, Dayong; Yuan, Jingli

    2012-05-01

    Silica-encapsulated luminescent lanthanide nanoparticles have shown great potential as biolabels for various time-gated luminescence bio-detections in recent years. The main problem of these nano-biolabels is their short excitation wavelengths within the UV region. In this work, a new type of silica-encapsulated luminescent europium nanoparticle, with a wide excitation range from UV to visible light in aqueous solutions, has been prepared using a conjugate of (3-isocyanatopropyl)triethoxysilane bound to a visible light-excited Eu3+ complex, 2,6-bis(1',1',1',2',2',3',3'-heptafluoro-4',6'-hexanedion-6'-yl)-dibenzothiophene-Eu3+-2-(N,N-diethylanilin-4-yl)-4,6-bis(pyrazol-1-yl)-1,3,5-triazine (IPTES-BHHD-Eu3+-BPT conjugate), as a functionalized precursor. The nanoparticles, which are prepared by the copolymerization of the IPTES-BHHD-Eu3+-BPT conjugate, tetraethyl orthosilicate and (3-aminopropyl)triethoxysilane in a water-in-oil reverse microemulsion consisting of Triton X-100, n-octanol, cyclohexane and water in the presence of aqueous ammonia, are monodisperse, spherical and uniform in size. Their diameter is 42 +/- 3 nm and they are strongly luminescent with a wide excitation range from UV to ~475 nm and a long luminescence lifetime of 346 μs. The nanoparticles were successfully used for streptavidin labeling and the time-gated luminescence imaging detection of two environmental pathogens, cryptosporidium muris and cryptosporidium parvium, in water samples. The results demonstrated the practical utility of the new nanoparticles as visible light-excited biolabels for time-gated luminescence bioassay applications.

  3. [Preparation of 1 µm non-porous C18 silica gel stationary phase for chiral-pressurized capillary electrochromatography].

    PubMed

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

    2015-03-01

    Non-porous C18 silica gel stationary phase (1 µm) was prepared and applied to chiral separation in pressurized capillary electrochromatography (pCEC) for the enantioseparation of various basic compounds. The non-porous silica particles (1 µm) were synthesized using modified St6ber method. C18 stationary phase (1 µm) was prepared by immobilization of chloro-dimethyl-octadecylsilane. Using carboxymethyl-β-cyclodextrin (CM-β-CD) as the chiral additive, the pCEC conditions including the content of acetonitrile (ACN), concentration of buffer, pH, the concentration of chiral additive and flow rate as well as applied voltage were investigated to obtain the optimal pCEC conditions for the separation of four basic chiral compounds. The column provided an efficiency of up to 190,000 plates/m. Bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, and esmolol hydrochloride were baseline separated under the conditions of 5 mmol/L ammonium acetate buffer at pH 4. 0 with 20% (v/ v) acetonitrile, and 15 mmol/L CM-β-CD as the chiral additive. The applied voltage was 2 kV and flow rate was 0.03 mL/min with splitting ratio of 300:1. The resolution were 1.55, 2.82, 1. 69, 1. 70 for bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, esmolol hydrochloride, respectively. The C18 coverage was improved by repeating silylation method. The synthesized 1 µm C18 packings have better mechanical strength and longer service life because of the special, non-porous structure. The column used in pCEC mode showed better separation of the racemates and a higher rate compared with those used in the capillary liquid chromatography (cLC) mode. This study provided an alternative way for the method of pCEC enantioseparation with chiral additives in the mobile phase and demonstrated the feasibility of micron particle stationary phase in chiral separation.

  4. [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. PMID:26983203

  5. Dexamethasone-loaded poly(ε-caprolactone)/silica nanoparticles composites prepared by supercritical CO2 foaming/mixing and deposition.

    PubMed

    de Matos, M B C; Piedade, A P; Alvarez-Lorenzo, C; Concheiro, A; Braga, M E M; de Sousa, H C

    2013-11-18

    A supercritical carbon dioxide (scCO2)-assisted foaming/mixing method (SFM) was implemented for preparing dexamethasone (DXMT)-loaded poly(ε-caprolactone)/silica nanoparticles (PCL/SNPs) composite materials suitable for bone regeneration. The composites were prepared from PCL and mesoporous SNPs (MCM-41/SBA-15) by means of scCO2-assisted SFM at several operational pressures, processing times and depressurization conditions. DXMT was loaded into SNPs (applying a scCO2 solvent impregnation/deposition method - SSID) and into PCL/SNPs composites (using the SFM method). The effects of the employed operational and compositional variables on the physicochemical and morphological features as well as in the in vitro release profiles of DXMT were analyzed in detail. This work demonstrates that the above-referred scCO2-based methods can be very useful for the preparation of DXMT-loaded PCL/SNPs composites with tunable physicochemical, thermomechanical, morphological and drug release properties and suitable for hard-tissue regeneration applications.

  6. 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.

  7. Lithography-assisted alignment control for preparation of mesoporous silica films with uniaxially oriented mesochannels.

    PubMed

    Yamauchi, Yusuke; Ishihara, Shinsuke; Suzuki, Norihiro; Wu, Kevin C W

    2014-03-01

    We report the lithography-assisted alignment control of one-dimensional (1D) mesochannels. The effectiveness on both nonionic and cationic surfactants is discussed, and a continuous film with fully uniaxially oriented mesochannels is also successfully prepared.

  8. A nanosized Ag-silica hybrid complex prepared by γ-irradiation activates the defense response in Arabidopsis

    NASA Astrophysics Data System (ADS)

    Chu, Hyosub; Kim, Hwa-Jung; Su Kim, Joong; Kim, Min-Soo; Yoon, Byung-Dae; Park, Hae-Jun; Kim, Cha Young

    2012-02-01

    Silver nanoparticles have antimicrobial activity against many pathogenic microbes. Here, the preparation of a nanosized Ag-silica hybrid complex (NSS) prepared by γ-irradiation is described. The effects of both NSS and reduced Ag nanoparticles (Ag 0) on the growth of the model plant Arabidopsis thaliana were tested. The application of 1-10 ppm NSS complex improved Arabidopsis growth in soil, whereas 100 ppm NSS resulted in weakly curled leaves. In addition, supplementation of Murashige and Skoog (MS) growth medium with 1 ppm NSS promoted the root growth of Arabidopsis seedlings, but root growth was inhibited by supplementation with 10 ppm NSS. To investigate whether the NSS complex could induce plant defense responses, the expression of pathogenesis-related ( PR) genes that are implicated in systemic acquired resistance (SAR) in Arabidopsis plants was examined. PR1, PR2 and PR5 were significantly up-regulated by each application of 10 ppm NSS complex or Ag 0 to the rosette leaves. Furthermore, pretreatment with the NSS complex induced more pathogen resistance to the virulent pathogen Pseudomonas syringae pv. tomato DC3000 ( Pst) compared to water treatment in Arabidopsis plants.

  9. 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.

  10. 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.

  11. One-step electrophoretic deposition for the preparation of superhydrophobic silica particle/trimethylsiloxysilicate composite coatings.

    PubMed

    Ogihara, Hitoshi; Katayama, Takafumi; Saji, Tetsuo

    2011-10-15

    SiO(2) particle/silicone resin (trimethylsiloxysilicate (TMSS)) composite coatings were prepared by electrophoretic deposition (EPD), and their wettability was examined. SiO(2) coatings prepared by EPD baths without TMSS were hydrophilic, while superhydrophobicity was observed for SiO(2)/TMSS composite coatings. IR spectra and EDS analyses revealed that not only SiO(2) particles but also TMSS electrophoretically moved toward a cathode; as a result, hydrophilic SiO(2) particles turned into superhydrophobic composite coatings by one-step EPD. SEM and AFM images of the superhydrophobic SiO(2)/TMSS composite coatings showed the presence of both nanometer- and micrometer-sized roughness in their surfaces. Particle size of SiO(2) had a great influence on the wettability of the composite coatings. The superhydrophobic SiO(2)/TMSS composite coatings showed excellent water repellency; they repelled running water continuously. In addition, by controlling the amount of deposited SiO(2) particles and TMSS, transparent superhydrophobic SiO(2)/TMSS composite coatings were prepared.

  12. Preparation of monodisperse polystyrene/silica core-shell nano-composite abrasive with controllable size and its chemical mechanical polishing performance on copper

    NASA Astrophysics Data System (ADS)

    Zhang, Lei; Wang, Haibo; Zhang, Zefang; Qin, Fei; Liu, Weili; Song, Zhitang

    2011-11-01

    Monodisperse silica-coated polystyrene (PS) nano-composite abrasives with controllable size were prepared via a two-step process. Monodisperse positively charged PS colloids were synthesized via polymerization of styrene by using a cationic initiator. In the subsequent coating process, silica formed shell on the surfaces of core PS particles via the ammonia-catalyzed hydrolysis and condensation of tetraethoxysilane. Neither centrifugation/water wash/redispersion cycle process nor surface modification or addition surfactant was needed in the whole process. The morphology of the abrasives was characterized by scanning electron microscope. Transmission electron microscope and energy dispersive X-ray analysis results indicated that silica layer was successfully coated onto the surfaces of PS particles. Composite abrasive has a core-shell structure and smooth surface. The chemical mechanical polishing performances of the composite abrasive and conventional colloidal silica abrasive on blanket copper wafers were investigated. The root mean square roughness decreases from 4.27 nm to 0.56 nm using composite abrasive. The PS/SiO2 core-shell composite abrasives exhibited little higher material removal rate than silica abrasives.

  13. 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.

  14. Preparation and Acid Catalytic Activity of TiO2 Grafted Silica MCM-41 with Sulfate Treatment

    NASA Astrophysics Data System (ADS)

    Guo, Dai-shi; Ma, Zi-feng; Yin, Chun-sheng; Jiang, Qi-zhong

    2008-02-01

    TiO2 grafted silica MCM-41 catalyst with and without sulfate treatment were prepared. The structural and acid properties of these materials were investigated by XRD, N2 adsorption-desorption, element analysis, thermal analysis, Raman and FTIR measurements. Their acid-catalytic activities were evaluated using the cyclization reaction of pseudoionone. It was found that the obtained materials possess well-ordered mesostructure, and the grafted TiO2 components were in highly dispersed amorphous form. T/MCM41 without sulfation contained only Lewis acid sites, while Brønsted and Lewis acidities were remarkably improved for the sulfated materials ST/MCM41 and d-ST/MCM41. T/MCM-41 was not active for the cyclization reaction of pseudoionone, but ST/MCM-41 and d-ST/MCM-41 possessed favorable catalytic activities. The catalytic performance of ST/MCM-41 was comparable with that of the commercial solid acid catalyst of Amberlyst-15, and better than that of d-ST/MCM-41, although the latter underwent a second TiO2 grafting process and accordingly had higher Ti and S content. The specific surface structure of Si-O-Ti-O-S=O in ST/MCM-41 and the bilateral induction effect of Si and S=O on Si-O-Ti bonds were speculated to account for its higher acid catalytic activity.

  15. 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. PMID:25890438

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

    PubMed

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

    2013-01-25

    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. PMID:23263661

  17. 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.

  18. 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.

  19. 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.

  20. Studies of the factors effecting the preparation of heterogeneous platinum-based catalyst on silica supports

    SciTech Connect

    Kim, Chang Young; Jung, Chi-Young; Jung, Jae-Woong; Jeong, Sung Hoon; Yi, Sung-Chul; Kim, Wha Jung

    2010-10-15

    Pt nanoparticles with an average size of {approx}3 nm were successfully immobilized on the surface of SiO{sub 2} functionalized with -NH{sub 2} and -SH groups through chemical reduction process using polyvinylpyrrolidone as a stabilizer and different reducing agents. The effects of molecular weight of polyvinylpyrrolidone, molar ratio of reducing agent to Pt salt, type of reducing agent on the size and degree of agglomeration of Pt nanoparticles on the SiO{sub 2} surface were investigated. The X-ray diffraction and transmission electron micrograph analyses were performed to identify the product phase, size and morphology of immobilized Pt onto SiO{sub 2}. UV-vis analysis was also conducted to identify the degree of reduction of Pt ions. The Pt-SiO{sub 2} nanocomposite prepared from both NH{sub 2}- and SH-functionalized SiO{sub 2} exhibited similar behavior. The number of immobilized Pt nanoparticles and their average size was increased with polyvinylpyrrolidone concentration while the number of immobilized Pt was decreased with its molecular weight.

  1. Preparation and characterization of ultrathin dual-layer ionic liquid lubrication film assembled on silica surfaces.

    PubMed

    Pu, Jibin; Wang, Liping; Mo, Yufei; Xue, Qunji

    2011-02-15

    A novel ultrathin dual-layer film, which contained both bonded and mobile phases in ionic liquids (ILs) layer, was fabricated successfully on a silicon substrate modified by a self-assembled monolayer (SAM). The formation and surface properties of the films were analyzed using ellipsometer, water contact angle meter, attenuated total reflectance Fourier transform infrared spectroscopy, multi-functional X-ray photoelectron spectroscopy, and atomic force microscope. Meanwhile, the adhesive and nanotribological behaviors of the films were evaluated by a homemade colloidal probe. A ball-on-plate tribometer was used to evaluate the microtribological performances of the films. Compared with the single-layer ILs film deposited directly on the silicon surface, the as-prepared dual-layer film shows the improved tribological properties, which is attributed to the special chemical structure and outstanding physical properties of the dual-layer film, i.e., the strong adhesion between bonded phase of ILs and silicon substrate via the chemical bonding with SAM, the interlinked hydrogen bonds among the molecules, and two-phase structure composed of steady bonded phase with load-carrying capacity and flowable mobile phase with self-replenishment property. PMID:21111428

  2. [The delivery mechanism of micro-porous osmotic pump tablets].

    PubMed

    Zhao, Xue-ling; Li, Qiang; Gong, Xian-feng; Li, San-ming

    2007-02-01

    To investigate the delivery mechanism of micro-porous osmotic pump tablets ( MPOP), taking tramadol hydrochloride ( TR) as the model drug, tramadol hydrochloride micro-porous osmotic pump tablets (TR MPOP) were prepared with compressible starch as diluent, cellulose acetate as coating material, polyethylene glycol 400 as pore-forming agents. The equilibrium solubility and osmolality of TR were determined. The effects of fillers in tablet cores, coating levels, and osmotic pressures of release media on expansion behavior of preparations were described. The influences of the category, osmolality, and pH value of release media, release methods, and release conditions on release curves of tablets were evaluated. Based on several models, the delivery pattern of TR MPOP was fitted. The equilibrium solubility in water and osmolality of TR were (775.8 +/- 17.7) g x L(-1) and 4.036 Osmol x kg(-1), respectively. During the drug-release period, it was observed that the tablets expanded markedly in response to the expansion characteristics of compressible starch and the osmotic pressure difference across the membrane. When osmotic pressure of release media increased, the significant change of the equilibrium solubility of TR was not found, but the release rates of TR MPOP decreased significantly. The delivery rate was not influenced by the pH of release mediums, dissolution methods and paddle stirring rates. The drug release profile conformed to the model of zero order in 8 h. The pore-forming agents were dissolved in release medium, which caused micro-pores. The expansion of tablets made the size of micropores bigger, and then the drug-releasing pores were obtained. It was proved that the drivers of drug delivering from TR MPOP were mainly the difference of osmotic pressure, and secondly the difference of solubility. TR MPOP were the controlled-release preparation.

  3. 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).

  4. 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

  5. Microporous Co@CoO nanoparticles with superior microwave absorption properties.

    PubMed

    Liu, Tong; Pang, Yu; Zhu, Mu; Kobayashi, Satoru

    2014-02-21

    Nanoporous metal materials with many potential applications have been synthesized by a chemical dealloying approach. The fabrication of nanoporous metal nanoparticles (NPs), however, is still challenging due to the difficulties in producing suitable nanoscale precursors. Herein, nanoporous Co NPs of 31 nm have been successfully prepared by dealloying Co-Al NPs, and surprisingly they possess micropores in a range from 0.7 to 1.7 nm and a large surface area of 50 m(2) g(-1). The crystalline size of the microporous NPs is 2-5 nm. Through the passivation process, the microporous Co NPs covered with CoO (Co@CoO) are generated as a result of the surface oxidation of Co. They exhibit better microwave absorption properties than their nonporous counterpart. An enhanced reflection loss (RL) value of -90.2 dB is obtained for the microporous Co@CoO NPs with a thickness of merely 1.3 mm. The absorption bandwidth corresponding to the RL below -10 dB reaches 7.2 GHz. The microwave absorption mechanism is discussed in terms of micropore morphology, core@shell structure and nanostructure. This novel microporous material may open new routes for designing high performance microwave absorbers.

  6. 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.

  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. PMID:26287395

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

    PubMed

    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 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

  11. 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

  12. Stability of amorphous silica-alumina in hot liquid water.

    PubMed

    Hahn, Maximilian W; Copeland, John R; van Pelt, Adam H; Sievers, Carsten

    2013-12-01

    Herein, the hydrothermal stability of amorphous silica-alumina (ASA) is investigated under conditions relevant for the catalytic conversion of biomass, namely in liquid water at 200 °C. The hydrothermal stability of ASA is much higher than that of pure silica or alumina. Interestingly, the synthetic procedure used plays a major role in its resultant stability: ASA prepared by cogelation (CG) lost its microporous structure, owing to hydrolysis of the siloxane bonds, but the resulting mesoporous material still had a considerable surface area. ASA prepared by deposition precipitation (DP) contained a silicon-rich core and an aluminum-rich shell. In hot liquid water, the latter structure was transformed into a layer of amorphous boehmite, which protected the particle from further hydrolysis. The surface area showed relatively minor changes during the transformation. Independent of the synthetic method used, the ASAs retained a considerable concentration of acid sites. The concentration of acid sites qualitatively followed the changes in surface area, but the changes were less pronounced. The performance of different ASAs for the hydrolysis of cellobiose into glucose is compared. PMID:24124062

  13. Preparation of silica-supported porous sorbent for heavy metal ions removal in wastewater treatment by organic-inorganic hybridization combined with sucrose and polyethylene glycol imprinting.

    PubMed

    Li, Feng; Du, Ping; Chen, Wei; Zhang, Shusheng

    2007-03-01

    A new porous sorbent for wastewater treatment of metal ions was synthesized by covalent grafting of molecularly imprinted organic-inorganic hybrid on silica gel. With sucrose and polyethylene glycol 4000 (PEG 4000) being synergic imprinting molecules, covalent surface coating on silica gel was achieved by using polysaccharide-incorporated sol-gel process starting from the functional biopolymer, chitosan and an inorganic epoxy-precursor, gamma-glycidoxypropyltrimethoxysiloxane (GPTMS) at room temperature. The prepared porous sorbent was characterized by using simultaneous thermogravimetry and differential scanning calorimeter (TG/DSC), scanning electron microscopy (SEM), nitrogen adsorption porosimetry measurement and X-ray diffraction (XRD). Copper ion, Cu(2+), was chosen as the model metal ion to evaluate the effectiveness of the new biosorbent in wastewater treatment. The influence of epoxy-siloxane dose, buffer pH and co-existed ions on Cu(2+) adsorption was assessed through batch experiments. The imprinted composite sorbent offered a fast kinetics for the adsorption of Cu(2+). The uptake capacity of the sorbent imprinted by two pore-building components was higher than those imprinted with only a single component. The dynamic adsorption in column underwent a good elimination of Cu(2+) in treating electric plating wastewater. The prepared composite sorbent exhibited high reusability. Easy preparation of the described porous composite sorbent, absence of organic solvents, cost-effectiveness and high stability make this approach attractive in biosorption. PMID:17386667

  14. Preparation of a nitro-substituted tris(indolyl)methane modified silica in deep eutectic solvents for solid-phase extraction of organic acids.

    PubMed

    Wang, Na; Wang, Jiamin; Liao, Yuan; Shao, Shijun

    2016-05-01

    A new sorbent for solid-phase extraction was synthesized by chemical immobilization of nitro-substituted tris(indolyl)methane on silica in new and green deep eutectic solvents. Elemental analysis results indicated that deep eutectic solvents could be an alternative to the traditional solvents in preparing nitro-substituted tris(indolyl)methane modified silica. Coupled with high performance liquid chromatography, the extraction performance of the sorbent was evaluated by using four organic acids as model analytes. The rebinding experiments results showed that the nitro-substituted tris(indolyl)methane modified silica sorbent had a good adsorption capacity towards the selected organic acids. Under the appropriate experimental conditions, good precision and wide linear ranges with coefficient of determination (R(2)) of higher than 0.9957 were obtained, and the limits of detection were in the range of 0.50-2.0μgL(-1) for the organic acids tested. The developed solid-phase extraction-high performance liquid chromatography-diode array detection (SPE-HPLC-DAD) method was successfully applied for the determination of organic acids in two drinking samples with recoveries ranging from 76.7% to 110.0% and 67.7% to 104.0% for all the selected organic acids, respectively.

  15. 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.

  16. Interactions of silica surfaces

    SciTech Connect

    Vigil, G.; Xu, Z.; Steinberg, S.; Israelachvili, J. . Dept. of Chemical and Nuclear Engineering and Materials Dept.)

    1994-07-01

    Adhesion, friction, and colloidal forces in air and aqueous salt solutions have been measured between various silica surfaces prepared by depositing amorphous but highly smooth silica films on mica. The results show four interesting and interrelated phenomena: (i) the adhesion of silica surfaces in air increases slowly with contact time, especially in humid air where the contacting surfaces become separated by an [approximately]20-[angstrom]-thick layer of hydrated silica or silica gel; (ii) the friction of two silica surfaces exhibits large sticking or stiction spikes, whose magnitude increases in the presence of water and when the surfaces are kept in contact longer before sliding; (iii) the non-DLVO repulsion commonly seen at short range (<40 A) between silica surfaces immersed in aqueous solutions is monotonically repulsive, with no oscillatory component, and is quite unlike theoretical expectations and previous measurements of forces due to solvent structure; (iv) dynamic contact angle measurements reveal time-dependent effects which cannot be due to a fixed surface chemical heterogeneity or roughness. The results indicate that silica surfaces undergo slow structural and chemical changes during interactions with water and with each other. More specifically, the authors propose that the unusual interfacial and colloidal properties of silica are due, not to hydration effects, but to the presence of an [approximately]10-[angstrom]-thick gel-like layer of protruding silanol and silicilic acid groups that grow on the surfaces in the presence of water. These protruding groups react chemically (sinter) with similar groups located on an opposing surface and give rise to the unusual time-dependent adhesion, friction, and non-DLVO forces observed. The proposed mechanism in terms of a surface layer of silica gel is consistent with the known surface chemistry of silica and accounts for the results reported and for other unusual surface and colloidal properties of silica.

  17. Size and spacial distribution of micropores in SBA-15 using CM-SANS

    SciTech Connect

    Pollock, Rachel A; Walsh, Brenna R; Fry, Jason A; Ghampson, Tyrone; Centikol, Ozgul; Melnichenko, Yuri B; Kaiser, Helmut; Pynn, Roger; Frederick, Brian G

    2011-01-01

    Diffraction intensity analysis of small-angle neutron scattering measurements of dry SBA-15 have been combined with nonlocal density functional theory (NLDFT) analysis of nitrogen desorption isotherms to characterize the micropore, secondary mesopore, and primary mesopore structure. The radial dependence of the scattering length density, which is sensitive to isolated surface hydroxyls, can only be modeled if the NLDFT pore size distribution is distributed relatively uniformly throughout the silica framework, not localized in a 'corona' around the primary mesopores. Contrast matching-small angle neutron scattering (CM-SANS) measurements, using water, decane, tributylamine, cyclohexane, and isooctane as direct probes of the size of micropores indicate that the smallest pores in SBA-15 have diameter between 5.7 and 6.2 {angstrom}. Correlation of the minimum pore size with the onset of the micropore size distribution provides direct evidence that the shape of the smallest micropores is cylinderlike, which is consistent with their being due to unraveling of the polymer template.

  18. 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).

  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. 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

    2015-12-01

    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.

  1. 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.

  2. 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.

  3. Mesoporous polymer networks-ultraporous DVB resins by hard-templating of close-packed silica spheres.

    PubMed

    Wilke, Antje; Weber, Jens

    2012-05-14

    The preparation of ultraporous polymer resins using a straightforward hard-templating synthesis is presented. Self-assembly of silica nanospheres into densely packed glasses allows an easy preparation of templates. Polydivinylbenzene resins with surface areas of up to 1000 m(2) g(-1) are synthesized as a model system and porosity analysis reveals bimodal porosity (spherical mesopores and micropores within the pore walls). The prepared systems can be further functionalized without loss of porosity as demonstrated by sulfonation. Because of their large pore sizes (13-28 nm), they are efficient adsorbents also for large molecules. Finally, the systems can also be used as model systems for the study of the pore drying and collapse process, which is of crucial importance for any application of mesoporous polymers.

  4. 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.

  5. 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. PMID:27240738

  6. Random lasing of microporous surface of Cr2+:ZnSe crystal induced by femtosecond laser

    NASA Astrophysics Data System (ADS)

    Yang, Xianheng; Feng, Guoying; Yao, Ke; Yi, Jiayu; Zhang, Hong; Zhou, Shouhuan

    2015-06-01

    We demonstrate a random lasing emission based on microporous surface of Cr2+:ZnSe crystal prepared by femtosecond pulsed laser ablation in high vacuum (below 5 × 10-4 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 Cr2+: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 Cr2+: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 Cr2+:ZnSe crystal. The peak position of excitation spectra is almost identical to the strongest absorption wavelength.

  7. 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.

  8. 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.

  9. Fabrication of silica-decorated graphene oxide nanohybrids and the properties of composite epoxy coatings research

    NASA Astrophysics Data System (ADS)

    Ma, Yu; Di, Haihui; Yu, Zongxue; Liang, Ling; Lv, Liang; Pan, Yang; Zhang, Yangyong; Yin, Di

    2016-01-01

    With the purpose of preparing anticorrosive coatings, solvent-based epoxy resins often serve as raw material. Unfortunately, plentiful micro-pores are fabricated via solvent evaporation in the resin' curing process, which is an intrinsic shortcoming and it is thus necessary to obstacle their micro-pore for enhancing antiseptic property. To reduce the intrinsic defect and increase the corrosion resistance of coating, we synthesize a series of SiO2-GO hybrids through anchoring silica (SiO2) on graphene oxide (GO) sheets with the help of 3-aminopropyltriethoxysilane and 3-glycidoxypropyltrimethoxysilane, and disperse the hybrids into epoxy resin at a low weight fraction of 2%. Furthermore, we investigate the appropriate preparation proportion of SiO2-GO hybrids (namely: SiO2-GO (1:5)). The electrochemical impedance spectroscopy (EIS) test and coatings' morphology monitoring in corrosion process reveal that the anticorrosive performance of epoxy coatings is significantly enhanced by incorporation of SiO2-GO (1:5) hybrids to epoxy compared with neat epoxy and other nanofillers including SiO2 or GO at the same contents. The superiority of the SiO2-GO (1:5) hybrids is related to their excellent dispersion in resin and sheet-like structure.

  10. 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

  11. An Elastic Monolithic Catalyst: A Microporous Metalloporphyrin-Containing Framework-Wrapped Melamine Foam for Process-Intensified Acyl Transfer.

    PubMed

    Wu, Keyi; Guo, Jia; Wang, Changchun

    2016-05-10

    The advent of conjugated microporous polymers (CMPs) has had significant impact in catalysis. However, the presence of only micropores in these polymers often imposes diffusion limitations, which has resulted in the low utilization of CMPs in catalytic reactions. Herein, the preparation of a foam-supporting CMP composite with interconnective micropores and macropores and elastic properties is reported. Metalloporphyrin-based CMP organogels are synthesized within the melamine foam by a room-temperature oxidative homocoupling reaction of terminal alkynes. Upon drying, the CMP-based xerogels tightly wrap the framework skeletons of the foam, while the foam cells are still open to allow for the preservation of elasticity and macroporosity. Such a hierarchical structure is efficient for acyl transfer, facilitates substrate diffusion within interpenetrative macropores and micropores, and could be used to intensify catalytic processes.

  12. 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.

  13. Preparation of sandwich-structured graphene/mesoporous silica composites with C8-modified pore wall for highly efficient selective enrichment of endogenous peptides for mass spectrometry analysis.

    PubMed

    Yin, Peng; Wang, Yuhua; Li, Yan; Deng, Chunhui; Zhang, Xiangmin; Yang, Pengyuan

    2012-09-01

    In this study, sandwich-structured graphene/mesoporous silica composites (C8-modified graphene@mSiO(2)) were synthesized by coating mesoporous silica onto hydrophilic graphene nanosheets through a surfactant-mediated cocondensation sol-gel process. The newly prepared C8-modified graphene@mSiO(2) nanocomposites possess unique properties of extended plate-like morphology, good water dispersibility, highly open pore structure, uniform pore size (2.8 nm), high surface area (632 m(2)/g), and C8-modified-interior pore walls. The unique structure of the C8-modified graphene@mSiO(2) composite nanosheets not only provide extended planes with hydrophilic surface that prevents aggregation in solution, but also offer a huge number of C8-modified mesopores with high surface area that can ensure an efficient adsorption of peptides through hydrophobic-hydrophobic interaction between C8-moified pore walls and target molecules. The obtained C8-modified graphene@mSiO(2) materials were utilized for size selectively and specifically enriching peptides in standard peptide mixtures and endogenous peptides in real biological samples (mouse brain tissue). PMID:22837154

  14. 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

    2013-11-01

    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.

  15. 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.

  16. 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. PMID:25990895

  17. Characterization and acidic properties of Al-SBA-15 materials prepared by post-synthesis alumination of a low-cost ordered mesoporous silica

    NASA Astrophysics Data System (ADS)

    Gómez-Cazalilla, M.; Mérida-Robles, J. M.; Gurbani, A.; Rodríguez-Castellón, E.; Jiménez-López, A.

    2007-03-01

    A series of Al-containing SBA-15 type materials with different Si/Al ratio, were prepared by post-synthesis modification of a pure highly ordered mesoporous silica SBA-15 obtained by using sodium silicate as silica source, and amphiphilic block copolymer as structure-directing agent. A high level of aluminum incorporation was achieved, reaching an Si/Al ratio of up to 5.5, without any significant loss in the textural properties of SBA-15. These materials were fully characterized by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), 27Al NMR spectroscopy, and N 2 adsorption at 77 K. The acid properties of these materials have been evaluated by NH 3-TPD, adsorption of pyridine and deuterated acetonitrile coupled to FTIR spectroscopy. The effective acidity of these materials was evaluated using two catalytic reactions: 2-propanol dehydrogenation and 1-butene isomerization. The adsorption of basic probe molecules and the catalytic behavior revealed an evolution of the acid properties with the Al content. These studies have shown that the Al-SBA-15 materials contain Brønsted and Lewis acid sites with medium acidity which makes them appropriate to be used as acid catalysts in heterogeneous catalysis, catalytic supports, and adsorbents.

  18. 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.

  19. Preparation and SO{sub 2} sorption/desorption behavior of an Ionic liquid supported on porous silica particles

    SciTech Connect

    Zhang, Z.M.; Wu, L.B.; Dong, J.; Li, B.G.; Zhu, S.P.

    2009-02-15

    The ionic liquid 1,1,3,3-tetramethylguanidinium lactate (TMGL) was supported onto porous silica particles via a facile impregnation-vaporization method. The TMGL-supported particles gave high porosity and large specific surface area. The SO{sub 2} sorption/desorption properties of the silica-supported TMGL (TMGL-SiO{sub 2}) were evaluated, and high SO{sub 2} sorption capacity and rate were achieved. Its capacity reached 0.6 g SO{sub 2}/g TMGL in 15-30 min with pure SO{sub 2} gas and 0.15 g SO{sub 2}/g TMGL in 17 h with a N{sub 2}/SO{sub 2} mixture gas that contained 2160 ppm SO{sub 2}. The SO{sub 2} concentration was reduced to 12.6 ppm after sorption. The TMGL-SiO{sub 2} system could be reused for many sorption/desorption cycles without change in its capacity. It was also characterized by good mechanical strength and thermal stability at temperature up to 130{sup o}C. The SO{sub 2} sorbent system appears to be useful in gas desulfurization.

  20. Preparation of silica-magnetite nanoparticle mixed hemimicelle sorbents for extraction of several typical phenolic compounds from environmental water samples.

    PubMed

    Zhao, Xiaoli; Shi, Yali; Wang, Thanh; Cai, Yaqi; Jiang, Guibin

    2008-04-25

    A novel type of superparamagnetic silica-coated (Fe3O4/SiO2 core/shell) magnetite nanoparticle modified by surfactants has been successfully synthesized and was applied as an effective sorbent material for the pre-concentration of several typical phenolic compounds (bisphenol A (BPA), 4-tert-octylphenol (4-OP) and 4-n-nonylphenol (4-NP)) from environmental water samples. Compared with pure magnetic particles, a thin and dense silica layer would protect the iron oxide core from leaching out in acidic conditions. In order to enhance their adsorptive tendency towards organic compounds, cetylpyridinium chloride (CPC) or cetyltrimethylammonium bromide (CTAB) were added, which adsorbed on the surface of the Fe3O4/SiO2 nanoparticles (Fe3O4/SiO2 NPs) and formed mixed hemimicelles. Main factors affecting the adsolubilization of analytes were optimized and comparative study on the use of CPC and CTAB-coated Fe3O4/SiO2 NPs mixed hemimicelles-based SPE was also carried out. CPC-coated Fe3O4/SiO2 NPs system was selected due to lower elution volume required and more effective adsorption of the target compounds. Under selected conditions, concentration factor of 1600 was achieved by using this method to extract 800 mL of different environmental water samples. The detection limits obtained for BPA, 4-OP and 4-NP with HPLC-FLD were 7, 14, and 20 ng/L, respectively.

  1. Optical models for the characterization of silica nanosphere monolayers prepared by the Langmuir-Blodgett method using ellipsometry in the quasistatic regime.

    PubMed

    Kozma, Peter; Fodor, Balint; Deak, Andras; Petrik, Peter

    2010-10-19

    We investigated different optical models (one-layer, multilayer, parametric multilayer, and statistical parametric) for the ellipsometric characterization of thin films made of silica spheres in the diameter (D) range of 90-450 nm prepared by the Langmuir-Blodgett (LB) technique. As a continuation of a previous work (Nagy, N., et al. Langmuir 2006, 22, 8416) in terms of threshold wavelength determination and optical models, we investigated the wavelength range of the quasistatic limit (requirement for the effective medium approximation) depending onD.We compared the above models in the aspect of fit quality, stability, uncertainty of parameters, and the amount of information that can be obtained from the evaluation. Besides fundamental properties like diameter, coverage, or packing density, using sophisticated models we can also determine the size distribution of the particles. The ellipsometric results were compared with the results of dynamic light scattering and of scanning electron microscopy.

  2. XAFS Study on Nano-Sized Metal Catalyst Prepared by a Photo-Assisted Deposition Using Ti-Containing Mesoporous Silica Thin Film Photocatalyst

    SciTech Connect

    Shimada, Makoto; Nishio, Shinichiro; Shimizu, Toshiaki; Mori, Kohsuke; Ohmichi, Tetsutaro; Katayama, Iwao; Yamashita, Hiromi

    2007-02-02

    Transparent Ti-containing mesoporous silica (TMS) thin films can be prepared on quartz plates using the spin-coating sol-gel method. These thin films have performed super-hydrophilic surface property. Using a photo-assisted deposition (PAD) method, nano-sized Pt metal can be highly deposited on TMS thin films under UV-light irradiation. XAFS measurement indicates that TMS thin films contain isolated and tetrahedrally coordinated Ti-oxide moieties in the frameworks and nano-sized Pt particles can be highly deposited on the photo-excited Ti species in TMS thin films. Measurement of contact angle of droplet water showed that the surface property of Pt/TMS thin film is also hydrophilic as comparable to that of original TMS thin film.

  3. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Filters, microporous polymeric. 177.2250 Section... as Components of Articles Intended for Repeated Use § 177.2250 Filters, microporous polymeric. Microporous polymeric filters identified in paragraph (a) of this section may be safely used, subject to...

  4. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Filters, microporous polymeric. 177.2250 Section... as Components of Articles Intended for Repeated Use § 177.2250 Filters, microporous polymeric. Microporous polymeric filters identified in paragraph (a) of this section may be safely used, subject to...

  5. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Filters, microporous polymeric. 177.2250 Section... as Components of Articles Intended for Repeated Use § 177.2250 Filters, microporous polymeric. Microporous polymeric filters identified in paragraph (a) of this section may be safely used, subject to...

  6. 21 CFR 177.2250 - Filters, microporous polymeric.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Filters, microporous polymeric. 177.2250 Section... as Components of Articles Intended for Repeated Use § 177.2250 Filters, microporous polymeric. Microporous polymeric filters identified in paragraph (a) of this section may be safely used, subject to...

  7. 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.

  8. Effect of the preparation method on the thermal stability of silica-supported nickel oxide as studied by EXAFS and TPR techniques

    SciTech Connect

    Clause, O. ); Bonneviot, L.; Che, M. )

    1992-11-01

    EXAFS analysis and Temperature-Programmed Reduction experiments (TPR) have been carried out on calcined Ni/SiO[sub 2] materials prepared by incipient wetness impregnation at different pH values, ion exchange with ammonia and ethylenediamine solutions, and deposition-precipitation. The interaction of the Ni(II) ions with silica is shown to be dependent on the first steps of catalyst preparation, i.e., deposition, washing, and drying. Silicates with a layer structure are formed in samples prepared by deposition-precipitation and ion exchange from ammoniacal solutions. Silicate formation inhibits the NiO crystallization up to 500[degrees]C. The silicate decomposition is favored when the thermal treatment is performed under reduced pressure. The reducibility of the nickel oxide phase resulting from silicate decomposition is strongly hindered in comparison with that of unsupported nickel oxide. The silicate formation is avoided using a strong chelating ligand such as ethylenediamine during ion exchange. With ethylenediamine, isolated Ni(II) species stable to 500[degrees]C are obtained. 35 refs., 10 figs., 2 tabs.

  9. 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.

  10. Factors affecting the preparation and properties of electrodeposited silica thin films functionalized with amine or thiol groups.

    PubMed

    Sibottier, Emilie; Sayen, Stéphanie; Gaboriaud, Fabien; Walcarius, Alain

    2006-09-26

    Well-adherent sol-gel-derived silica films functionalized with amine or thiol groups have been electrogenerated on gold electrodes and both the deposition process and the film properties have been studied by various physicochemical techniques. Electrodeposition was achieved by combining the formation of a self-assembled "nanoglue" on the electrode surface, the sol-gel process, and the electrochemical manipulation of pH to catalyze polycondensation of the precursors. Gold electrodes pretreated with mercaptopropyltrimethoxysilane (MPTMS) were immersed in sol solutions containing the selected precursors (tetraethoxysilane, TEOS, in mixture with (3-aminopropyl)triethoxysilane, APTES, or MPTMS) where they underwent a cathodic electrolysis to generate the hydroxyl ions that are necessary to catalyze the formation of the organosilica films on the electrode surface. Special attention was given to analyze the effects of deposition time and applied potential and to compare APTES and MPTMS films. Characterization was made using quartz crystal microbalance, scanning electron microscopy, cyclic voltammetry, and atomic force microscopy (including in situ monitoring). The electrodeposition process was found to occur at two growing rates: a first slow stage giving rise to rather homogeneous, yet rough, films with thickness in the sub-mum range (increasing continuously when increasing the deposition time), which was followed by a faster gelification step resulting in much thicker (>1 microm) and rougher macroporous deposits. These two successive situations were observed independently on the applied potential except that more cathodic values led to narrower sub-microm ranges (as expected from the larger amounts of the electrogenerated hydroxyl catalyst). Thiol-functionalized silica films were deposited more rapidly than the amine ones and, for both of them, permeability to redox probe was found to decrease when increasing the film thickness because of higher resistance to mass

  11. Synthesis and characterization of high-surface-area millimeter-sized silica beads with hierarchical multi-modal pore structure by the addition of agar

    SciTech Connect

    Han, Yosep; Choi, Junhyun; Tong, Meiping; Kim, Hyunjung

    2014-04-01

    Millimeter-sized spherical silica foams (SSFs) with hierarchical multi-modal pore structure featuring high specific surface area and ordered mesoporous frameworks were successfully prepared using aqueous agar addition, foaming and drop-in-oil processes. The pore-related properties of the prepared spherical silica (SSs) and SSFs were systematically characterized by field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), small-angle X-ray diffraction (SAXRD), Hg intrusion porosimetry, and N{sub 2} adsorption–desorption isotherm measurements. Improvements in the BET surface area and total pore volume were observed at 504 m{sup 2} g{sup −1} and 5.45 cm{sup 3} g{sup −1}, respectively, after an agar addition and foaming process. Despite the increase in the BET surface area, the mesopore wall thickness and the pore size of the mesopores generated from the block copolymer with agar addition were unchanged based on the SAXRD, TEM, and BJH methods. The SSFs prepared in the present study were confirmed to have improved BET surface area and micropore volume through the agar loading, and to exhibit interconnected 3-dimensional network macropore structure leading to the enhancement of total porosity and BET surface area via the foaming process. - Highlights: • Millimeter-sized spherical silica foams (SSFs) are successfully prepared. • SSFs exhibit high BET surface area and ordered hierarchical pore structure. • Agar addition improves BET surface area and micropore volume of SSFs. • Foaming process generates interconnected 3-D network macropore structure of SSFs.

  12. 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.

  13. 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

    2016-08-01

    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.

  14. 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

  15. Large-Pore Mesoporous Silica with Three-Dimensional Wormhole Framework Structures

    PubMed Central

    Park, In; Pinnavaia, Thomas J.

    2009-01-01

    Large-pore mesoporous silica with 3D wormhole framework structures (denoted MSU-J) are prepared through a supramolecular hydrogen-bonding assembly pathway from low-cost sodium silicate as the silica source and commercially available mono- and triamine Jeffamine and Surfonamine surfactants as structure-directing porogens. The calcined mesostructures exhibit large pore sizes (up to 8.2 nm), surface areas (632–1030 m2/g) and pore volumes (0.5–2.0 cm3/g), depending on the surfactant chain length and synthesis temperature (25–65 °C). The textural properties of these new wormhole mesostructures are comparable to those of hexagonal SBA-15 derivatives and large pore MCM-48. However, unlike the SBA-15 structure type, wherein the 3D pore network is formed by connecting 1D cylindrical mesopores through micropores, MSU-J mesophases have wormhole framework structures containing fully interconnected 3D mesopores that can minimize the diffusion limitations often encountered in adsorption and chemical catalysis. Also, unlike large pore MCM-48, which requires cost-intensive tetraethylorthosilicate as a silica source and the use of a co-surfactant as a pore expander under strong acid conditions, MSU-J mesostructures are assembled from low cost sodium silicate in the presence of a single Jeffamine or Surfonamine porogen at near-neutral pH. PMID:20126285

  16. Large-Pore Mesoporous Silica with Three-Dimensional Wormhole Framework Structures.

    PubMed

    Park, In; Pinnavaia, Thomas J

    2009-02-01

    Large-pore mesoporous silica with 3D wormhole framework structures (denoted MSU-J) are prepared through a supramolecular hydrogen-bonding assembly pathway from low-cost sodium silicate as the silica source and commercially available mono- and triamine Jeffamine and Surfonamine surfactants as structure-directing porogens. The calcined mesostructures exhibit large pore sizes (up to 8.2 nm), surface areas (632-1030 m(2)/g) and pore volumes (0.5-2.0 cm(3)/g), depending on the surfactant chain length and synthesis temperature (25-65 °C). The textural properties of these new wormhole mesostructures are comparable to those of hexagonal SBA-15 derivatives and large pore MCM-48. However, unlike the SBA-15 structure type, wherein the 3D pore network is formed by connecting 1D cylindrical mesopores through micropores, MSU-J mesophases have wormhole framework structures containing fully interconnected 3D mesopores that can minimize the diffusion limitations often encountered in adsorption and chemical catalysis. Also, unlike large pore MCM-48, which requires cost-intensive tetraethylorthosilicate as a silica source and the use of a co-surfactant as a pore expander under strong acid conditions, MSU-J mesostructures are assembled from low cost sodium silicate in the presence of a single Jeffamine or Surfonamine porogen at near-neutral pH.

  17. 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.

  18. 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

    2016-07-01

    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.

  19. 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

    2016-07-01

    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. PMID:27258427

  20. 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.

  1. Tailoring the properties of sub-3 μm silica core-shell particles prepared by a multilayer-by-multilayer process.

    PubMed

    Dong, Hanjiang; Brennan, John D

    2015-01-01

    Sub-3 μm silica core-shell particles (CSPs) were fabricated by a multilayer-by-multilayer method recently developed in our group. In this work, we report on methods to prepare and modify the properties of these CSPs by high temperature calcination, pore size enlargement under basic conditions, and rehydrolyzation in boiling water to make them more suitable as starting materials for preparation of HPLC columns. The chemical, physical and mechanical properties of these modified CSPs were characterized by scanning electron microscopy (SEM), infrared spectroscopy (IR), thermogravimetric analysis (TGA), and nitrogen sorption porosimetry. CSPs obtained after these treatments were observed to have the following properties: particle diameter ∼2.7 μm, shell thickness ∼0.5 μm, surface area ∼200 m(2)/g, pore diameter ∼10 nm (and almost no mesopores), pore volume ∼0.5 cc/g, and Si-OH group surface concentration ∼4 OH/nm(2). These properties are in line with those of commercially available sub-3 μm CSP products. PMID:25310582

  2. 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. PMID:27023632

  3. 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.

  4. 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.

  5. The Synthesis and Structure of SSZ-73: an All-Silica Zeolite with an Unusual Framework Topology

    SciTech Connect

    Wragg,D.; Morris, R.; Burton, A.; Zones, S.; Ong, K.; Lee, G.

    2007-01-01

    This paper reports the synthesis, characterization, and crystallographic studies of the new all-silica zeolite SSZ-73. The framework topology of SSZ-73 is isostructural with the aluminophosphate STA-6 (SAS). SSZ-73 is prepared from fluoride-containing gels using 3-ethyl-1,3,8,8-tetramethyl-3-azoniabicyclo[3.2.1]octane cation as a structure-directing agent. SSZ-73 is an all-silica zeolite with a one-dimensional system of eight-ring pores. However, SSZ-73 possesses a remarkably high micropore volume (0.25 cm{sup 3}/g) due to the rather large cages in the structure. A single-crystal X-ray diffraction study of the as-made material shows that fluoride resides within the double six-ring cages of the SAS framework. Molecular docking studies were performed for the two geometric isomers of the structure-directing agent in the all-silica frameworks of SAS, RTH, ITE, and STF. The studies suggest that the isomer with the ethyl group cis to the bridgehead carbon is the likely structure-directing agent for SSZ-73 and that the other isomer may be responsible for the small amounts of RTH impurity observed in some preparations of SSZ-73.

  6. 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

  7. 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.

  8. 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.

  9. 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

  10. Preparation of periodic mesoporous silica-included divacant Keggin units for the catalytic oxidation of styrene to synthesize styrene oxide

    NASA Astrophysics Data System (ADS)

    Yu, Xiaodan; Xu, Leilei; Yang, Xia; Guo, Yingna; Li, Kexin; Hu, Jianglei; Li, Wei; Ma, Fengyan; Guo, Yihang

    2008-05-01

    Periodic mesoporous composite catalysts, [( n-C 4H 9) 4N] 4[γ-SiW 10O 34(H 2O) 2]/SBA-15 (TBA-1*/SBA-15, where TBA-1* = [( n-C 4H 9) 4N] 4[γ-SiW 10O 34(H 2O) 2]), with TBA-1* loadings of 4.3-14.8% were prepared by simultaneous hydrolysis and co-condensation of the tetraethoxysilane (TEOS) in the presence of divacant Keggin-type polyoxometalate and triblock copolymer surfactant (P123) followed by hydrothermal treatment process. Structure integrity of the Keggin unit in as-prepared composites was studied by Fourier transform infrared spectroscopy (FT-IR), Raman scattering spectra, and 29Si magic-angle spinning (MAS) NMR. Periodic mesoporous structure of the composites was evaluated by low-angle X-ray powder diffraction (LXRD) patterns, nitrogen porosimetry, and transmission electron microscope (TEM) measurements. As-prepared TBA-1*/SBA-15 was used as an heterogeneous oxidation catalyst for the styrene epoxidation reaction to synthesize styrene oxide in the presence of dilute H 2O 2 (30%), and influences of solvent, molar ratio of styrene to H 2O 2, TBA-1* loading on the styrene conversion, styrene oxide yield and selectivity were considered.

  11. 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

  12. 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.

  13. Microporous polyimide films for reduced dielectric applications

    SciTech Connect

    Saunders, R.S.; Aubert, J.H.; McNamara, W.F.

    1996-08-01

    Limiting factor to computer chip speed and size is the dielectric constant of the interlayer insulating materials, which has been reduced going from inorganic to organic type materials. A further reduction, together with better mechanical properties, is still needed. We have developed a spincoating method in conjunction with a thermodynamic process (Non-solvent Induced Phase Separation) to create microporous polyimide films with both lower dielectric constant and better stress reduction properties compared to solid films. In this method, we spincoat a soluble polyimide solution in 1, 3-dimethoxybenzene solvent onto a Si wafer, and then immediately submerse the wet polymer film into a non-solvent bath, typically toluene. Phase separation of the polymer occurs on a micron size scale and the resulting microporous structure becomes locked in by the high glass transition temperature of the polyimide. Factors affecting film morphology, thickness, pore size, and % porosity include polymer concentration, spin speed, and non-solvent type. Morphology is explained in terms of thermodynamics and kinetics of phase separation and diffusion, using an idealized ternary phase diagram. One particular film having 68% porosity, 22 microns thickness, and 1.4 micron pore size had a dielectric constant of 1.88 and loss of 0.002. Stress measurements indicated that the microporous film reduced surface stress on the wafer by more than a factor of 10 compared to analogous solid polyimide film.

  14. 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

  15. 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.

  16. Improved fibroblast functionalities by microporous pattern fabricated by microelectromechanical systems.

    PubMed

    Wei, Hongbo; Zhao, Lingzhou; Chen, Bangdao; Bai, Shizhu; Zhao, Yimin

    2014-01-01

    Fibroblasts, which play an important role in biological seal formation and maintenance, determine the long-term success of percutaneous implants. In this study, well-defined microporous structures with micropore diameters of 10-60 µm were fabricated by microelectromechanical systems and their influence on the fibroblast functionalities was observed. The results show that the microporous structures with micropore diameters of 10-60 µm did not influence the initial adherent fibroblast number; however, those with diameters of 40 and 50 µm improved the spread, actin stress fiber organization, proliferation and fibronectin secretion of the fibroblasts. The microporous structures with micropore diameters of 40-50 µm may be promising for application in the percutaneous part of an implant.

  17. Preparation of organic-inorganic hybrid silica monolith with octyl and sulfonic acid groups for capillary electrochromatograhpy and application in determination of theophylline and caffeine in beverage.

    PubMed

    Chen, Ming-Luan; Zheng, Ming-Ming; Feng, Yu-Qi

    2010-05-21

    An organic-inorganic hybrid silica monolithic column with octyl and sulfonic acid groups has been prepared by sol-gel technique for capillary electrochromatograhpy. The structure of hybrid monolith was optimized by changing the composition of tetraethoxysilane (TEOS), octyltriethoxysilane (C(8)-TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) in the mixture of precursors. Then, the obtained hybrid monolith was oxidized using hydrogen peroxide (30%, w/w) to yield sulfonic acid groups. The sulfonic acid group, which served as strong cation-exchanger, dominated the charge on the surface of the capillary column and generated stable electroosmotic flow (EOF) in a wide range of pH. The monolithic column was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and elemental analysis (EA), and the performance of column was evaluated in detail by separating different kinds of compounds with column efficiency up to 155,000 plates/m for thiourea. In addition, this monolithic column was also applied in the analysis of theophylline (TP) and caffeine (CA) in beverages. The detection limits were 0.39 and 0.48 microg/mL for theophylline and caffeine, respectively. The method reproducibility was tested by evaluating the intra- and inter-day precisions, and relative standard deviations of less than 3.9 and 8.4%, respectively, were obtained. Recoveries of compounds from spiked beverage samples ranged from 87.2 to 105.2%.

  18. Preparation of imidazole-functionalized silica by surface-initiated atom transfer radical polymerization and its application for hydrophilic interaction chromatography.

    PubMed

    Zhang, Lei; Dai, Xiaojun; Xu, Fei; Wang, Fuqiang; Gong, Bolin; Wei, Yinmao

    2012-09-01

    A novel imidazole-functionalized stationary phase for hydrophilic interaction chromatography (HILIC) was prepared via surface-initiated atom transfer radical polymerization (SI-ATRP). 1-Vinylimidazole as a monomer was polymerized on the surface of initiator-immobilized silica by SI-ATRP using CuCl and 2,2'-bipyridyl as a catalyst. The graft chain length and polymer grafting density were controlled by varying the ratio of monomer to initiator. The resulting materials were characterized by elemental analysis and thermogravimetric analysis. Then, high-performance liquid chromatography separation of eight nucleobases/nucleosides was performed on the imidazole-functionalized chromatographic column in HILIC mode. The effects of mobile phase composition, buffer pH, and column temperature on the separation of nucleobases/nucleosides were investigated, and the retention mechanisms were studied. Chromatographic parameters were calculated, and the results showed that surface adsorption through hydrogen bonding and electrostatic interaction dominated the retention behavior of the solutes in HILIC mode. Lastly, the stationary phase was successfully used to determine the nucleobases and nucleosides from Cordyceps militaris.

  19. 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.

  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. Three-dimensional interconnected microporous poly(dimethylsiloxane) microfluidic devices.

    PubMed

    Yuen, Po Ki; Su, Hui; Goral, Vasiliy N; Fink, Katherine A

    2011-04-21

    This technical note presents a fabrication method and applications of three-dimensional (3D) interconnected microporous poly(dimethylsiloxane) (PDMS) microfluidic devices. Based on soft lithography, the microporous PDMS microfluidic devices were fabricated by molding a mixture of PDMS pre-polymer and sugar particles in a microstructured mold. After curing and demolding, the sugar particles were dissolved and washed away from the microstructured PDMS replica revealing 3D interconnected microporous structures. Other than introducing microporous structures into the PDMS replica, different sizes of sugar particles can be used to alter the surface wettability of the microporous PDMS replica. Oxygen plasma assisted bonding was used to enclose the microstructured microporous PDMS replica using a non-porous PDMS with inlet and outlet holes. A gas absorption reaction using carbon dioxide (CO(2)) gas acidified water was used to demonstrate the advantages and potential applications of the microporous PDMS microfluidic devices. We demonstrated that the acidification rate in the microporous PDMS microfluidic device was approximately 10 times faster than the non-porous PDMS microfluidic device under similar experimental conditions. The microporous PDMS microfluidic devices can also be used in cell culture applications where gas perfusion can improve cell survival and functions.

  2. 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

    2014-12-01

    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

  3. 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

    2014-12-01

    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

  4. [Recombinant strain producing thermostable lipase from Thermomyces lanuginosus immobilized into nanocarbon silica matrices and properties of the prepared biocatalyzers].

    PubMed

    Kovalenko, G A; Beklemishev, A B; Perminova, L V; Chuenko, T V; Ivanov, I D; Moiseenkov, S I; Kuznetsov, V L

    2013-01-01

    Multicomponent composite biocatalyzers with lipolytic activity have been studied. These biocatalyzers were prepared through the immobilization of a recombinant producer strain of thermostable lipase from Thermomyces lanuginosus into SiO2 xerogel, which contains a nanocarbon component, i.e., multilayered carbon nanotubes with varying diameters, and also bulblike structured carbon nanospheres ("nanobulb"). The properties of lipase were studied both in cell suspensions of a recombinant producer strain constructed based on E. coli BL21(DE3) and in the immobilized state with regard to the structure and dispersibility of the nanocarbon component used in the composition of the biocatalyzers. It was shown that the recombinant intracellular lipase exerted its activity in a reaction of tributirin hydrolysis on average comprising 50 U/mg of dried cells and had a high level of thermostability. Upon heating in olive oil at 100 degrees C, the inactivation constant and the period of semi-inactivation comprised 6 x 10(-3) min(-1) and 2 h, respectively, exceeding by one order the thermostability of lipase in a buffer solution. Biocatalyzers that contained aggregated "thick" nanotubes with a diameter of 20-22 nm had the maximum initial activity-250 U/g. PMID:23882949

  5. 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.

  6. 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.

  7. 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.

  8. Microporous polyimide films for reduced dielectric applications

    SciTech Connect

    Saunders, R.S.; Aubert, J.H.; McNamara, W.F.

    1995-01-01

    With all the advances in the microelectronics industry, a limiting factor to computer chip speed and size is becoming the dielectric constant of the interlayer insulating materials. Dielectric constants of these layers have been reduced in going from inorganic to organic type materials. A further reduction in dielectric constant, coupled with better mechanical properties are still required for these types of materials. The authors have developed a technique involving spincoating in conjunction with a thermodynamic process called {open_quotes}Non-solvent Induced Phase Separation{close_quotes} (NSIPS) to create microporous polyimide films that exhibit both a lower dielectric constant and better stress reduction properties compared to their solid film counterparts. In this technique, the authors spincoat a soluble polyimide solution in 1,3-dimethoxybenzene solvent onto a silicon wafer, and then immediately submerse the {open_quotes}wet{close_quotes} polymer film into a non-solvent bath, typically toluene. Phase separation of the polymer occurs on a micron size scale and the resulting microporous structure becomes locked in by the high glass transition temperature of the polyimide. The authors have determined the factors affecting the film morphology, thickness, pore size, and percent porosity; these factors include the polymer concentration, spin speed, and the type of non-solvent used. The different morphologies obtained for the varying non-solvents are explained in terms of thermodynamics and kinetics of phase separation and diffusion, using an idealized ternary phase diagram. One particular film having a porosity of 68%, thickness of 22 microns and pore size of 1.4 microns had a measured dielectric constant of 1.88 and dielectric loss of 0.002. Stress measurements indicated that the microporous film reduced surface stress on the wafer by more than a factor of 10 when compared to the analogous solid polyimide film.

  9. 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.

  10. 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.

  11. Thermodynamics and transport in microporous media

    SciTech Connect

    Glandt, E.D.

    1992-09-01

    Focus of this report is on the thermodynamic properties/behavior of fluids contained or adsorbed on the random microporus materials (disordered solids). The Madden-Glandt formalism for fluids in disordered matrices is applied to realistic systems (gas adsorption in carbons, polymer partitioning). Work on microgeometry of solids and their percolation and connectedness properties was continued; a study of the simplest model for microporous materials (random-pore or ''Swiss cheese'' model) was completed. Work on irreversible adsorption was continued; a simple model for correlated adsorption was studied.

  12. 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.

  13. 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.

  14. Preparation of phenothiazine bonded silica gel as sorbents of solid phase extraction and their application for determination of nitrobenzene compounds in environmental water by gas chromatography-mass spectrometry.

    PubMed

    Peng, Xi-Tian; Zhao, Xing; Feng, Yu-Qi

    2011-12-30

    In this paper, two phenothiazine bonded silica (PTZ-Si) sorbents were prepared and used as sorbents of solid-phase extraction (SPE) for the determination of nitrobenzene compounds in environmental water samples by gas chromatography-mass spectrometry (GC-MS). Different synthesis routes were proposed to obtain high bonded amount of PTZ on the surface of silica gel. PTZ molecule was derived to its amino or acyl chloride derivatives for reacting with isocyanate or amino silane coupling agent, which was further reacted with the surface silanol groups of silica gel to obtain the PTZ-Si sorbents. The resultant PTZ-Si sorbents were characterized by nitrogen sorption porosimetry (NSP), Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to assure the successful bonding of PTZ on the surface of silica gel. Then the PTZ-Si sorbents were served as SPE sorbents for the enrichment of nitrobenzene compounds. Several parameters affecting the extraction performance were investigated. Under the optimized conditions, the proposed method was applied to the analysis of six nitrobenzene compounds in environmental water samples. Good linearities were obtained for all nitrobenzene compounds with R(2) larger than 0.9958. The limits of detection were found to be in the range of 0.06-0.3 ng/mL. The method recoveries of nitrobenzene compounds spiked in water samples were from 71.4% to 124.3%, with relative standard deviations (RSDs) less than 10.1%. PMID:22129571

  15. Understanding effect of wall structure on the hydrothermal stability of mesostructured silica SBA-15.

    PubMed

    Zhang, Fuqiang; Yan, Yan; Yang, Haifeng; Meng, Yan; Yu, Chengzhong; Tu, Bo; Zhao, Dongyuan

    2005-05-12

    Mesostructured silica SBA-15 materials with different structural parameters, such as pore size, pore volume, and wall thickness, etc., were prepared by varying the postsynthesis hydrothermal treatment temperature and adding inorganic salts. The hydrothermal stabilities of these materials in steam (100% water vapor) were systematically investigated using a variety of techniques including powder X-ray diffraction, transmission electron microscopy, nitrogen sorption, and (29)Si solid-state NMR. The effect of the pore size, microporosity or mesoporosity, and wall thickness on the stability was discussed. The results show that all of the SBA-15 materials have a good hydrothermal stability under steam of 600 degrees C for at least 24 h. N(2) sorption measurements show that the Brumauer-Emmett-Teller surface area of SBA-15 materials is decreased by about 62% after treatment under steam at 600 degrees C for 24 h. The materials with thicker walls and more micropores show relatively better hydrothermal stability in steam of 600 degrees C. Interestingly, we found that the microporosity of the mesostructured silica SBA-15 is a very important factor for the hydrothermal stability. To the materials with more micropores, the recombination of Si-O-Si bonds during the high-temperature steam treatment may not cause direct destruction to the wall structure. As a result, SBA-15 materials with more micropores show better stability in pure steam of 600 degrees C. Nevertheless, these materials are easily destroyed in steam of 800 degrees C for 6 h. Two methods to effectively improve the hydrothermal stability are introduced here: one is a high-temperature treatment, and another is a carbon-propping thermal treatment. Thermal treatment at 900 degrees C can enhance the polymerization degree of Si-O-Si bonds and effectively improve the hydrothermal stability of these SBA-15 materials in 800 degrees C steam for 12 h. But, this approach will cause very serious shrinkage of the mesopores

  16. Nanoscale assembly of lanthanum silica with dense and porous interfacial structures

    NASA Astrophysics Data System (ADS)

    Ballinger, Benjamin; Motuzas, Julius; Miller, Christopher R.; Smart, Simon; Diniz da Costa, João C.

    2015-02-01

    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.

  17. 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

  18. π-Conjugated Microporous Polymer Films: Designed Synthesis, Conducting Properties, and Photoenergy Conversions

    PubMed Central

    Gu, Cheng; Huang, Ning; Chen, Youchun; Qin, Leiqiang; Xu, Hong; Zhang, Shitong; Li, Fenghong; Ma, Yuguang; Jiang, Donglin

    2015-01-01

    Conjugated microporous polymers are a unique class of polymers that combine extended π-conjugation with inherent porosity. However, these polymers are synthesized through solution-phase reactions to yield insoluble and unprocessable solids, which preclude not only the evaluation of their conducting properties but also the fabrication of thin films for device implementation. Here, we report a strategy for the synthesis of thin films of π-conjugated microporous polymers by designing thiophene-based electropolymerization at the solution–electrode interface. High-quality films are prepared on a large area of various electrodes, the film thickness is controllable, and the films are used for device fabrication. These films are outstanding hole conductors and, upon incorporation of fullerenes into the pores, function as highly efficient photoactive layers for energy conversions. Our film strategy may boost the applications in photocatalysis, energy storage, and optoelectronics. PMID:26418672

  19. Ordered microporous layered lanthanide 1,3,5-benzenetriphosphonates pillared with cationic organic molecules.

    PubMed

    Araki, Takahiro; Kondo, Atsushi; Maeda, Kazuyuki

    2015-04-13

    Novel isomorphous pillared-layer-type crystalline lanthanide 1,3,5-benzenetriphosphonates were prepared with bpy and dbo as organic pillars (LnBP-bpy and LnBP-dbo; Ln: Ce, Pr, and Nd). Ab initio crystal structure solution using synchrotron X-ray powder diffraction data revealed that the organic pillars do not exist as neutral coordinating ligands but as cationic molecules. Especially the LnBP-dbo phases have ordered interlayer space filled with water molecules between the dbo pillars, and the interlayer water is successfully removed by heating under vacuum with slightly distorted but basically retained pillared layer structures. Microporosity of the materials is confirmed by adsorption of nitrogen, carbon dioxide, and hydrogen gases. Such microporous layered metal phosphonates pillared with cationic molecules should be unprecedented and should offer new strategies to design ordered microporous materials.

  20. Hydrogenotrophic denitrification in a microporous membrane bioreactor.

    PubMed

    Mansell, Bruce O; Schroeder, Edward D

    2002-11-01

    Hydrogenotrophic denitrification of nitrate contaminated groundwater in a bench-scale microporous membrane bioreactor has been investigated. To prevent microbial contamination of the effluent from the reactor the nitrate-laden water treated was separated from the denitrifying culture with a 0.02 microm pore diameter membrane. Equal pressure was maintained across the membrane and nitrate was removed by molecular diffusion through the membrane and into the denitrifying culture. The system was operated with a hydrogenotrophic denitrification culture to circumvent the addition of an organic substrate to the water. Removal efficiencies ranging from 96% to 92% were achieved at influent concentrations ranging from 20 to 40 mg/L NO3(-)-N. The flux values achieved in this study were 2.7-5.3 g NO3-N m 2d(-1). The microporous membrane served as an effective barrier for preventing microbial contamination of the product water as evidenced by the effluent heterotrophic plate count of 9 (+/- 3.5) CFU/mL. The hydrogenotrophic culture was analyzed using available 16S and 23S rRNA-targeted oligonucleotide probes. It was determined that the enrichment process selected for organisms belonging to the beta subclass of Proteobacteria. Further analysis of the hydrogenotrophic culture indicated that the organisms may belong to the beta-3 subgroup of Proteobacteria and have yet to be identified as hydrogenotrophic denitrifiers.

  1. Immersion Calorimetry: Molecular Packing Effects in Micropores.

    PubMed

    Madani, S Hadi; Silvestre-Albero, Ana; Biggs, Mark J; Rodríguez-Reinoso, Francisco; Pendleton, Phillip

    2015-12-21

    Repeated and controlled immersion calorimetry experiments were performed to determine the specific surface area and pore-size distribution (PSD) of a well-characterized, microporous poly(furfuryl alcohol)-based activated carbon. The PSD derived from nitrogen gas adsorption indicated a narrow distribution centered at 0.57±0.05 nm. Immersion into liquids of increasing molecular sizes ranging from 0.33 nm (dichloromethane) to 0.70 nm (α-pinene) showed a decreasing enthalpy of immersion at a critical probe size (0.43-0.48 nm), followed by an increase at 0.48-0.56 nm, and a second decrease at 0.56-0.60 nm. This maximum has not been reported previously. After consideration of possible reasons for this new observation, it is concluded that the effect arises from molecular packing inside the micropores, interpreted in terms of 2D packing. The immersion enthalpy PSD was consistent with that from quenched solid density functional theory (QSDFT) analysis of the nitrogen adsorption isotherm.

  2. Immersion Calorimetry: Molecular Packing Effects in Micropores.

    PubMed

    Madani, S Hadi; Silvestre-Albero, Ana; Biggs, Mark J; Rodríguez-Reinoso, Francisco; Pendleton, Phillip

    2015-12-21

    Repeated and controlled immersion calorimetry experiments were performed to determine the specific surface area and pore-size distribution (PSD) of a well-characterized, microporous poly(furfuryl alcohol)-based activated carbon. The PSD derived from nitrogen gas adsorption indicated a narrow distribution centered at 0.57±0.05 nm. Immersion into liquids of increasing molecular sizes ranging from 0.33 nm (dichloromethane) to 0.70 nm (α-pinene) showed a decreasing enthalpy of immersion at a critical probe size (0.43-0.48 nm), followed by an increase at 0.48-0.56 nm, and a second decrease at 0.56-0.60 nm. This maximum has not been reported previously. After consideration of possible reasons for this new observation, it is concluded that the effect arises from molecular packing inside the micropores, interpreted in terms of 2D packing. The immersion enthalpy PSD was consistent with that from quenched solid density functional theory (QSDFT) analysis of the nitrogen adsorption isotherm. PMID:26394883

  3. 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.

  4. Performance and long term stability of mesoporous silica membranes for desalination.

    PubMed

    Elma, Muthia; Yacou, Christelle; Diniz da Costa, João C; Wang, David K

    2013-01-01

    This work shows the preparation of silica membranes by a two-step sol-gel method using tetraethyl orthosilicate in ethanolic solution by employing nitric acid and ammonia as co-catalysts. The sols prepared in pH 6 resulted in the lowest concentration of silanol (Si-OH) species to improve hydrostability and the optimized conditions for film coating. The membrane was tested to desalinate 0.3-15 wt % synthetic sodium chloride (NaCl) solutions at a feed temperature of 22 °C followed by long term membrane performance of up to 250 h in 3.5 wt % NaCl solution. Results show that the water flux (and salt rejection) decrease with increasing salt concentration delivering an average value of 9.5 kg m-2 h-1 (99.6%) and 1.55 kg m-2 h-1 (89.2%) from the 0.3 and 15 wt % saline feed solutions, respectively. Furthermore, the permeate salt concentration was measured to be less than 600 ppm for testing conditions up to 5 wt % saline feed solutions, achieving below the recommended standard for potable water. Long term stability shows that the membrane performance in water flux was stable for up to 150 h, and slightly reduced from thereon, possibly due to the blockage of large hydrated ions in the micropore constrictions of the silica matrix. However, the integrity of the silica matrix was not affected by the long term testing as excellent salt rejection of >99% was maintained for over 250 h.

  5. Performance and Long Term Stability of Mesoporous Silica Membranes for Desalination

    PubMed Central

    Elma, Muthia; Yacou, Christelle; Diniz da Costa, João C.; Wang, David K.

    2013-01-01

    This work shows the preparation of silica membranes by a two-step sol-gel method using tetraethyl orthosilicate in ethanolic solution by employing nitric acid and ammonia as co-catalysts. The sols prepared in pH 6 resulted in the lowest concentration of silanol (Si–OH) species to improve hydrostability and the optimized conditions for film coating. The membrane was tested to desalinate 0.3–15 wt % synthetic sodium chloride (NaCl) solutions at a feed temperature of 22 °C followed by long term membrane performance of up to 250 h in 3.5 wt % NaCl solution. Results show that the water flux (and salt rejection) decrease with increasing salt concentration delivering an average value of 9.5 kg m–2 h–1 (99.6%) and 1.55 kg m–2 h–1 (89.2%) from the 0.3 and 15 wt % saline feed solutions, respectively. Furthermore, the permeate salt concentration was measured to be less than 600 ppm for testing conditions up to 5 wt % saline feed solutions, achieving below the recommended standard for potable water. Long term stability shows that the membrane performance in water flux was stable for up to 150 h, and slightly reduced from thereon, possibly due to the blockage of large hydrated ions in the micropore constrictions of the silica matrix. However, the integrity of the silica matrix was not affected by the long term testing as excellent salt rejection of >99% was maintained for over 250 h. PMID:24956942

  6. Effect of structure and composition on epoxidation of hexene catalyzed by microporous and mesoporous Ti-Si mixed oxides

    SciTech Connect

    Liu, Z.; Crumbaugh, G.M.; Davis, R.J.

    1996-03-01

    A series of microporous titania-silica mixed oxides were characterized and tested as catalysts for the liquid-phase epoxidation of 1-hexene with t-butyl hydroperoxide. Results from {sup 29}Si MAS NMR spectroscopy verified results from earlier characterization studies that indicated cohydrolysis of alkoxide precursors produced well-mixed oxide samples. The catalytic activity of the samples for hexene epoxidation at 353 K increased with increasing silica content. Since the fraction of tetrahedral Ti atoms in the samples also increased with silica content, the active site for the reaction is proposed to be a tetrahedrally coordinated Ti atom in a silica matrix. Polar solvents like water, acetone, and methanol inhibited the epoxidation reaction. To investigate the effect of pore size on activity, mesoporous Ti-Si mixed oxides analogous to MCM-41 were synthesized. The mesoporous samples were the most active and selective catalysts for epoxidation with TBHP, presumably due to the ease of access of the reactants to the active Ti sites. Results from EXAFS and UV reflectance spectroscopy indicated that Ti atoms in the mesoporous mixed oxides are tetrahedrally coordinated to oxygen atoms with the same Ti-O bond distance as TS-1. However, the activities of mesoporous samples are orders of magnitude lower than that of TS-1 for hexene epoxidation with aqueous hydrogen peroxide. Lower hydrophobicity of a silica mesopore (2-4 nm) compared to a TS-1 micropore (0.6 nm) may account for the difference in activity observed in reactions with aqueous hydrogen peroxide. 26 refs., 5 figs., 5 tabs.

  7. One-pot preparation of silica-supported hybrid immobilized metal affinity adsorbent with macroporous surface based on surface imprinting coating technique combined with polysaccharide incorporated sol--gel process.

    PubMed

    Li, Feng; Li, Xue-Mei; Zhang, Shu-Sheng

    2006-10-01

    A simple and reliable one-pot approach using surface imprinting coating technique combined with polysaccharide incorporated sol-gel process was established to synthesize a new organic-inorganic hybrid matrix possessing macroporous surface and functional ligand. Using mesoporous silica gel being a support, immobilized metal affinity adsorbent with a macroporous shell/mesoporous core structure was obtained after metal ion loading. In the prepared matrix, covalently bonded coating and morphology manipulation on silica gel was achieved by using one-pot sol-gel process starting from an inorganic precursor, -glycidoxypropyltrimethoxysiloxane (GPTMS), and a functional biopolymer, chitosan (CS) at the atmosphere of imprinting polyethylene glycol (PEG). Self-hydrolysis of GPTMS, self-condensation, and co-condensation of silanol groups (Si-OH) from siloxane and silica gel surface, and in situ covalent cross-linking of CS created an orderly coating on silica gel surface. PEG extraction using hot ammonium hydroxide solution gave a chemically and mechanically stabilized pore structure and deactivated residual epoxy groups. The prepared matrix was characterized by using X-ray energy dispersion spectroscopy (EDX), scanning electron microscopy (SEM) and mercury intrusion porosimetry. The matrix possessed a high capacity for copper ion loading. Protein adsorption performance of the new immobilized metal affinity adsorbent was evaluated by batch adsorption and column chromatographic experiment using bovine serum albumin (BSA) as a simple model protein. Under the optimized coating conditions, the obtained macroporous surface resulted in a fast kinetics and high capability for protein adsorption, while the matrix non-charged with metal ions offered a low non-specific adsorption. PMID:16860332

  8. Molecular simulation of RMM: ordered mesoporous SBA-15 type material having microporous ZSM-5 walls.

    PubMed

    Sonwane, C G; Li, Q

    2005-09-29

    SBA-15 is a novel porous material with uniform size mesopores arranged in a regular pattern. The adjacent mesopores are connected to each other by microporous walls. The major disadvantages of these materials are that the walls are amorphous and have low thermal, hydrothermal, and mechanical stability. Recently, there have been a few attempts to either coat the walls of SBA-15 by microporous crystalline zeolites or to fabricate SBA-15 using CMK-3 in such a way that the walls are made up of ZSM-5. The present work provides a first-ever study of RMM (replicated mesoporous materials, which are SBA-15 like ordered mesoporous materials with walls made up of ZSM-5) using molecular modeling. A random orientation of the unit cells and the distribution of sizes of the supercells located at nucleation sites would be ideal to model the RMM. However, such a study would introduce more uncertainties with regard to voids between the individual supercells, noncrystalline silica, and the location of active sites where the nucleation occurs. In a simpler model studied in the present work, the walls of SBA-15 were made up of regularly arranged ZSM-5 having the same orientation. The structure was characterized by estimating the nitrogen accessible area/volume by Connolly surfaces, small-angle and wide-angle X-ray diffraction patterns, methane adsorption, and ice as a probe to study the pore structure. It was found that RMMs have significantly higher methane adsorption capacity compared to SBA-15 and the majority of methane is adsorbed in the microporous walls of RMM. Further research in the field of RMM is needed to obtain the details of zeolitic wall structure. PMID:16853309

  9. Monodisperse Aluminosilicate Spheres with Tunable Al/Si Ratio and Hierarchical Macro-Meso-Microporous Structure.

    PubMed

    Sheng, Yuan; Zeng, Hua Chun

    2015-06-24

    While tremendous success has been seen in the development of ordered mesoporous silica by soft-templated methods, synthesis of hierarchical structures with controllable multiscale pore networks has remained a challenging topic. On the other hand, introduction of heteroatoms as an effective method of chemically functionalizing silica leads to difficulties in morphological control of the product, and multistep synthesis has been necessary for functionalized silica particles with hierarchical pore structure and uniform size. The present work demonstrates that the conflict between morphological control and heteroatom incorporation can be resolved in a CTAB-stabilized toluene-water-ethanol microemulsion system. For the first time, monodisperse macro-meso-microporous aluminosilicate spheres (MASS) are synthesized in one step at room temperature. Simultaneous tuning of Al/Si ratio (0-0.35) and the hierarchical pore structure is realized by Hofmeister anion effects of the Al source itself, [Al(OH)4](-), which change the geometry of CTAB micelles and giant vesicles. The Al is incorporated purely in a tetrahedrally coordinated status, and preliminary results from catalytic experiments show improved acidity of MASS as a catalyst support.

  10. 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.

  11. Ultra-thin microporous/hybrid materials

    DOEpatents

    Jiang, Ying-Bing; Cecchi, Joseph L.; Brinker, C. Jeffrey

    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.

  12. 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.

  13. 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.

  14. 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

  15. 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. PMID:25215454

  16. Nanoparticle-doped radioluminescent silica optical fibers

    NASA Astrophysics Data System (ADS)

    Mrazek, J.; Nikl, M.; Kasik, I.; Podrazky, O.; Aubrecht, J.; Beitlerova, A.

    2014-05-01

    This contribution deals with the preparation and characterization of the silica optical fibers doped by nanocrystalline zinc silicate. The sol-gel approach was employed to prepare colloidal solution of zinc silicate precursors. Prepared sol was thermally treated to form nanocrystalline zinc silicate disperzed inside amorphous silica matrix or soaked inside the porous silica frit deposed inside the silica substrate tube which was collapsed into preform and drawn into optical fiber. Single mode optical fiber with the core diameter 15 μm and outer diamer 125 μm was prepared. Optical and waveguiding properties of the fiber were analyzed. Concentration of the zinc silicate in the fiber was 0.93 at. %. Radioluminescence properties of nanocrystalline zinc silicate powder and of the prepared optical fiber were investigated. The nanoparticle doped samples appear a emission maximum at 390 nm.

  17. 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.

  18. Preparation and characterization of 4-isopropylcalix[4]arene-capped (3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles as chiral stationary phase for high-performance liquid chromatography.

    PubMed

    Chelvi, S K Thamarai; Zhao, Jia; Chen, Lijuan; Yan, Shi; Yin, Xiaoxing; Sun, Jiaquan; Yong, E L; Wei, Qunli; Gong, Yinhan

    2014-01-10

    A new type of 4-isopropylcalix[4]arene-capped (3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)propylsilyl-appended silica particles (IPC4CD-HPS) has been prepared by treatment of bromoacetate-substituted (3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)propylsilyl-appended silica particles (BACD-HPS) with 4-isopropylcalix[4]arene oxyanions in anhydrous N-methyl-2-pyrrolidone. The bonded silica IPC4CD-HPS has been successfully used as chiral stationary phase (CSP) in high-performance liquid chromatography (HPLC) for the first time. The synthetic stationary phase was characterized by means of elemental analysis and Fourier transform infrared spectroscopy. This new CSP has a chiral selector with two anchored functional moieties: 4-isopropylcalix[4]arene and β-cyclodextrin. The chromatographic performance of IPC4CD-HPS was investigated by separation of positional isomers of several disubstituted benzenes and enantiomers of some chiral drug compounds under reversed-phase conditions. The results showed that IPC4CD-HPS had excellent selectivity for the separation of aromatic positional isomers and enantiomers of chiral compounds due to the cooperative functioning of the anchored 4-isopropylcalix[4]arenes and β-cyclodextrins.

  19. Preparation and application of a chiral stationary phase based on (+)-(1 8-crown-6)-2,3,11,12-tetracarboxylic acid without extra free aminopropyl groups on silica surface.

    PubMed

    Hyun, Myung Ho; Cho, Yoon Jae

    2005-01-01

    A crown ether-based chiral stationary phase (CSP) without extra aminopropyl groups on the surface of silica gel was newly prepared by bonding (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid to silica gel. The new CSP was applied to the resolution of various racemic alpha-amino acids, amines, and amino alcohols. The chiral recognition efficiency of the new CSP was generally superior to that of the original CSP containing unreacted residual aminopropyl groups on the surface of silica gel in terms of the separation (alpha) and the resolution factors (Rs). The retention behaviors of analytes on the new CSP with the variation of the content of organic and acidic modifiers in aqueous mobile phase were consistent with those on the original CSP in the resolution of alpha-amino acids, but somewhat different in the resolution of racemic amines and amino alcohols from those on the original CSP and the difference was rationalized by the lipophilicity difference of the two CSPs. The effect of the column temperature on the chromatographic resolution behaviors on the new CSP was consistent with that on the original CSP.

  20. 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

  1. 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.

  2. Preparation of C60-functionalized magnetic silica microspheres for the enrichment of low-concentration peptides and proteins for MALDI-TOF MS analysis.

    PubMed

    Chen, Hemei; Qi, Dawei; Deng, Chunhui; Yang, Penyuan; Zhang, Xiangmin

    2009-01-01

    In this work, for the first time, a novel C60-functionalized magnetic silica microsphere (designated C60-f-MS) was synthesized by radical polymerization of C60 molecules on the surface of magnetic silica microspheres. The resulting C60-f-MS microsphere has magnetite core and thin C60 modified silica shell, which endow them with useful magnetic responsivity and surface affinity toward low-concentration peptides and proteins. As a result of their excellent magnetic property, the synthesized C60-f-MS microspheres can be easily separated from sample solution without ultracentrifuge. The C60-f-MS microspheres were successfully applied to the enrichment of low-concentration peptides in tryptic protein digest and human urine via a MALDI-TOF MS analysis. Moreover, they were demonstrated to have enrichment efficiency for low-concentration proteins. Due to the novel materials maintaining excellent magnetic properties and admirable adsorption, the process of enrichment and desalting is very fast (only 5 min), convenient and efficient. As it has been demonstrated in the study, newly developed fullerene-derivatized magnetic silica materials are superior to those already available in the market. The facile and low-cost synthesis as well as the convenient and efficient enrichment process of the novel C60-f-MS microspheres makes it a promising candidate for isolation of low-concentration peptides and proteins even in complex biological samples such as serum, plasma, and urine or cell lysate. PMID:19086100

  3. 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.

  4. 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.

  5. An AFM determination of the effects on surface roughness caused by cleaning of fused silica and glass substrates in the process of optical biosensor preparation.

    PubMed

    Henke, Lisa; Nagy, Noemi; Krull, Ulrich J

    2002-06-01

    The covalent attachment of organic films and of biological molecules to fused silica and glass substrates is important for many applications. For applications such as biosensor development, it is desired that the immobilised molecules be assembled in a uniform layer on the surface so as to provide for reproducibility and speed of surface interactions. For optimal derivatisation the surface must be appropriately cleaned to remove contamination, to create surface attachment sites such as hydroxyl groups, and to control surface roughness. The irregularity of the surface can be significant in defining the integrity and density of immobilised films. Numerous cleaning methods exist for fused silica and glass substrates and these include gas plasmas, and combinations of acids, bases and organic solvents that are allowed to react at varying temperatures. For many years, we have used a well established method based on a combination of washing with basic peroxide followed by acidic peroxide to clean and hydroxylate the surface of fused silica and glass substrates before oligonucleotide immobilisation. Atomic force microscopy (AFM) has been used to evaluate the effect of cleaning on surface roughness for various fused silica and glass samples. The results indicate that surface roughness remains substantial after use of this common cleaning routine, and can provide a surface area that is more than 10% but less than 30% larger than anticipated from geometric considerations of a planar surface.

  6. 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.

  7. Structure and Capacitance of Electrical Double Layers inside Micropores

    NASA Astrophysics Data System (ADS)

    Feng, Guang; Qiao, Rui; Huang, Jingsong; Sumpter, Bobby G.; Meunier, Vincent

    2010-03-01

    Recent experiments indicate that the specific capacitance of micropores (diameter less than 2nm) increases anomalously as the pore size decreases^[1]. To understand the physical origin of this discovery, we performed a series of molecular dynamics simulations to study the electrical double layers (EDLs) in micropores with different shapes (tube vs slit) and pore sizes (0.668nm - 3.342nm). Several different aqueous electrolytes (K^+, Na^+, Cl^-, and F^- in water) were used in these micropores. We quantified the structure of EDLs inside the pores, and computed the capacitance of EDLs. The scaling of capacitance shows a qualitative agreement with the experimental observations. We attribute the anomalous enhancement of capacitance in micropores to the short-range ionelectrode and ionsolvent interactions.[1] J. Chmiola, G. Yushin, Y. Gogotsi, C. Portet, P. Simon, and P.L. Taberna, Science 2006, 313, 1760.

  8. Supercritical Processing of Functionalized Size Selective Microporous Materials

    SciTech Connect

    Shin, Yongsoon; Zemanian, Thomas S.; Fryxell, Glen E.; Wang, Li Q.; Liu, Jun

    2000-05-01

    Zeolites and related microporous materials are qidely used in industry as size selective catalysts due to the uniform pore size and shape. The modification of such materials by organic funtional molecules will greatly broaden the application.

  9. 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.

  10. 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.

  11. 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. PMID:26810114

  12. Diclofenac delays micropore closure following microneedle treatment in human subjects.

    PubMed

    Brogden, Nicole K; Milewski, Mikolaj; Ghosh, Priyanka; Hardi, Lucia; Crofford, Leslie J; Stinchcomb, Audra L

    2012-10-28

    Drugs absorbed poorly through the skin are commonly delivered via injection with a hypodermic needle, which is painful and increases the risk of transmitting infectious diseases. Microneedles (MNs) selectively and painlessly permeabilize the outermost skin layer, allowing otherwise skin-impermeable drugs to cross the skin through micron-sized pores and reach therapeutic concentrations. However, rapid healing of the micropores prevents further drug delivery, blunting the clinical utility of this unique transdermal technique. We present the first human study demonstrating that micropore lifetime can be extended following MN treatment. Subjects received one-time MN treatment and daily topical application of diclofenac sodium. Micropore closure was measured with impedance spectroscopy, and area under the admittance-time curve (AUC) was calculated. AUC was significantly higher at MN+diclofenac sodium sites vs. placebo, suggesting slower rates of micropore healing. Colorimetry measurements confirmed the absence of local erythema and irritation. This mechanistic human proof-of-concept study demonstrates that micropore lifetime can be prolonged with simple topical administration of a non-specific cyclooxygenase inhibitor, suggesting the involvement of subclinical inflammation in micropore healing. These results will allow for longer patch wear time with MN-enhanced delivery, thus increasing patient compliance and expanding the transdermal field to a wider variety of clinical conditions. PMID:22929967

  13. SANS Investigations of CO2 Adsorption in Microporous Carbon

    DOE PAGESBeta

    Bahadur, Jitendra; Melnichenko, Yuri B.; He, Lilin; Contescu, Cristian I.; Gallego, Nidia C.; Carmichael, Justin R.

    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

  14. Microporous Cell-laden Hydrogels for Engineered Tissue Constructs

    PubMed Central

    Park, Jae Hong; Chung, Bong Geun; Lee, Won Gu; Kim, Jinseok; Brigham, Mark D.; Shim, Jaesool; Lee, Seunghwan; Hwang, Changmo; Durmus, Naside Gozde; Demirci, Utkan; Khademhosseini, Ali

    2010-01-01

    In this paper, we describe an approach to generate microporous cell-laden hydrogels for fabricating biomimetic tissue engineered constructs. Micropores at different length scales were fabricated in cell-laden hydrogels by micromolding fluidic channels and leaching sucrose crystals. Microengineered channels were created within cell-laden hydrogel precursors that contained agarose solution mixed with sucrose crystals. The rapid cooling of the agarose solution was used to gel the solution and form micropores in place of the sucrose crystals. The sucrose leaching process generated micropores that were homogeneously distributed within the gels, while enabling the direct immobilization of cells within the gels. We also characterized the physical, mechanical, and biological properties (i.e. microporosity, diffusivity, and cell viability) of cell-laden agarose gels as a function of engineered porosity. The microporosity was controlled from 0% to 40% and the diffusivity of molecules in the porous agarose gels increased as compared to controls. Furthermore, the viability of human hepatocyte cells that were cultured in microporous agarose gels corresponded to the diffusion profile generated away from the microchannels. Based on their enhanced diffusive properties, microporous cell-laden hydrogels containing a microengineered fluidic channel could be a useful tool for generating tissue structures for regenerative medicine and drug discovery applications. PMID:20091766

  15. Preparation of nanoporous carbons via a grafting method for the application to electrochemical double layer capacitors.

    PubMed

    Kim, Wooyoung; Kang, Mi Yeong; Kim, Nam Dong; Joo, Ji Bong; Yi, Jongheop

    2011-01-01

    Nanoporous carbon materials with a controlled pore size and surface area were prepared using grafting method. The use of 3-mercaptopropyltrimethoxysilane (MPTMS) as a grafting material played an important role in producing a porous structure by linking the silica to the polymer, with the subsequent formation of a silica-polymer composite. Importantly, the use of an organic solvent, compared to an aqueous solvent, has a positive effect in forming uniform and well-developed carbon structures, due to the high degree of dispersion with well-mixing of the carbon and silica precursors. The amounts of MPTMS and carbon precursor used determined the pore size and surface area of resulting carbon materials. The optimum ratio of MPTMS and carbon precursor for achieving a high surface area in excess of 2000 m2/g was determined. The use of a large amount of carbon precursor resulted in carbons with a relatively small surface area and an increase in MPTMS content led to an increase in the microporous structures. The capacitance value of the porous carbon prepared using the optimum ratio was determined to be 150 F/g.

  16. Efficient fixation of CO2 by a zinc-coordinated conjugated microporous polymer.

    PubMed

    Xie, Yong; Wang, Ting-Ting; Yang, Rui-Xia; Huang, Nian-Yu; Zou, Kun; Deng, Wei-Qiao

    2014-08-01

    Zinc-coordinated conjugated microporous polymers (Zn-CMPs), prepared by linking salen zinc and 1,3,5-triethynylbenzene, exhibit extraordinary activities (turnover frequencies of up to 11600 h(-1) ), broad substrate scope, and group tolerance for the synthesis of functional organic carbonates by coupling epoxides with CO2 at 120 °C and 3.0 MPa without the use of additional solvents. The catalytic activity of Zn-CMP is comparable to those of homogeneous catalysts and superior to those of other heterogeneous catalysts. This catalyst could be reused more than ten times without a significant decrease in performance.

  17. Conjugated microporous polymers: design, synthesis and application.

    PubMed

    Xu, Yanhong; Jin, Shangbin; Xu, Hong; Nagai, Atsushi; Jiang, Donglin

    2013-10-21

    Conjugated microporous polymers (CMPs) are a class of organic porous polymers that combine π-conjugated skeletons with permanent nanopores, in sharp contrast to other porous materials that are not π-conjugated and with conventional conjugated polymers that are nonporous. As an emerging material platform, CMPs offer a high flexibility for the molecular design of conjugated skeletons and nanopores. Various chemical reactions, building blocks and synthetic methods have been developed and a broad variety of CMPs with different structures and specific properties have been synthesized, driving the rapid growth of the field. CMPs are unique in that they allow the complementary utilization of π-conjugated skeletons and nanopores for functional exploration; they have shown great potential for challenging energy and environmental issues, as exemplified by their excellent performance in gas adsorption, heterogeneous catalysis, light emitting, light harvesting and electrical energy storage. This review describes the molecular design principles of CMPs, advancements in synthetic and structural studies and the frontiers of functional exploration and potential applications.

  18. Silica reusable surface insulation

    NASA Technical Reports Server (NTRS)

    Goldstein, H. E.; Smith, M.; Leiser, D. B. (Inventor)

    1976-01-01

    A reusable silica surface insulation material is provided by bonding amorphous silica fibers with colloidal silica at an elevated temperature. The surface insulation is ordinarily manufactured in the form of blocks (i.e., tiles).

  19. Preparation of silica-sustained electrospun polyvinylpyrrolidone fibers with uniform mesopores via oxidative removal of template molecules by H{sub 2}O{sub 2} treatment

    SciTech Connect

    Kang, Haigang; Zhu, Yihua; Shen, Jianhua; Yang, Xiaoling; Chen, Cheng; Cao, Huimin; Li, Chungzhong

    2010-07-15

    Silica-sustained electrospun PVP fibers with uniform mesopores were synthesized via facile oxidative removal of template molecules by H{sub 2}O{sub 2} extraction. Tetraethyl orthosilicate, polyvinylpyrrolidone (PVP), and triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) copolymer pluronic P{sub 123} compose the electrospinning sol to fabricate the silica-sustained PVP hybrid fibers. The effect of different post-treatment methods on the pore size distribution was investigated by calcination and extraction, respectively. Experimental results showed that oxidative removal of structure-directing agent P{sub 123} in the hybrid fibers by H{sub 2}O{sub 2} treatment can easily form narrow pore size distribution, and the incorporation of 3D silica skeleton built by hot steam aging facilitated preserving the original cylindrical morphology of fibers. Scanning electron microscopy (SEM), N{sub 2} adsorption-desorption isotherm, transmission electron microscopy (TEM), X-ray diffraction (XRD), FT-IR spectra and thermogravimetric analysis (TGA) were used to characterize the hybrid fibers. The hybrid fibers can be expected to have potential applications in drug release or tissue engineering because of their suitable pore size, large surface area and good biocompatibility.

  20. 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.

  1. Is there any microporosity in ordered mesoporous silicas?

    PubMed

    Silvestre-Alberto, A; Jardim, E O; Bruijn, E; Meynen, V; Cool, P; Sepulveda-Escribano, A; Silvestre-Alberto, J; Rodriguez-Reinoso, F

    2009-01-20

    The porous structure of nanostructured silicas MCM-41 and SBA-15 has been characterized using N2 adsorption at 77 K, before and after n-nonane preadsorption, together with immersion calorimetry into liquids of different molecular dimensions. Selective blocking of the microporosity with n-nonane proves experimentally that MCM-41 is exclusively mesoporous while SBA-15 exhibits both micro- and mesopores. Additionally, N2 adsorption experiments on the preadsorbed samples show that the microporosity on SBA-15 is located in intrawall positions, the micropore volume accounting for only approximately 7-8 % of the total pore volume. Calorimetric measurements into n-hexane (0.43 nm), 2-methylpentane (0.49 nm), and 2,2-dimethylbutane (0.56 nm) estimate the size of these micropores to be < or = 0.56 nm.

  2. Consolidated silica glass from nanoparticles

    SciTech Connect

    Mayerhoefer, Thomas G. Shen Zhijian; Leonova, Ekaterina; Eden, Mattias; Kriltz, Antje; Popp, Juergen

    2008-09-15

    A dense silica glass was prepared by consolidating a highly dispersed silicic acid powder (particle size <10 nm) with the Spark Plasma Sintering (SPS) technique. The glass was characterized by ellipsometry, transmission electron microscopy (TEM), infrared reflectance and transmittance spectroscopy, as well as by Raman, UV-Vis-NIR and solid-state nuclear magnetic resonance (NMR) spectroscopy. The prototypic sample showed a transmittance of about 63% compared to silica glass in the UV-Vis spectral range. Based on the results of infrared transmittance spectroscopy this lower transparency is due to the comparably high water content, which is about 40 times higher than that in silica glass. {sup 1}H magic-angle spinning (MAS) NMR confirmed an increase in hydroxyl groups in the sample prepared by SPS relative to that of the conventional SiO{sub 2} reference glass. Aside from the comparably high water content, we conclude from the similarity of the IR-reflectance and the {sup 29}Si MAS NMR spectra of the SPS sample and the corresponding spectra of the conventionally prepared silica glass, that the short- and medium-range order is virtually the same in both materials. Raman spectroscopy, however, suggests that the number of three- and four-membered rings is significantly smaller in the SPS sample compared to the conventionally prepared sample. Based on these results we conclude that it is possible to prepare glasses by compacting amorphous powders by the SPS process. The SPS process may therefore enable the preparation of glasses with compositions inaccessible by conventional methods. - Graphical abstract: We report the preparation of SiO{sub 2} glass by consolidating a highly dispersed silicic acid powder with the Spark Plasma Sintering (SPS) technique. The glass was characterized by ellipsometry, transmission electron microscopy (TEM), infrared reflectance and transmittance spectroscopy, as well as by Raman-, UV-Vis-NIR- and solid-state nuclear magnetic resonance (NMR

  3. 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. PMID:22864212

  4. 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.

  5. 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

  6. Responsive Guest Encapsulation of Dynamic Conjugated Microporous Polymers

    NASA Astrophysics Data System (ADS)

    Xu, Lai; Li, Youyong

    2016-06-01

    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.

  7. Responsive Guest Encapsulation of Dynamic Conjugated Microporous Polymers.

    PubMed

    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

  8. Molecular simulations of supercritical fluid permeation through disordered microporous carbons.

    PubMed

    Boţan, Alexandru; Vermorel, Romain; Ulm, Franz-Josef; Pellenq, Roland J-M

    2013-08-13

    Fluid transport through microporous carbon-based materials is inherent in numerous applications, ranging from gas separation by carbon molecular sieves to natural gas production from coal seams and gas shales. The present study investigates the steady-state permeation of supercritical methane in response to a constant cross-membrane pressure drop. We performed dual control volume grand canonical molecular dynamics (DCV-GCMD) simulations to mimic the conditions of actual permeation experiments. To overcome arbitrary assumptions regarding the investigated porous structures, the membranes were modeled after the CS1000a and CS1000 molecular models, which are representative of real microporous carbon materials. When adsorption-induced molecular trapping (AIMT) mechanisms are negligible, we show that the permeability of the microporous material, although not significantly sensitive to the pressure gradient, monotonically decreases with temperature and reservoir pressures, consistent with diffusion theory. However, when AIMT occurs, the permeability increases with temperature in agreement with experimental data found in the literature. PMID:23886335

  9. 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.

  10. 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. PMID:26784977

  11. [Preparation of xylitol and maltitol modified silica as novel stationary phases for hydrophilic interaction liquid chromatography and evaluation of their separation performance].

    PubMed

    Yong, Tian; Wu, Fan; Xiao, Hongbin; Wan, Boshun

    2015-09-01

    New types of stationary phases for hydrophilic interaction liquid chromatography (HILIC) with unique selectivity are very important for the separation of various polar and hydrophilic analytes. Two novel HILIC stationary phases based on sugar alcohol modified silica were synthesized by a simple two-step reaction in which xylitol and maltitol were bonded onto the surface of silica particles via the addition reaction between -NCO and -OH. The effect of acetonitrile content on the retention indicated that the two stationary phases were of typical HILIC character and exhibited strong retention for polar and hydrophilic analytes. They succeeded in the separation of a wide range of polar and hydrophilic analytes including water soluble vitamins, salicylic acid and its analogues, nucleic acid bases and nucleosides, and icariin and its analogues with unique selectivity. Especially, the maltitol stationary phase showed unique selectivity on glycosyl group, compared to xylitol stationary phase. Furthermore, the effects of buffer pH as well as salt concentration on the retention indicated that electrostatic interaction played an important role in the separation mechanism of the two stationary phases. For sure, the efficient stationary phases are of great potential applications in HILIC.

  12. [Preparation of xylitol and maltitol modified silica as novel stationary phases for hydrophilic interaction liquid chromatography and evaluation of their separation performance].

    PubMed

    Yong, Tian; Wu, Fan; Xiao, Hongbin; Wan, Boshun

    2015-09-01

    New types of stationary phases for hydrophilic interaction liquid chromatography (HILIC) with unique selectivity are very important for the separation of various polar and hydrophilic analytes. Two novel HILIC stationary phases based on sugar alcohol modified silica were synthesized by a simple two-step reaction in which xylitol and maltitol were bonded onto the surface of silica particles via the addition reaction between -NCO and -OH. The effect of acetonitrile content on the retention indicated that the two stationary phases were of typical HILIC character and exhibited strong retention for polar and hydrophilic analytes. They succeeded in the separation of a wide range of polar and hydrophilic analytes including water soluble vitamins, salicylic acid and its analogues, nucleic acid bases and nucleosides, and icariin and its analogues with unique selectivity. Especially, the maltitol stationary phase showed unique selectivity on glycosyl group, compared to xylitol stationary phase. Furthermore, the effects of buffer pH as well as salt concentration on the retention indicated that electrostatic interaction played an important role in the separation mechanism of the two stationary phases. For sure, the efficient stationary phases are of great potential applications in HILIC. PMID:26753275

  13. 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

  14. 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.

  15. Dense silica coatings on ceramic powder particles

    SciTech Connect

    Opitz, J.F.A.; Mayr, W.

    1995-09-01

    Dense silica coatings on the surface of inorganic powders particles are prepared by the hydrolysis of tetraethoxysilane (TEOS) in alcoholic suspensions. In a first reaction step, the TEOS is pre-hydrolysed in acidic solution and afterwards, a suspension of powder particles in this reaction solution is treated with ammonia which results in a dense silica coating of typically 10 - 100 nm thickness. Different luminescent powders which are used in the manufacture of cathode-ray tubes or fluorescent lamps have been coated by this procedure. The silica coating forms a transparent layer and the suspension properties of the coated powders are determined by the silica layer. The silica coating also protects sulfidic luminescent powders from being attacked by oxidizing agents like dichromate ions which are used in the suspension formulations for TV tube fabrication.

  16. Silica/silicone nanofilament hybrid coatings with almost perfect superhydrophobicity.

    PubMed

    Zhang, Junping; Seeger, Stefan

    2013-06-01

    A facile method for the preparation of silica/silicone nanofilament hybrid coatings with almost perfect superhydrophobicity (contact angle=179.8° and sliding angle=1.3°) is presented. The coatings are obtained by dip-coating of silica nanoparticles, followed by chemical vapor deposition of silicone nanofilaments. Predominant growth of silicone nanofilaments onto aggregated silica nanoparticles generates a two-tier structure. The effect of silica nanoparticle size on the growth of silicone nanofilaments, along with their anti-wetting properties and transparency are investigated in detail. Surface roughness and anti-wetting properties can be simply regulated by controlling the size of silica nanoparticles.

  17. Imine-linked polymer-derived nitrogen-doped microporous carbons with excellent CO2 capture properties.

    PubMed

    Wang, Jiacheng; Senkovska, Irena; Oschatz, Martin; Lohe, Martin R; Borchardt, Lars; Heerwig, Andreas; Liu, Qian; Kaskel, Stefan

    2013-04-24

    A series of nitrogen-doped microporous carbons (NCs) was successfully prepared by direct pyrolysis of high-surface-area microporous imine-linked polymer (ILP, 744 m(2)/g) which was formed using commercial starting materials based on the Schiff base condensation under catalyst-free conditions. These NCs have moderate specific surface areas of up to 366 m(2)/g, pore volumes of 0.43 cm(3)/g, narrow micropore size distributions, and a high density of nitrogen functional groups (5.58-8.74%). The resulting NCs are highly suitable for CO2 capture adsorbents because of their microporous textural properties and large amount of Lewis basic sites. At 1 bar, NC-800 prepared by the pyrolysis of ILP at 800 °C showed the highest CO2 uptakes of 1.95 and 2.65 mmol/g at 25 and 0 °C, respectively. The calculated adsorption capacity for CO2 per m(2) (μmol of CO2/m(2)) of NC-800 is 7.41 μmol of CO2/m(2) at 1 bar and 25 °C, the highest ever reported for porous carbon adsorbents. The isosteric heats of CO2 adsorption (Qst) for these NCs are as high as 49 kJ/mol at low CO2 surface coverage, and still ~25 kJ/mol even at high CO2 uptake (2.0 mmol/g), respectively. Furthermore, these NCs also exhibit high stability, excellent adsorption selectivity for CO2 over N2, and easy regeneration and reuse without any evident loss of CO2 adsorption capacity.

  18. The formation of helical mesoporous silica nanotubes

    NASA Astrophysics Data System (ADS)

    Wan, Xiaobing; Pei, Xianfeng; Zhao, Huanyu; Chen, Yuanli; Guo, Yongmin; Li, Baozong; Hanabusa, Kenji; Yang, Yonggang

    2008-08-01

    Three chiral cationic gelators were synthesized. They can form translucent hydrogels in pure water. These hydrogels become highly viscous liquids under strong stirring. Mesoporous silica nanotubes with coiled pore channels in the walls were prepared using the self-assemblies of these gelators as templates. The mechanism of the formation of this hierarchical nanostructure was studied using transmission electron microscopy at different reaction times. The results indicated that there are some interactions between the silica source and the gelator. The morphologies of the self-assemblies of gelators changed gradually during the sol-gel transcription process. It seems that the silica source directed the organic self-assemblies into helical nanostructures.

  19. 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.

  20. Anisotropic microporous supports impregnated with polymeric ion-exchange materials

    DOEpatents

    Friesen, Dwayne; Babcock, Walter C.; Tuttle, Mark

    1985-05-07

    Novel ion-exchange media are disclosed, the media comprising polymeric anisotropic microporous supports containing polymeric ion-exchange or ion-complexing materials. The supports are anisotropic, having small exterior pores and larger interior pores, and are preferably in the form of beads, fibers and sheets.

  1. Anisotropic microporous supports impregnated with polymeric ion-exchange materials

    DOEpatents

    Friesen, D.; Babcock, W.C.; Tuttle, M.

    1985-05-07

    Novel ion-exchange media are disclosed, the media comprising polymeric anisotropic microporous supports containing polymeric ion-exchange or ion-complexing materials. The supports are anisotropic, having small exterior pores and larger interior pores, and are preferably in the form of beads, fibers and sheets. 5 figs.

  2. 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. PMID:27523573

  3. 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.

  4. Investigation of the ion storage/transfer behavior in an electrical double-layer capacitor by using ordered microporous carbons as model materials.

    PubMed

    Nishihara, Hirotomo; Itoi, Hiroyuki; Kogure, Taichi; Hou, Peng-Xiang; Touhara, Hidekazu; Okino, Fujio; Kyotani, Takashi

    2009-01-01

    An ordered microporous carbon, which was prepared with zeolite as a template, was used as a model material to understand the ion storage/transfer behavior in electrical double-layer capacitor (EDLC). Several types of such zeolite-templated carbons (ZTCs) with different structures (framework regularity, particle size and pore diameter) were prepared and their EDLC performances were evaluated in an organic electrolyte solution (1 M Et(4)NBF(4)/propylene carbonate). Moreover, a simple method to evaluate a degree of wettability of microporous carbon with propylene carbonate was developed. It was found that the capacitance was almost proportional to the surface area and this linearity was retained even for the carbons with very high surface areas (>2000 m(2) g(-1)). It has often been pointed out that thin pore walls limit capacitance and this usually gives rise to the deviation from linearity, but such a limitation was not observed in ZTCs, despite their very thin pore walls (a single graphene, ca. 0.34 nm). The present study clearly indicates that three-dimensionally connected and regularly arranged micropores were very effective at reducing ion-transfer resistance. Despite relatively small pore diameter ZTCs (ca. 1.2 nm), their power density remained almost unchanged even though the particle size was increased up to several microns. However, when the pore diameter became smaller than 1.2 nm, the power density was decreased due to the difficulty of smooth ion-transfer in such small micropores. PMID:19338036

  5. Positively charged microporous ceramic membrane for the removal of Titan Yellow through electrostatic adsorption.

    PubMed

    Cheng, Xiuting; Li, Na; Zhu, Mengfu; Zhang, Lili; Deng, Yu; Deng, Cheng

    2016-06-01

    To develop a depth filter based on the electrostatic adsorption principle, positively charged microporous ceramic membrane was prepared from a diatomaceous earth ceramic membrane. The internal surface of the highly porous ceramic membrane was coated with uniformly distributed electropositive nano-Y2O3 coating. The dye removal performance was evaluated through pressurized filtration tests using Titan Yellow aqueous solution. It showed that positively charged microporous ceramic membrane exhibited a flow rate of 421L/(m(2)·hr) under the trans-membrane pressure of 0.03bar. Moreover it could effectively remove Titan Yellow with feed concentration of 10mg/L between pH3 to 8. The removal rate increased with the enhancement of the surface charge properties with a maximum rejection of 99.6%. This study provides a new and feasible method of removing organic dyes in wastewater. It is convinced that there will be a broad market for the application of charged ceramic membrane in the field of dye removal or recovery from industry wastewater. PMID:27266317

  6. Development of microporous structure and its application to optical film for cellulose triacetate containing diisodecyl adipate.

    PubMed

    Shimada, Hikaru; Nobukawa, Shogo; Yamaguchi, Masayuki

    2015-04-20

    Phase separation in plasticized cellulose triacetate (CTA) films is investigated to produce a microporous film that can be used in optical devices. Hot-stretched CTA films containing diisodecyl adipate (DIDA) show negative orientation birefringence similar to the hot-stretched pure CTA. After extracting DIDA from the stretched films by immersion into an organic solvent, however, the films exhibit positive birefringence. Moreover, the magnitude of the birefringence increases with the wavelength, known as extraordinary dispersion, which is an essential property in the preparation of an ideal quarter-wave plate. Numerous ellipsoidal pores with micro-scale were detected in the film after the immersion, indicating that DIDA were segregated and formed ellipsoidal domains in the CTA matrix during annealing and stretching. These results indicate that extraordinary wavelength dispersion is given by the combinations of orientation birefringence from CTA and form birefringence from micropores. Furthermore, it was found that annealing time and stretching condition affect the phase separation as well as the shape and size of pores. PMID:25662683

  7. A multifunctional role of trialkylbenzenes for the preparation of aqueous colloidal mesostructured/mesoporous silica nanoparticles with controlled pore size, particle diameter, and morphology

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

    Both the pore size and particle diameter of aqueous colloidal mesostructured/mesoporous silica nanoparticles (CMSS/CMPS) derived from tetrapropoxysilane were effectively and easily controlled by the addition of trialkylbenzenes (TAB). Aqueous highly dispersed CMPS with large pores were successfully obtained through removal of surfactants and TAB by a dialysis process. The pore size (from 4 nm to 8 nm) and particle diameter (from 50 nm to 380 nm) were more effectively enlarged by the addition of 1,3,5-triisopropylbenzene (TIPB) than 1,3,5-trimethylbenzene (TMB), and the enlargement did not cause the variation of the mesostructure and particle morphology. The larger molecular size and higher hydrophobicity of TIPB than TMB induce the incorporation of TIPB into micelles without the structural change. When TMB was used as TAB, the pore size of CMSS was also enlarged while the mesostructure and particle morphology were varied. Interestingly, when tetramethoxysilane and TIPB were used, CMSS with a very small particle diameter (20 nm) with concave surfaces and large mesopores were obtained, which may strongly be related to the initial nucleation of CMSS. A judicious choice of TAB and Si sources is quite important to control the mesostructure, size of mesopores, particle diameter, and morphology.Both the pore size and particle diameter of aqueous colloidal mesostructured/mesoporous silica nanoparticles (CMSS/CMPS) derived from tetrapropoxysilane were effectively and easily controlled by the addition of trialkylbenzenes (TAB). Aqueous highly dispersed CMPS with large pores were successfully obtained through removal of surfactants and TAB by a dialysis process. The pore size (from 4 nm to 8 nm) and particle diameter (from 50 nm to 380 nm) were more effectively enlarged by the addition of 1,3,5-triisopropylbenzene (TIPB) than 1,3,5-trimethylbenzene (TMB), and the enlargement did not cause the variation of the mesostructure and particle morphology. The larger molecular size

  8. 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

  9. Biodiesel production from sunflower, soybean, and waste cooking oils by transesterification using lipase immobilized onto a novel microporous polymer.

    PubMed

    Dizge, Nadir; Aydiner, Coskun; Imer, Derya Y; Bayramoglu, Mahmut; Tanriseven, Aziz; Keskinler, Bülent

    2009-03-01

    This study aims at carrying out lipase-catalyzed synthesis of fatty acid methyl esters (biodiesel) from various vegetable oils using lipase immobilized onto a novel microporous polymeric matrix (MPPM) as a low-cost biocatalyst. The research is focused on three aspects of the process: (a) MPPM synthesis (monolithic, bead, and powder forms), (b) microporous polymeric biocatalyst (MPPB) preparation by immobilization of lipase onto MPPM, and (c) biodiesel production by MPPB. Experimental planning of each step of the study was separately carried out in accordance with design of experiment (DoE) based on Taguchi methodology. Microporous polymeric matrix (MPPM) containing aldehyde functional group was synthesized by polyHIPE technique using styrene, divinylbenzene, and polyglutaraldehyde. Thermomyces lanuginosus lipase was covalently attached onto MPPM with 80%, 85%, and 89% immobilization efficiencies using bead, powder, and monolithic forms, respectively. Immobilized enzymes were successfully used for the production of biodiesel using sunflower, soybean, and waste cooking oils. It was shown that immobilized enzymes retain their activities during 10 repeated batch reactions at 25 degrees C, each lasting 24h. Since the developed novel method is simple yet effective, it could have a potential to be used industrially for the production of chemicals requiring immobilized lipases. PMID:19028094

  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. 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.

  12. Suppressed N2O formation during NH3 selective catalytic reduction using vanadium on zeolitic microporous TiO2

    NASA Astrophysics Data System (ADS)

    Lee, Seung Gwan; Lee, Hyun Jeong; Song, Inhak; Youn, Seunghee; Kim, Do Heui; Cho, Sung June

    2015-08-01

    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.

  13. 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

    Ishige, Ryohei; Williams, Gregory A; Higaki, Yuji; Ohta, Noboru; Sato, Masugu; Takahara, Atsushi; Guan, Zhibin

    2016-05-01

    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

  14. 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

  15. 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 PAGESBeta

    Ishige, Ryohei; Williams, Gregory A.; Higaki, Yuji; Ohta, Noboru; Sato, Masugu; Takahara, Atsushi; Guan, Zhibin

    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

  16. 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.

  17. What Is Crystalline Silica?

    MedlinePlus

    ... silica, and requires a repirator protection program until engineering controls are implemented. Additionally, OSHA has a National ... silica materials with safer substitutes, whenever possible. ■ Provide engineering or administrative controls, where feasible, such as local ...

  18. 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.

  19. 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. PMID:27575922

  20. 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.

  1. 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.

  2. 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.

  3. Engineering Surface Energy and Nanostructure of Microporous Films for Expanded Membrane Distillation Applications.

    PubMed

    Boo, Chanhee; Lee, Jongho; Elimelech, Menachem

    2016-08-01

    We investigated the factors that determine surface omniphobicity of microporous membranes and evaluated the potential application of these membranes in desalination of low surface tension wastewaters by membrane distillation (MD). Specifically, the effects of surface morphology and surface energy on membrane surface omniphobicity were systematically investigated by evaluating wetting resistance to low surface tension liquids. Single and multilevel re-entrant structures were achieved by using cylindrical glass fibers as a membrane substrate and grafting silica nanoparticles (SiNPs) on the fibers. Surface energy of the membrane was tuned by functionalizing the fiber substrate with fluoroalkylsilane (FAS) having two different lengths of fluoroalkyl chains. Results show that surface omniphobicity of the modified fibrous membrane increased with higher level of re-entrant structure and with lower surface energy. The secondary re-entrant structure achieved by SiNP coating on the cylindrical fibers was found to play a critical role in enhancing the surface omniphobicity. Membranes coated with SiNPs and chemically modified by the FAS with a longer fluoroalkyl chain (or lower surface energy) exhibited excellent surface omniphobicity and showed wetting resistance to low surface tension liquids such as ethanol (22.1 mN m(-1)). We further evaluated performance of the membranes in desalination of saline feed solutions with varying surface tensions by membrane distillation (MD). The engineered membranes exhibited stable MD performance with low surface tension feed waters, demonstrating the potential application omniphobic membranes in desalinating complex, high salinity industrial wastewaters. PMID:27391088

  4. Engineering Surface Energy and Nanostructure of Microporous Films for Expanded Membrane Distillation Applications.

    PubMed

    Boo, Chanhee; Lee, Jongho; Elimelech, Menachem

    2016-08-01

    We investigated the factors that determine surface omniphobicity of microporous membranes and evaluated the potential application of these membranes in desalination of low surface tension wastewaters by membrane distillation (MD). Specifically, the effects of surface morphology and surface energy on membrane surface omniphobicity were systematically investigated by evaluating wetting resistance to low surface tension liquids. Single and multilevel re-entrant structures were achieved by using cylindrical glass fibers as a membrane substrate and grafting silica nanoparticles (SiNPs) on the fibers. Surface energy of the membrane was tuned by functionalizing the fiber substrate with fluoroalkylsilane (FAS) having two different lengths of fluoroalkyl chains. Results show that surface omniphobicity of the modified fibrous membrane increased with higher level of re-entrant structure and with lower surface energy. The secondary re-entrant structure achieved by SiNP coating on the cylindrical fibers was found to play a critical role in enhancing the surface omniphobicity. Membranes coated with SiNPs and chemically modified by the FAS with a longer fluoroalkyl chain (or lower surface energy) exhibited excellent surface omniphobicity and showed wetting resistance to low surface tension liquids such as ethanol (22.1 mN m(-1)). We further evaluated performance of the membranes in desalination of saline feed solutions with varying surface tensions by membrane distillation (MD). The engineered membranes exhibited stable MD performance with low surface tension feed waters, demonstrating the potential application omniphobic membranes in desalinating complex, high salinity industrial wastewaters.

  5. Cell instructive microporous scaffolds through interface engineering

    PubMed Central

    Viswanathan, Priyalakshmi; Chirasatitsin, Somyot; Ngamkham, Kamolchanok; Engler, Adam J.; Battaglia, Giuseppe

    2013-01-01

    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 characterisation 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. PMID:23163574

  6. Bimodal mesoporous silica with bottleneck pores.

    PubMed

    Reber, M J; Brühwiler, D

    2015-11-01

    Bimodal mesoporous silica consisting of two sets of well-defined mesopores is synthesized by a partial pseudomorphic transformation of an ordered mesoporous starting material (SBA-15 type). The introduction of a second set of smaller mesopores (MCM-41 type) establishes a pore system with bottlenecks that restricts the access to the core of the bimodal mesoporous silica particles. The particle size and shape of the starting material are retained, but micropores present in the starting material disappear during the transformation, leading to a true bimodal mesoporous product. A varying degree of transformation allows the adjustment of the pore volume contribution of the two mesopore domains. Information on the accessibility of the mesopores is obtained by the adsorption of fluorescence-labeled poly(amidoamine) dendrimers and imaging by confocal laser scanning microscopy. This information is correlated with nitrogen sorption data to provide insights regarding the spatial distribution of the two mesopore domains. The bimodal mesoporous materials are excellent model systems for the investigation of cavitation effects in nitrogen desorption isotherms. PMID:26399172

  7. Highly Conductive Anion-Exchange Membranes from Microporous Tröger's Base Polymers.

    PubMed

    Yang, Zhengjin; Guo, Rui; Malpass-Evans, Richard; Carta, Mariolino; McKeown, Neil B; Guiver, Michael D; Wu, Liang; Xu, Tongwen

    2016-09-12

    The development of polymeric anion-exchange membranes (AEMs) combining high ion conductivity and long-term stability is a major challenge for materials chemistry. AEMs with regularly distributed fixed cationic groups, based on the formation of microporous polymers containing the V-shape rigid Tröger's base units, are reported for the first time. Despite their simple preparation, which involves only two synthetic steps using commercially available precursors, the polymers provide AEMs with exceptional hydroxide conductivity at relatively low ion-exchange capacity, as well as a high swelling resistance and chemical stability. An unprecedented hydroxide conductivity of 164.4 mS cm(-1) is obtained at a relatively a low ion-exchange capacity of 0.82 mmol g(-1) under optimal operating conditions. The exceptional anion conductivity appears related to the intrinsic microporosity of the charged polymer matrix, which facilitates rapid anion transport. PMID:27505421

  8. Surface texture and percolation effects in microporous oriented films of polyolefins

    NASA Astrophysics Data System (ADS)

    Novikov, D. V.; Kuryndin, I. S.; Bukošek, V.; Elyashevich, G. K.

    2012-11-01

    The surface structure of polypropylene and polyethylene microporous films prepared by the extrusion of the polymer melt with the subsequent stages of annealing, uniaxial extension, and thermal fixation of the samples has been analyzed using scanning electron microscopy. It has been shown that percolation through pores corresponds to the axial texture of the surface with the channel structure described by the fractal cluster model. The transition from open pores (through-flow channels) to closed pores leads to the formation of surface regions with a biaxial texture. An increase in the density of the solid phase cluster is accompanied by the formation of a homogeneous biaxial texture with a period of alternation of the density in two mutually perpendicular directions, one of which coincides with the direction of orientation of the films.

  9. Microporous Polymers from a Carbazole-Based Triptycene Monomer: Synthesis and Their Applications for Gas Uptake.

    PubMed

    Zhai, Tian-Long; Tan, Liangxiao; Luo, Yi; Liu, Jun-Min; Tan, Bien; Yang, Xiang-Liang; Xu, Hui-Bi; Zhang, Chun

    2016-01-01

    Two kinds of novel organic microporous polymers TCPs (TCP-A and TCP-B) were prepared by two cost-effective synthetic strategies from the monomer of tricarbazolyltriptycene (TCT). Their structure and properties were characterized by FT-IR, solid (13) C NMR, powder XRD, SEM, TEM, and gas absorption measurements. TCP-B displayed a high surface area (1469 m(2)  g(-1) ) and excellent H2 storage (1.70 wt % at 1 bar/77 K) and CO2 uptake abilities (16.1 wt % at 1 bar/273 K), which makes it a promising material for potential application in gas storage.

  10. 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.

  11. Silica nanoporous membranes and their applications

    NASA Astrophysics Data System (ADS)

    Khabibullin, Amir

    This thesis describes the development of novel silica and hybrid nanoporous membranes. Nanoporous membranes are widely used in various applications. This thesis focuses on their potential applications in the energy area, such as fuel cells and lithium batteries, and in separations and ultrafiltration. We use silica colloidal spheres and polymer-modified silica spheres to prepare the membranes in a time-, cost- and material-efficient manner. First, we prepared novel silica nanoporous membranes by pressing silica colloidal spheres followed by sintering. The pore size, the thickness, and the area of the membrane are precisely controlled by experiment parameters. The resulting membranes are mechanically and thermally durable, crack-free, and capable of size-selective transport. Next, to demonstrate the utility of the pressed membranes, described above, the proton-conductive pore-filled silica colloidal membranes were prepared and the fuel cells were constructed using these membranes. We modified these membranes by filling the membrane pores with surface-attached proton-conductive polymer brushes and prepared membrane-electrode assemblies to test fuel cell performance. We studied the proton conductivity and fuel cell performance as a function of the amount of sulfonic groups in the membrane. We also prepared and characterized reversible hybrid nanoporous membranes, self-assembled from solution containing polymer-modified silica colloidal spheres. Here we applied the new concept of noncovalent membranes, where the material is held together via noncovalent interactions of polymer brushes. This enables so-called reversible assembly of the membranes, in which membrane can be assembled in one solvent and dissolved in other. This approach provides advantages in recycling and reusing of the material. This work is one of the first of its kind and it opens a whole new area of research on reversible membranes made of polymer-modified nanoparticles. Finally, we applied our

  12. 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

  13. 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.

  14. 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.

  15. 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.

  16. 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

    2016-01-01

    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

  17. 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

  18. Molding mineral within microporous hydrogels by a polymer-induced liquid-precursor (PILP) process.

    PubMed

    Cheng, Xingguo; Gower, Laurie B

    2006-01-01

    Natural biominerals often have exquisite morphologies, where the cells exercise a high degree of crystallographic control through secretion of biological macromolecules and regulation of ion transport. One important example is the sea urchin spine. It has recently been shown to be formed through deposition of a transient amorphous calcium carbonate (ACC) precursor phase that later transforms to single-crystalline calcite, ultimately forming an elaborate three-dimensional microporous calcium carbonate structure with interconnected pores. Macromolecules associated with the mineral phase are thought to play a key role in regulating this transformation. The work described here mimics this type of morphological control by "molding" an amorphous calcium carbonate precursor within a porous poly(2-hydroxyethyl methacrylate) (PHEMA) hydrogel that has been prepared as a negative replica from the void space of an urchin spine. Using an acidic biomimetic polymer as a process-directing agent, we show that polyaspartic acid induces amorphous calcium carbonate (ACC) nanoparticles, which have fluidic character and therefore are able to infiltrate the PHEMA hydrogel replica and coalesce into the convoluted morphology that replicates the original microporous structure of the sea urchin spine. By "molding" calcium carbonate into a complex morphology at room temperature, using a precursor process that is induced by a biomimetic acidic macromolecule, the PILP process is a useful in vitro model for examining different aspects of the amorphous-to-crystalline transformation process that is apparently used by a variety of biomineralizing organisms. For example, although we were able to replicate the overall morphology of the spine, it had polycrystalline texture; further studies with this system will focus on controlling the nucleation event, which may help to elucidate how such a convoluted structure can be prepared with single-crystalline texture via an amorphous precursor. Through a

  19. Synthesis of ultrabright nanoporous fluorescent silica discoids using an inorganic silica precursor

    NASA Astrophysics Data System (ADS)

    Volkov, Dmytro O.; Cho, Eun-Bum; Sokolov, Igor

    2011-05-01

    The templated sol-gel synthesis of ultrabright fluorescent nanoporous silica particles based on the use of organic silica sources has previously been reported. The use of organosilanes as the main silica precursors has a number of issues, in particular, the low robustness of the synthesis due to instability of the organic silica source. Here we report on a novel synthesis of ultrabright fluorescent nanoporous silica discoids (a specific shape in-between the sphere and disk) of 3.1 +/- 0.7 microns in size, which were prepared using a stable inorganic sodium silicate silica source. Organic fluorescent dye Rhodamine 6G (R6G) was physically (non-covalently) entrapped inside cylindrical nanochannels of ~4-5 nm in diameter. In contrast to the synthesis with organic silica precursors, the obtained particles showed an excessive leakage of dye. To prevent this leakage, we modified the synthesis by adding a small amount of a secondary silica source. The synthesized particles show virtually no leakage, high photostability, and a brightness equivalent to the fluorescence of up to 7 × 107 free R6G molecules. This is about 7 times higher than the fluorescent brightness of particles of the same size made of CdSe/ZnS quantum dots, and 420 times higher than the brightness of the same volume of aqueous solution of free R6G dye.

  20. 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.

  1. 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.

  2. 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.

  3. Preparation of H{sub 2}-permselective silica membranes by alternating reactant deposition. Quarterly progress report, September 1, 1993--December 31, 1993

    SciTech Connect

    Kim, Soojin; Gavalas, G.R.

    1993-12-31

    Thin SiO{sub 2} layers were deposited on the surface of porous Vycor glass by alternating vapor phase reaction with SiCl{sub 4} and H{sub 2}O. The membranes prepared by this technique had H{sub 2} permeance of 0.3--0.4 cm{sup 3} (STP)/(min{center_dot}cm{sup 2}{center_dot}atm) and H{sub 2}:N{sub 2} selectivity of 500--1000 at 600{degrees}C. The SiCl{sub 4} dosage at each silylation cycle, the concentration of initial surface -OH groups, and the reaction temperature influence significantly the deposit layer thickness- After two weeks of heating at 550{degrees}C under 3 atmospheres of water vapor, the membrane H{sub 2} permeance decreased by about 20%, and the selectivity increased to more than 2000. The membrane properties after this hydrothermal treatment are superior to those of membranes prepared earlier by one-sided (steady flow) deposition. A simple model incorporating diffusion and surface reaction was used to study the effect of various parameters on the formation of the deposit layer.

  4. Properties of maxillofacial silicone elastomers reinforced with silica powder.

    PubMed

    Andreopoulos, A G; Evangelatou, M; Tarantili, P A

    1998-07-01

    Compounds of a silicone elastomer suitable for preparing maxillofacial prostheses, reinforced with various amounts of silica powder, have been studied for their mechanical response and wetting properties in terms of contact angle. Tensile strength and elongation at break showed an increase with increasing silica volume fraction up to 35%, whereas the Young modulus displayed small dependence on the silica content and the resistance to tear increased continuously with filler volume fraction (Vf). The wetting properties assessed via the contact angle, seemed to degrade with increasing silica Vf, but a dependence on the elastomer network density has also been recorded.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Silica, silicosis, and cancer

    SciTech Connect

    Goldsmith, D.F.; Winn, D.M.; Shy, C.M.

    1986-01-01

    These proceedings collect papers on occupational exposure. Topics include: measurement of silica dust, mortality in granite workers, effects of quartz in coal mine dust, pneumoconiosis, and lung cancer.

  13. 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.

  14. Chitosan-silica hybrid porous membranes.

    PubMed

    Pandis, Christos; Madeira, Sara; Matos, Joana; Kyritsis, Apostolos; Mano, João F; Ribelles, José Luis Gómez

    2014-09-01

    Chitosan-silica porous hybrids were prepared by a novel strategy in order to improve the mechanical properties of chitosan (CHT) in the hydrogel state. The inorganic silica phase was introduced by sol-gel reactions in acidic medium inside the pores of already prepared porous scaffolds. In order to make the scaffolds insoluble in acidic media chitosan was cross-linked by genipin (GEN) with an optimum GEN concentration of 3.2 wt.%. Sol-gel reactions took place with Tetraethylorthosilicate (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTMS) acting as silica precursors. GPTMS served also as a coupling agent between the free amino groups of chitosan and the silica network. The morphology study of the composite revealed that the silica phase appears as a layer covering the chitosan membrane pore walls. The mechanical properties of the hybrids were characterized by means of compressive stress-strain measurements. By immersion in water the hybrids exhibit an increase in elastic modulus up to two orders of magnitude. PMID:25063153

  15. 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.

  16. 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.

  17. Surfactant removal and silica condensation during the photochemical calcination of thin film silica mesophases.

    PubMed

    Dattelbaum, Andrew M; Amweg, Meri L; Ruiz, Julia D; Ecke, Laurel E; Shreve, Andrew P; Parikh, Atul N

    2005-08-01

    The evolution of photochemical surfactant removal and silica condensation from organically templated thin film silica nanocomposites with mesoscopic ordering has been probed using a combined application of Fourier transform infrared (FT-IR) spectroscopy and single wavelength ellipsometry. Thin films of silica nanocomposites were prepared by a previously reported evaporation-induced self-assembly process. Specifically, oxidized silicon and gold substrates were withdrawn at 25 mm/min from a subcritical micelle concentration solution containing an ethylene oxide surfactant as a structure-directing agent and tetraethyl orthosilicate as a silica precursor. Real-time grazing incidence difference FT-IR spectra of the nanocomposite films on gold taken during exposure to short-wavelength ultraviolet light (184-257 nm) show that surfactant removal and silica condensation occur gradually and concomitantly. Surfactant removal and silica reconstructions were found to be nearly complete after 90 min of exposure. Further, a transient feature was observed in the FT-IR spectra around 1713 cm(-1) during the UV exposure process and was assigned to a carbonyl (C=O) stretching mode absorption, reflecting the transient formation of a partially oxidized surfactant intermediate. From these data we propose a stepwise model for surfactant removal from the nanocomposite films. Ellipsometrically determined index of refraction values collected as a function of UV exposure are also shown to support such a stepwise mechanism of surfactant removal from the ordered nanocomposite silica thin film mesophases studied here. PMID:16852834

  18. Silica-metal core-shell nanostructures.

    PubMed

    Jankiewicz, B J; Jamiola, D; Choma, J; Jaroniec, M

    2012-01-15

    Silica-metal nanostructures consisting of silica cores and metal nanoshells attract a lot of attention because of their unique properties and potential applications ranging from catalysis and biosensing to optical devices and medicine. The important feature of these nanostructures is the possibility of controlling their properties by the variation of their geometry, shell morphology and shell material. This review is devoted to silica-noble metal core-shell nanostructures; specifically, it outlines the main methods used for the preparation and surface modification of silica particles and presents the major strategies for the formation of metal nanoshells on the modified silica particles. A special emphasis is given to the Stöber method, which is relatively simple, effective and well verified for the synthesis of large and highly uniform silica particles (with diameters from 100 nm to a few microns). Next, the surface chemistry of these particles is discussed with a special focus on the attachment of specific organic groups such as aminopropyl or mercaptopropyl groups, which interact strongly with metal species. Finally, the synthesis, characterization and application of various silica-metal core-shell nanostructures are reviewed, especially in relation to the siliceous cores with gold or silver nanoshells. Nowadays, gold is most often used metal for the formation of nanoshells due to its beneficial properties for many applications. However, other metals such as silver, platinum, palladium, nickel and copper were also used for fabrication of core-shell nanostructures. Silica-metal nanostructures can be prepared using various methods, for instance, (i) growth of metal nanoshells on the siliceous cores with deposited metal nanoparticles, (ii) reduction of metal species accompanied by precipitation of metal nanoparticles on the modified silica cores, and (iii) formation of metal nanoshells under ultrasonic conditions. A special emphasis is given to the seed

  19. Poroelastic theory applied to the adsorption-induced deformation of vitreous silica.

    PubMed

    Coasne, Benoit; Weigel, Coralie; Polian, Alain; Kint, Mathieu; Rouquette, Jérome; Haines, Julien; Foret, Marie; Vacher, René; Rufflé, Benoit

    2014-12-11

    When vitreous silica is submitted to high pressures under a helium atmosphere, the change in volume observed is much smaller than expected from its elastic properties. It results from helium penetration into the interstitial free volume of the glass network. We present here the results of concurrent spectroscopic experiments using either helium or neon and molecular simulations relating the amount of gas adsorbed to the strain of the network. We show that a generalized poromechanical approach, describing the elastic properties of microporous materials upon adsorption, can be applied successfully to silica glass in which the free volume exists only at the subnanometer scale. In that picture, the adsorption-induced deformation accounts for the small apparent compressibility of silica observed in experiments. PMID:25383694

  20. Thermodynamics and transport in microporous media. Progress report

    SciTech Connect

    Glandt, E.D.

    1992-09-01

    Focus of this report is on the thermodynamic properties/behavior of fluids contained or adsorbed on the random microporus materials (disordered solids). The Madden-Glandt formalism for fluids in disordered matrices is applied to realistic systems (gas adsorption in carbons, polymer partitioning). Work on microgeometry of solids and their percolation and connectedness properties was continued; a study of the simplest model for microporous materials (random-pore or ``Swiss cheese`` model) was completed. Work on irreversible adsorption was continued; a simple model for correlated adsorption was studied.

  1. 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.

  2. Construction of nano- and microporous frameworks from octahedral bubble clusters.

    PubMed

    Woodley, S M; Watkins, M B; Sokol, A A; Shevlin, S A; Catlow, C R A

    2009-05-01

    We report a general method of constructing microporous, cubic frameworks from eight different high symmetry small clusters of ZnO, which were previously predicted via the application of an evolutionary algorithm. Using interatomic potentials, the lattice energies of the structures formed are computed. We analyse the relative stabilities within particular subsets of these periodic structures, and show that frameworks constructed from edge-sharing units of clusters with the T(h) point group are predicted to be much more stable than those with T(d). Our results have general implications for the nanostructures of systems whose bulk structures are based on tetrahedral coordination.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Characterization of vanadium/silica and copper/silica aerogel catalysts

    SciTech Connect

    Owens, L.; Tillotson, T.M.; Hair, L.M.

    1995-09-01

    Vanadium/silica and copper/silica aerogels have been prepared using the sol-gel method followed by CO{sub 2} exchange and supercritical extraction. Structural properties of samples supercritically dried, oxidized and used in reactions studies conducted with a feed representing the average composition of automobile exhaust from a lean burn engine were investigated using laser Raman spectroscopy and temperature-programmed reduction. No evidence of crystalline V{sub 2}O{sub 5} was found for the vanadium/silica aerogel, freshly extracted, oxidized or following exposure to reaction conditions using these techniques. However, results obtained for the copper/silica sample indicate that changes in the structure of the copper species had occurred as the sample was oxidized and exposed to reaction conditions.

  8. 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

  9. Observation of microporous cesium salts of 12-tungstosilicic acid using scanning transmission electron microscopy.

    PubMed

    Hiyoshi, Norihito; Kamiya, Yuichi

    2015-06-21

    Heteropolyanions and their arrays in microporous cesium salts of 12-tungstosilicic acid, Cs2.5H1.5[SiW12O40] and Cs4.0[SiW12O40], were observed by aberration-corrected scanning transmission electron microscopy. Microstructures that form micropores in the polyoxometalates were visualized.

  10. Impact of mineral micropores on transport and fate of organic contaminants: a review.

    PubMed

    Cheng, Hefa; Hu, Erdan; Hu, Yuanan

    2012-03-15

    Nanometer-scale pores are abundant in porous geological media (soils, sediments, and aquifer materials), and may account for over >90% of total mineral surface areas. Sorption of organic contaminants in mineral micropores (<2 nm) plays a key role in controlling their fate and transport when the porous geological media have very low organic carbon contents (<0.1%). Significant adsorption of hydrophobic organic contaminants could only occur in the hydrophobic micropore spaces because of the strong competition from water. The rate of desorption from micropores is very slow due to hindered diffusion, resulting in distinct two-stage desorption behavior for microporous solids. Size exclusion effect prevents micropore-sorbed contaminants from being accessed by microorganisms and their extracellular enzymes, thus reducing their bioavailability and biodegradation rates. Results from recent studies indicate that sorption in micropores can also inhibit abiotic degradation of reactive contaminants by protecting them in confined spaces with little reactive water, slowing down hydrolysis and other water-mediated transformations. As a result of the inhibitory effect on abiotic and biotic transformations, and the slow desorption due to hindered diffusion, sorption in hydrophobic micropores of porous geological media can cause preservation of anthropogenic organic contaminants in the subsurface and may increase their persistence to the time scale of geological ages under appropriate conditions. From a practical perspective, understanding the role of mineral micropores is important in assessing the long-term ecotoxicological risk of organic contaminants in the subsurface and designing remediation strategies.

  11. Submicroporous/microporous and compatible/incompatible multi-functional dual-layer polymer electrolytes and their interfacial characteristics with lithium metal anode

    NASA Astrophysics Data System (ADS)

    Lee, Young-Gi; Kyhm, Kwangseuk; Choi, Nam-Soon; Ryu, Kwang Sun

    A novel multi-functional dual-layer polymer electrolyte was prepared by impregnating the interconnected pores with an ethylene carbonate (EC)/dimethyl carbonate (DMC)/lithium hexafluorophosphate (LiPF 6) solution. An incompatible layer is based on a microporous polyethylene (PE) and a compatible layer, based on a poly(vinylidenefluoride-co-hexafluoropropylene) (P(VdF-co-HFP)) is sub-microporous and compatible with an electrolyte solution. The Li electrode/the dual-layer polymer electrolyte/Li[Ni 0.15Li 0.23M n0.62]O 2 cell showed stable cycle performance under prolonged cycle number. This behavior is due to the enhanced compatibility between the matrix polymer and the liquid electrolytes within the submicroporous compatible layer, which could lead to a controlled Li + deposition on the Li anode surface by forming homegeneous electrolyte zone near the anode.

  12. Improved bioresorbable microporous intravascular stents for gene therapy.

    PubMed

    Ye, Y W; Landau, C; Meidell, R S; Willard, J E; Moskowitz, A; Aziz, S; Carlisle, E; Nelson, K; Eberhart, R C

    1996-01-01

    Drug imbibing microporous stents are under development at a number of centers to enhance healing of the arterial wall after balloon coronary angioplasty procedures. The authors improved the mechanical strength and reservoir properties of a biodegradable microporous stent reported to this Society in 1994. A combined tubular/helical coil stent is readily fabricated by flotation/precipitation and casting/ winding techniques. A two stage solvent swelling technique allows precise adjustment of the surface hydrophilic/hydrophobic balance. These developments permit seven-fold improvement in drug capacity without significantly altering mechanical properties. Stents modified in this manner retain tensile and compressive strength and are suitable for remote deployment. Elution kinetics of these modified stents suggest they are suitable for gene delivery. Successful gene transfer and transmural expression have been demonstrated after implantation of stents impregnated with a recombinant adenovirus carrying a nuclear localizing beta-galactosidase reporter gene into rabbit carotid arteries. These studies suggest that surface modified, bioresorbable polymer stents ultimately may be useful adjunctive devices for gene transfer during percutaneous transluminal revascularization.

  13. Osteoinductive silk-silica composite biomaterials for bone regeneration

    PubMed Central

    Mieszawska, Aneta J.; Fourligas, Nikolaos; Georgakoudi, Irene; Ouhib, Nadia; Belton, David J.; Perry, Carole C.; Kaplan, David L.

    2010-01-01

    Osteoinductive and biodegradable composite biomaterials for bone regeneration were prepared by combining silk fibroin with silica particles. The influence of these composite systems on osteogenesis was evaluated with human mesenchymal stem cells (hMSCs) subjected to osteogenic differentiation. hMSCs adhered, proliferated, and differentiated towards osteogenic lineages on silk/silica films. The addition of the silica to the silk films influenced gene expression leading to upregulation of bone sialoprotein (BSP) and collagen type 1 (Col 1) osteogenic markers. Evidence for early bone formation in the form of collagen fibers and apatite nodules was obtained on the silk/silica films. Collagen fibers were closely associated with apatite deposits and overall collagen content was higher for the silica containing samples. Also, smaller sized silica particles (24 nm – 2 μm) with large surface area facilitated silica biodegradation in vitro through particle dissolution, leading to ~5 fold decrease in silica content over 10 weeks. These results indicate suitability of silk/silica composite system towards bone regeneration, where degradation/remodeling rates of the organic and inorganic components can be controlled. PMID:20817293

  14. Preparation of a compressible and hierarchically porous polyimide sponge via the sol-gel process of an aliphatic tetracarboxylic dianhydride and an aromatic triamine.

    PubMed

    Lee, Jeongmin; Chang, Ji Young

    2016-08-16

    A compressible and monolithic microporous polyimide sponge was prepared from an aliphatic tetracarboxylic dianhydride and an aromatic triamine. The sponge had a hierarchical pore structure, in which spherical microporous polyimide particles were interconnected to form a macroscopic network. It showed an amphiphilic character, because of the balanced presence of hydrophobic and hydrophilic groups. PMID:27484707

  15. 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. PMID:26979477

  16. Hard magnetism in structurally engineered silica nanocomposite.

    PubMed

    Song, Hyon-Min; Zink, Jeffrey I

    2016-09-21

    Creation of structural complexity by simple experimental control will be an attractive approach for the preparation of nanomaterials, as a classical bottom-up method is supplemented by a more efficient and more direct artificial engineering method. In this study, structural manipulation of MCM-41 type mesoporous silica is investigated by generating and imbedding hard magnetic CoFe2O4 nanoparticles into mesoporous silica. Depending on the heating rate and target temperature, mesoporous silica undergoes a transformation in shape to form hollow silica, framed silica with interior voids, or melted silica with intact mesostructures. Magnetism is governed by the major CoFe2O4 phase, and it is affected by antiferromagnetic hematite (α-Fe2O3) and olivine-type cobalt silicate (Co2SiO4), as seen in its paramagnetic behavior at the annealing temperature of 430 °C. The early formation of Co2SiO4 than what is usually observed implies the effect of the partial substitution of Fe in the sites of Co. Under slow heating (2.5 °C min(-1)) mesostructures are preserved, but with significantly smaller mesopores (d100 = 1.5 nm). In addition, nonstoichiometric CoxFe1-xO with metal vacancies at 600 °C, and spinel Co3O4 at 700 °C accompany major CoFe2O4. The amorphous nature of silica matrix is thought to contribute significantly to these structurally diverse and rich phases, enabled by off-stoichiometry between Si and O, and accelerated by the diffusion of metal cations into SiO4 polyhedra at an elevated temperature. PMID:27537252

  17. Hard magnetism in structurally engineered silica nanocomposite.

    PubMed

    Song, Hyon-Min; Zink, Jeffrey I

    2016-09-21

    Creation of structural complexity by simple experimental control will be an attractive approach for the preparation of nanomaterials, as a classical bottom-up method is supplemented by a more efficient and more direct artificial engineering method. In this study, structural manipulation of MCM-41 type mesoporous silica is investigated by generating and imbedding hard magnetic CoFe2O4 nanoparticles into mesoporous silica. Depending on the heating rate and target temperature, mesoporous silica undergoes a transformation in shape to form hollow silica, framed silica with interior voids, or melted silica with intact mesostructures. Magnetism is governed by the major CoFe2O4 phase, and it is affected by antiferromagnetic hematite (α-Fe2O3) and olivine-type cobalt silicate (Co2SiO4), as seen in its paramagnetic behavior at the annealing temperature of 430 °C. The early formation of Co2SiO4 than what is usually observed implies the effect of the partial substitution of Fe in the sites of Co. Under slow heating (2.5 °C min(-1)) mesostructures are preserved, but with significantly smaller mesopores (d100 = 1.5 nm). In addition, nonstoichiometric CoxFe1-xO with metal vacancies at 600 °C, and spinel Co3O4 at 700 °C accompany major CoFe2O4. The amorphous nature of silica matrix is thought to contribute significantly to these structurally diverse and rich phases, enabled by off-stoichiometry between Si and O, and accelerated by the diffusion of metal cations into SiO4 polyhedra at an elevated temperature.

  18. Silica Embedded Metal Hydrides

    SciTech Connect

    Heung, L.K.; Wicks, G.G.

    1998-08-01

    A method to produce silica embedded metal hydride was developed. The product is a composite in which metal hydride particles are embedded in a matrix of silica. The silica matrix is highly porous. Hydrogen gas can easily reach the embedded metal hydride particles. The pores are small so that the metal hydride particles cannot leave the matrix. The porous matrix also protects the metal hydride particles from larger and reactive molecules such as oxygen, since the larger gas molecules cannot pass through the small pores easily. Tests show that granules of this composite can absorb hydrogen readily and withstand many cycles without making fines.

  19. Fluoride Release from Hollow Silica Microsphere-Containing Dental Restorative Acrylate Resin.

    PubMed

    Ji, Yuqin; Gao, Jun; Yin, Hengbo; Wang, Aili; Jiang, Tingshun; Wu, Gang; Wu, Zhanao

    2015-05-01

    Hollow silica microspheres with mesoporous shells were prepared by the sacrificial template method. Hollow silica microsphere-containing acrylate resin-based dental restoration materials were prepared by using hollow silica microspheres as NaF reservoirs. Fluoride release performances from naked hollow silica microspheres, acrylate resin, and hollow silica microsphere-containing acrylate resin-based dental restorative materials in an artificial saliva were investigated. The results showed that hollow silica microsphere-containing acrylate resin-based dental restorative materials had higher cumulative fluoride release quantities and sustained fluoride release rates than traditional acrylate resin-based dental restorative materials. Fluoride release could be tuned by changing the mesoporous shell thickness of hollow silica microsphere.

  20. The use of Reactive Ion Etching for obtaining “free” silica nano test tubes

    NASA Astrophysics Data System (ADS)

    Buyukserin, Fatih; Martin, Charles R.

    2010-10-01

    Silica nano test tubes are one-dimensional inorganic nanostructures with several biotechnological applications including biosensing, magnetic resonance imaging, and targeted cancer therapeutics. They are generally prepared by sol-gel deposition of silica to nanoporous alumina templates. Preparing samples composed of isolated free silica nano test tubes can be a challenging process due to the conformal coating of silica on the template. This causes the formation of a top-surface silica layer which laterally connects the nano test tubes. Herein, we detailed the use of Reactive Ion Etching to remove this top-surface silica layer which yields free silica nano test tubes with template dissolution. Compared with the mechanical polishing approach, Reactive Ion Etching treatment allows a fine manipulation ability of the surface material at the nanoscale level. When used excessively, Reactive Ion Etching causes an orifice closing phenomenon that may be employed to create novel one-dimensional nanocapsules.

  1. 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. PMID:24410024

  2. Organosiloxane reactivity on dehydroxylated silica surfaces

    SciTech Connect

    Grabbe, A.; Michalske, T.A.

    1995-12-31

    In most cases, the surface reactivity of silica glass is controlled by the presence of silanol groups. However, glass surfaces that are produced by high temperature forming processes possess little if any silanol groups. Previous work demonstrated that the reactivity of glass surfaces formed at high temperature is controlled by the existence of strained siloxane rings. In this study, the authors conducted experiments on highly dehydroxylated silica powder surfaces and silica surfaces that were formed directly from the melt to explore the reactivity of strained siloxane rings with various organosiloxanes reactants. The authors use infrared spectrometry to show that strained dimer rings react with organosiloxane molecules or with water at comparable rates, depending on the structure of the organosiloxane. The data indicate that the important features of the reacting molecule are its polarity, steric accessibility and bond strain. Since the measured reactions require approximately six orders of magnitude of gas exposure to go from 1% to 99% completion, these data present strong evidence that the surface is highly heterogeneous. By applying a linear distribution of activation energies, the authors estimate that spread in activation energy to be approximately 40 kJ/mole. In this presentation, the authors discuss the implications of this newly discovered silica chemistry for novel approaches to tailor melt-formed surfaces for improved polymer adhesion and hydrolytic stability. They will also discuss efforts to prepare true melt-formed surfaces by blowing bubbles of silica in a vacuum environment.

  3. Electrochemical Sensors: Functionalized Silica

    SciTech Connect

    Fryxell, Glen E.; Lin, Yuehe; Yantasee, Wassana

    2009-03-24

    This chapter summarizes recent devellopment of electrochemical sensors based on functionlized mesoporous silica materials. The nanomatrials based sensors have been developed for sensitive and selective enrironmental detection of toxic heavy metal and uranium ions.

  4. Adsorption Characteristics of Silica Gels Treated with Fluorinated Silylation Agents

    PubMed

    Monde; Nakayama; Yano; Yoko; Konakahara

    1997-01-01

    Branched-chain polyfluorosilane (monochlorodimethyl[4,4-bis(trifluoromethyl)-5,5,6,6,7,7,7-heptafluoroheptyl)-bonded silica gels were prepared. The surface properties of the silica gels modified with various organic silanes were evaluated by the adsorption density of polar and nonpolar gases calculated from adsorption isotherms of nitrogen, carbon dioxide, and normal butane gases. The polyfluorocarbon-bonded silica gel surface was found to be both hydrophobic and oleophobic in nature, whereas the hydrocarbon-bonded silica gel surface was characterized only as hydrophobic. The trifunctional fluorinated silane provides the silica gel surface with a more hydrophilic nature than the monofunctional silane because of the formation of a denser polymeric coating layer with a larger number of silanols. PMID:9056313

  5. Adsorption Characteristics of Silica Gels Treated with Fluorinated Silylation Agents

    PubMed

    Monde; Nakayama; Yano; Yoko; Konakahara

    1997-01-01

    Branched-chain polyfluorosilane (monochlorodimethyl[4,4-bis(trifluoromethyl)-5,5,6,6,7,7,7-heptafluoroheptyl)-bonded silica gels were prepared. The surface properties of the silica gels modified with various organic silanes were evaluated by the adsorption density of polar and nonpolar gases calculated from adsorption isotherms of nitrogen, carbon dioxide, and normal butane gases. The polyfluorocarbon-bonded silica gel surface was found to be both hydrophobic and oleophobic in nature, whereas the hydrocarbon-bonded silica gel surface was characterized only as hydrophobic. The trifunctional fluorinated silane provides the silica gel surface with a more hydrophilic nature than the monofunctional silane because of the formation of a denser polymeric coating layer with a larger number of silanols.

  6. Evaluation of occupational exposure to free silica in Alberta foundries.

    PubMed

    Ayalp, A; Myroniuk, D

    1982-11-01

    The Occupational Hygiene Branch of Alberta Workers' Health, Safety and Compensation conducted a comprehensive study of the foundry industry in Alberta. The surveys assessed both the degree of health hazards present and the effectiveness of existing control systems for airborne contaminants. All nine of Alberta's ferrous foundries were surveyed in the course of the project. The foundries varied from those which were small with limited mechanization to those which were large and highly automated. The concentrations of free silica in the work environment are correlated to the different attempts to control silica using substitution and various ventilation systems. The particular foundry processes evaluated for airborne free silica were sand preparation, shakeout, dry sand transport and sand molding. Workers' exposure to free airborne silica was evaluated by personal and area samples. The free silica content of the samples was determined by infra-red spectrophotometry. The results indicated most control systems were inadequate. Effective control methods are described to reduce the health hazard.

  7. Crystalline Silica Primer

    USGS Publications Warehouse

    ,

    1992-01-01

    substance and will present a nontechnical overview of the techniques used to measure crystalline silica. Because this primer is meant to be a starting point for anyone interested in learning more about crystalline silica, a list of selected readings and other resources is included. The detailed glossary, which defines many terms that are beyond the scope of this publication, is designed to help the reader move from this presentation to a more technical one, the inevitable next step.

  8. Effects of temperature on trichloroethylene desorption from silica gel and natural sediments. 1. Isotherms

    SciTech Connect

    Werth, C.J.; Reinhard, M.

    1997-03-01

    Aqueous phase isotherms were calculated from vapor phase desorption isotherms measured at 15, 30, and 60{degree}C for trichloroethylene on a silica gel, an aquifer sediment, a soil, a sand fraction, and a clay and silt fraction, all at 100% relative humidity. Isosteric heats of adsorption (Q{sub st}(q)) were calculated as a function of the sorbed concentration, q, and examined with respect to the following mechanisms: adsorption on water wet mineral surfaces, sorption in amorphous organic matter (AOM), and adsorption in hydrophobic micropores. Silica gel, sand fraction, and clay and silt fraction 60{degree}C isotherms are characterized by a Freundlich region and a region at very low concentrations where isotherm points deviate from log-log linear behavior. The latter is designated the non-Freundlich region. For the silica gel, values of Q{sub st}(q) (9.5-45 kJ/mol) in both regions are consistent with adsorption in hydrophobic micropores. For the natural solids, values of Q{sub st}(q) in the Freundlich regions are less than or equal to zero and are consistent with sorption on water wet mineral surfaces and in AOM. In the non-Freundlich regions, diverging different temperature isotherms with decreasing q and Q{sub st}(q) value of 34 kJ/mol for the clay and silt fraction suggest that adsorption is occurring in hydrophobic micropores. The General Adsorption Isotherm is used to capture this adsorption heterogeneity. 57 refs., 5 figs., 2 tabs.

  9. Suppression of secondary electron yield by micro-porous array structure

    NASA Astrophysics Data System (ADS)

    Ye, M.; He, Y. N.; Hu, S. G.; Wang, R.; Hu, T. C.; Yang, J.; Cui, W. Z.

    2013-02-01

    We study secondary electron yield (SEY) suppression for metal materials using a roughened surface with a micro-porous array. First, we perform a Monte Carlo simulation of the electron trajectory in a single cylindrical well using a phenomenological model of secondary electron emission and the SEY suppression efficiency of a micro-porous array. The simulation results show that the SEY of a roughened surface is affected significantly by the aspect ratio of the micro-pores and the surface porosity of the metal plate. Then, to verify the simulation results, we produce a micro-porous array on metal plates using photolithography and measure their SEYs. We show that the micro-porous array structure can efficiently suppress the SEY of metal materials, and the measurements agree quantitatively with the corresponding simulation results. Finally, we derive an analytical formula to evaluate easily the SEY suppression efficiency of the Ag micro-porous array. In total, the micro-porous array proposed in this paper offers an alternative to SEY suppression in related areas such as multipactor effects in satellite payloads or electron cloud effects in accelerators.

  10. Suppression of secondary electron yield by micro-porous array structure

    SciTech Connect

    Ye, M.; He, Y. N.; Hu, S. G.; Wang, R.; Hu, T. C.; Yang, J.; Cui, W. Z.

    2013-02-21

    We study secondary electron yield (SEY) suppression for metal materials using a roughened surface with a micro-porous array. First, we perform a Monte Carlo simulation of the electron trajectory in a single cylindrical well using a phenomenological model of secondary electron emission and the SEY suppression efficiency of a micro-porous array. The simulation results show that the SEY of a roughened surface is affected significantly by the aspect ratio of the micro-pores and the surface porosity of the metal plate. Then, to verify the simulation results, we produce a micro-porous array on metal plates using photolithography and measure their SEYs. We show that the micro-porous array structure can efficiently suppress the SEY of metal materials, and the measurements agree quantitatively with the corresponding simulation results. Finally, we derive an analytical formula to evaluate easily the SEY suppression efficiency of the Ag micro-porous array. In total, the micro-porous array proposed in this paper offers an alternative to SEY suppression in related areas such as multipactor effects in satellite payloads or electron cloud effects in accelerators.

  11. 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.

  12. A three-dimensional microporous coordination polymer with fluorescent property

    NASA Astrophysics Data System (ADS)

    Gao, Chaoying; Liu, Shuxia; Xie, Linhua; Ren, Yuanhang; Cao, Ruige; Cao, Jianfang; Zhao, Xinyu

    2008-11-01

    A microporous metal-organic coordination polymer formulated as [Cd 2(btec)(H 2O) 2]·0.8DMF (1), where btec = 1,2,4,5-benzenetetracarboxylate and DMF = N, N-dimethylformamide, has been isolated under solvothermal condition and characterized by elemental analyses, IR, thermal stability analysis, fluorescent spectrum, and single-crystal X-ray diffraction analysis. The framework in 1 possesses a three-dimensional architecture with ordered one-dimensional rhombus channels, the dimensions of channels are approximately 10 Å at the widest and 3 Å at the narrowest spacing considering the van der Waal radii of atoms in the framework running along the a-axis. Furthermore, compound 1 shows intense photoluminescent property at room temperature.

  13. 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.

  14. 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.

  15. Nanoscale encapsulation: the structure of cations in hydrophobic microporous aluminosilicates

    SciTech Connect

    Wasserman, S.R.; Yuchs, S.E.; Giaquinta, D.; Soderholm, L.; Song, Kang

    1996-10-01

    Hydrophobic microporous aluminosilicates, created by organic surface modification of inherently hydrophilic materials such as zeolites and clays, are currently being investigated as storage media for hazardous cations. Use of organic monolayers to modify the surface of an aluminosilicate after introducing an ion into the zeolite/clay reduces the interaction of water with the material. Resulting systems are about 20 times more resistant to leaching of stored ion. XAS spectra from the encapsulated ion demonstrate that byproducts from the organic modifier can complex with the stored cation. This complexation can result in a decreased affinity of the cation for the aluminosilicate matrix. Changing the organic modifier eliminates this problem. XAS spectra also indicate that the reactivity and speciation of the encapsulated ion may change upon application of the hydrophobic layer.

  16. Electrochemically Produced Graphene for Microporous Layers in Fuel Cells.

    PubMed

    Najafabadi, Amin Taheri; Leeuwner, Magrieta J; Wilkinson, David P; Gyenge, Előd L

    2016-07-01

    The microporous layer (MPL) is a key cathodic component in proton exchange membrane fuel cells owing to its beneficial influence on two-phase mass transfer. However, its performance is highly dependent on material properties such as morphology, porous structure, and electrical resistance. To improve water management and performance, electrochemically exfoliated graphene (EGN) microsheets are considered as an alternative to the conventional carbon black (CB) MPLs. The EGN-based MPLs decrease the kinetic overpotential and the Ohmic potential loss, whereas the addition of CB to form a composite EGN+CB MPL improves the mass-transport limiting current density drastically. This is reflected by increases of approximately 30 and 70 % in peak power densities at 100 % relative humidity (RH) compared with those for CB- and EGN-only MPLs, respectively. The composite EGN+CB MPL also retains the superior performance at a cathode RH of 20 %, whereas the CB MPL shows significant performance loss. PMID:27254459

  17. 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.

  18. Silica, hybrid silica, hydride silica and non-silica stationary phases for liquid chromatography.

    PubMed

    Borges, Endler M

    2015-04-01

    Free silanols on the surface of silica are the "villains", which are responsible for detrimental interactions of those compounds and the stationary phase (i.e., bad peak shape, low efficiency) as well as low thermal and chemical stability. For these reasons, we began this review describing new silica and hybrid silica stationary phases, which have reduced and/or shielded silanols. At present, in liquid chromatography for the majority of analyses, reversed-phase liquid chromatography is the separation mode of choice. However, the needs for increased selectivity and increased retention of hydrophilic bases have substantially increased the interest in hydrophilic interaction chromatography (HILIC). Therefore, stationary phases and this mode of separation are discussed. Then, non-silica stationary phases (i.e., zirconium oxide, titanium oxide, alumina and porous graphitized carbon), which afford increased thermal and chemical stability and also selectivity different from those obtained with silica and hybrid silica, are discussed. In addition, the use of these materials in HILIC is also reviewed.

  19. Kinetic modelling of molecular hydrogen transport in microporous carbon materials.

    SciTech Connect

    Hankel, M.; Zhang, H.; Nguyen, T. X.; Bhatia, S. K.; Gray, S. K.; Smith, S. C.

    2011-01-01

    The proposal of kinetic molecular sieving of hydrogen isotopes is explored by employing statistical rate theory methods to describe the kinetics of molecular hydrogen transport in model microporous carbon structures. A Lennard-Jones atom-atom interaction potential is utilized for the description of the interactions between H{sub 2}/D{sub 2} and the carbon framework, while the requisite partition functions describing the thermal flux of molecules through the transition state are calculated quantum mechanically in view of the low temperatures involved in the proposed kinetic molecular sieving application. Predicted kinetic isotope effects for initial passage from the gas phase into the first pore mouth are consistent with expectations from previous modeling studies, namely, that at sufficiently low temperatures and for sufficiently narrow pore mouths D{sub 2} transport is dramatically favored over H{sub 2}. However, in contrast to expectations from previous modeling, the absence of any potential barrier along the minimum energy pathway from the gas phase into the first pore mouth yields a negative temperature dependence in the predicted absolute rate coefficients - implying a negative activation energy. In pursuit of the effective activation barrier, we find that the minimum potential in the cavity is significantly higher than in the pore mouth for nanotube-shaped models, throwing into question the common assumption that passage through the pore mouths should be the rate-determining step. Our results suggest a new mechanism that, depending on the size and shape of the cavity, the thermal activation barrier may lie in the cavity rather than at the pore mouth. As a consequence, design strategies for achieving quantum-mediated kinetic molecular sieving of H{sub 2}/D{sub 2} in a microporous membrane will need, at the very least, to take careful account of cavity shape and size in addition to pore-mouth size in order to ensure that the selective step, namely passage

  20. Hierarchical control of porous silica by pH adjustment: Alkyl polyamines as surfactants for bimodal silica synthesis and its carbon replica

    NASA Astrophysics Data System (ADS)

    Abellán, G.; Carrillo, A. I.; Linares, N.; Serrano, E.; García-Martínez, J.

    2009-08-01

    Bimodal macro-mesoporous silica networks have been prepared in a simple one-pot synthesis using an inexpensive tetramine surfactant and tetraethoxysilane as a silica precursor. These novel materials show high pore volumes and templated mesopores (average pore size 3.0 nm) embedded in 20 nm thick walls forming interparticle large meso/macropores. The judicious control of the pH during the silica formation allows for the precise control of the interparticle condensation, likely due to the change in the interaction between the tetramine surfactant and the silica precursors. Finally, a highly porous carbon replica with bimodal porosity was prepared by using the bimodal silica as a hard sacrificial template. The microstructure of the silica template was accurately transferred to the carbon material obtaining high surface areas (up to 1300 m 2 g -1) and total pore volumes ≥2 cm 3 g -1.