scholarly journals Highly Active Ruthenium Catalyst Supported on Magnetically Separable Mesoporous Organosilica Nanoparticles

2020 ◽  
Vol 10 (17) ◽  
pp. 5769
Author(s):  
Suheir Omar ◽  
Raed Abu-Reziq

A facile and direct method for synthesizing magnetic periodic mesoporous organosilica nanoparticles from pure organosilane precursors is described. Magnetic ethylene- and phenylene-bridged periodic mesoporous organosilica nanoparticles (PMO NPs) were prepared by nanoemulsification techniques. For fabricating magnetic ethylene- or phenylene-bridged PMO NPs, hydrophobic magnetic nanoparticles in an oil-in-water (o/w) emulsion were prepared, followed by a sol–gel condensation of the incorporated bridged organosilane precursor (1,2 bis(triethoxysilyl)ethane or 1,4 bis(triethoxysilyl)benzene), respectively. The resulting materials were characterized using high-resolution scanning electron microscopy (HR-SEM), high-resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray (EDX) spectroscopy, powder X-ray diffraction (XRD), solid-state NMR analysis, and nitrogen sorption analysis (N2-BET). The magnetic ethylene-bridged PMO NPs were successfully loaded using a ruthenium oxide catalyst by means of sonication and evaporation under mild conditions. The obtained catalytic system, termed Ru@M-Ethylene-PMO NPS, was applied in a reduction reaction of aromatic compounds. It exhibited very high catalytic behavior with easy separation from the reaction medium by applying an external magnetic field.

2020 ◽  
Vol 10 (17) ◽  
pp. 5960
Author(s):  
Suheir Omar ◽  
Raed Abu-Reziq

We describe, for the first time, a successful strategy for synthesizing chiral periodic mesoporous organosilica nanoparticles (PMO NPs). The chiral PMO nanoparticles were synthesized in a sol–gel process under mild conditions; their preparation was mediated by hydrolysis and condensation of chiral-bridged organo-alkoxysilane precursor compounds, (OR‘)3Si-R-Si(OR‘)3, in the presence of cetyltrimethylammonium bromide (CTAB) surfactant. The resulting nanoparticles were composed merely from a chiral- bridged organo-alkoxysilane monomer. These systems were prepared by applying different surfactants and ligands that finally afforded monodispersed chiral PMO NPs consisting of 100% bridged-organosilane precursor. In addition, the major advancement that was achieved here was, for the first time, success in preparing magnetic chiral PMO NPs. These nanoparticles were synthesized by the co-polymerization of 1,1′-((1R,2R)-1,2-diphenylethane-1,2-diyl)bis(3-(3-(triethoxysilyl) propyl) urea) chiral monomer by an oil in water (o/w) emulsion process, to afford magnetic chiral PMO NPs with magnetite NPs in their cores. The obtained materials were characterized with high-resolution scanning electron microscopy (HR-SEM), high-resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray (EDX) spectroscopy, powder X-ray diffraction (XRD), solid-state NMR analysis, circular dichroism (CD) analysis, and nitrogen sorption analysis (N2-BET).


Materials ◽  
2020 ◽  
Vol 13 (7) ◽  
pp. 1569
Author(s):  
Hao Li ◽  
Laurence Raehm ◽  
Clarence Charnay ◽  
Jean-Olivier Durand ◽  
Roser Pleixats

We report herein the preparation of mixed periodic mesoporous organosilica nanoparticles (E-Pn 75/25 and 90/10 PMO NPs) by sol-gel co-condensation of E-1,2-bis(triethoxysilyl)ethylene ((E)-BTSE or E) with previously synthesized disilylated tert-butyl 3,5-dialkoxybenzoates bearing either sulfide (precursor P1) or carbamate (precursor P2) functionalities in the linker. The syntheses were performed with cetyltrimethylammonium bromide (CTAB) as template in the presence of sodium hydroxide in water at 80 °C. The nanomaterials have been characterized by Transmission Electron Microscopy (TEM), nitrogen-sorption measurements (BET), Dynamic Light Scattering (DLS), zeta-potential, Thermogravimetric Analysis (TGA), FTIR, 13C CP MAS NMR and small angle X-ray diffraction (p-XRD). All the nanomaterials were obtained as mesoporous rodlike-shape nanoparticles. Remarkably, E-Pn 90/10 PMO NPs presented high specific surface areas ranging from 700 to 970 m2g−1, comparable or even higher than pure E PMO nanorods. Moreover, XRD analyses showed an organized porosity for E-P1 90/10 PMO NPs typical for a hexagonal 2D symmetry. The other materials showed a worm-like mesoporosity.


2021 ◽  
Vol 19 (1) ◽  
Author(s):  
Pardis Rahimi Salekdeh ◽  
Leila Ma’mani ◽  
Javad Tavakkoly-Bazzaz ◽  
Hossein Mousavi ◽  
Mohammad Hossein Modarressi ◽  
...  

Abstract Background There is a great interest in the efficient intracellular delivery of Cas9-sgRNA ribonucleoprotein complex (RNP) and its possible applications for in vivo CRISPR-based gene editing. In this study, a nanoporous mediated gene-editing approach has been successfully performed using a bi-functionalized aminoguanidine-PEGylated periodic mesoporous organosilica (PMO) nanoparticles (RNP@AGu@PEG1500-PMO) as a potent and biocompatible nanocarrier for RNP delivery. Results The bi-functionalized MSN-based nanomaterials have been fully characterized using electron microscopy (TEM and SEM), nitrogen adsorption measurements, thermogravimetric analysis (TGA), X-ray powder diffraction (XRD), Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR), and dynamic light scattering (DLS). The results confirm that AGu@PEG1500-PMO can be applied for gene-editing with an efficiency of about 40% as measured by GFP gene knockdown of HT1080-GFP cells with no notable change in the morphology of the cells. Conclusions Due to the high stability and biocompatibility, simple synthesis, and cost-effectiveness, the developed bi-functionalized PMO-based nano-network introduces a tailored nanocarrier that has remarkable potential as a promising trajectory for biomedical and RNP delivery applications.


2013 ◽  
Vol 11 (10) ◽  
pp. 1689-1698 ◽  
Author(s):  
Carmen Racles ◽  
Alexandra Nistor ◽  
Maria Cazacu

AbstractSilver nanoparticles (AgNPs) were obtained by a redox reaction, using a glucose-containing cyclosiloxane as a reduction agent and stabilizer. Then the AgNPs aqueous solution was used as the reaction medium for the sol-gel process, starting from tetraethylorthosilicate (TEOS) as silica precursor. The nanocomposite material resulted (SilAg) after solvent removal, aging and calcination and was investigated by infrared spectroscopy (FT-IR), atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-ray system (SEM/EDX), transmission electron microscopy (TEM), energy-dispersive X-ray fluorescence spectroscopy (EDXRF), X-ray diffraction (XRD) and dynamic vapor sorption (DVS). The results were compared to model silicas obtained without silver. A higher condensation degree in SilAg was obtained due to the basic medium used in the first step and was confirmed by a sorption capacity lower than for the model silicas. The solid surface area calculated with GAB analysis using DVS data for the water vapors is 210 m2 g−1. The nanocomposite showed good catalytic activity for hydrogen peroxide decomposition.


Author(s):  
Robert A. Grant ◽  
Laura L. Degn ◽  
Wah Chiu ◽  
John Robinson

Proteolytic digestion of the immunoglobulin IgG with papain cleaves the molecule into an antigen binding fragment, Fab, and a compliment binding fragment, Fc. Structures of intact immunoglobulin, Fab and Fc from various sources have been solved by X-ray crystallography. Rabbit Fc can be crystallized as thin platelets suitable for high resolution electron microscopy. The structure of rabbit Fc can be expected to be similar to the known structure of human Fc, making it an ideal specimen for comparing the X-ray and electron crystallographic techniques and for the application of the molecular replacement technique to electron crystallography. Thin protein crystals embedded in ice diffract to high resolution. A low resolution image of a frozen, hydrated crystal can be expected to have a better contrast than a glucose embedded crystal due to the larger density difference between protein and ice compared to protein and glucose. For these reasons we are using an ice embedding technique to prepare the rabbit Fc crystals for molecular structure analysis by electron microscopy.


Author(s):  
G. Van Tendeloo ◽  
J. Van Landuyt ◽  
S. Amelinckx

Polytypism has been studied for a number of years and a wide variety of stacking sequences has been detected and analysed. SiC is the prototype material in this respect; see e.g. Electron microscopy under high resolution conditions when combined with x-ray measurements is a very powerful technique to elucidate the correct stacking sequence or to study polytype transformations and deviations from the ideal stacking sequence.


Author(s):  
R. Gronsky

The phenomenon of clustering in Al-Ag alloys has been extensively studied since the early work of Guinierl, wherein the pre-precipitation state was characterized as an assembly of spherical, ordered, silver-rich G.P. zones. Subsequent x-ray and TEM investigations yielded results in general agreement with this model. However, serious discrepancies were later revealed by the detailed x-ray diffraction - based computer simulations of Gragg and Cohen, i.e., the silver-rich clusters were instead octahedral in shape and fully disordered, atleast below 170°C. The object of the present investigation is to examine directly the structural characteristics of G.P. zones in Al-Ag by high resolution transmission electron microscopy.


Author(s):  
Yun Lu ◽  
David C. Joy

High resolution scanning electron microscopy (SEM) and energy dispersive x-ray analysis (EDXA) were performed to investigate microparticles in blended cements and their hydration products containing sodium-rich chemical wastes. The physical appearance of powder particles and the morphological development at different hydration stages were characterized by using high resolution SEM Hitachi S-900 and by SEM S-800 with a EDX spectrometer. Microparticles were dispersed on the sample holder and glued by 1% palomino solution. Hydrated bulk samples were dehydrated by acetone and mounted on the holder by silver paste. Both fracture surfaces and flat cutting sections of hydrating samples were prepared and examined. Some specimens were coated with an 3 nm thick Au-Pd or Cr layer to provide good conducting surfaces. For high resolution SEM S-900 observations the accelerating voltage of electrons was 1-2 KeV to protect the electron charging. Microchemical analyses were carried out by S800/EDS equipped with a LINK detector of take-off angle =40°.


Author(s):  
W. Coene ◽  
F. Hakkens ◽  
T.H. Jacobs ◽  
K.H.J. Buschow

Intermetallic compounds of the type RE2Fe17Cx (RE= rare earth element) are promising candidates for permanent magnets. In case of Y2Fe17Cx, the Curie temperature increases from 325 K for x =0 to 550 K for x = 1.6 . X ray and electron diffraction reveal a carbon - induced structural transformation in Y2Fe17Cx from the hexagonal Th2Ni17 - type (x < 0.6 ) to the rhombohedral Th2Zn17 - type ( x ≥ 0.6). Planar crystal defects introduce local sheets of different magnetic anisotropy as compared with the ordered structure, and therefore may have an important impact on the coercivivity mechanism .High resolution electron microscopy ( HREM ) on a Philips CM30 / Super Twin has been used to characterize planar crystal defects in rhombohedral Y2Fe17Cx ( x ≥ 0.6 ). The basal plane stacking sequences are imaged in the [100] - orientation, showing an ABC or ACB sequence of Y - atoms and Fe2 - dumbbells, for both coaxial twin variants, respectively . Compounds resulting from a 3 - week annealing treatment at high temperature ( Ta = 1000 - 1100°C ) contain a high density of planar defects.


1999 ◽  
Vol 82 (08) ◽  
pp. 271-276 ◽  
Author(s):  
Glen Spraggon ◽  
Stephen Everse ◽  
Russell Doolittle

IntroductionAfter a long period of anticipation,1 the last two years have witnessed the first high-resolution x-ray structures of fragments from fibrinogen and fibrin.2-7 The results confirmed many aspects of fibrinogen structure and function that had previously been inferred from electron microscopy and biochemistry and revealed some unexpected features. Several matters have remained stubbornly unsettled, however, and much more work remains to be done. Here, we review several of the most significant findings that have accompanied the new x-ray structures and discuss some of the problems of the fibrinogen-fibrin conversion that remain unresolved. * Abbreviations: GPR—Gly-Pro-Arg-derivatives; GPRPam—Gly-Pro-Arg-Pro-amide; GHRPam—Gly-His-Arg-Pro-amide


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