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1.
Ultramicroscopy ; 227: 113200, 2021 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-33581922

RESUMEN

Scanning Electron Microscopes (SEMs) often generate images with a shaded appearance which gives a natural 3D impression. Ergo, quite a few methods to reconstruct the 3D surface topography from these using shape-from-shading methods are available in the literature. Here, a novel approach is discussed which uses BackScatter Electron (BSE) images from multiple detectors to reconstruct the topography. Classically, algorithms exist which resort to a quad-BSE detector setup. However, other detector configurations are often found in SEMs. A set of images of these non-conforming detectors still contains enough information to allow for reconstruction, but requires a more general algorithm to do so. This article discusses a method based on a modal decomposition of the principal image components. The resulting method is shown to be efficient and independent of the number of detectors or their orientation. In fact, the orientation is identified as part of the algorithm and thus requires very little calibration.

2.
ACS Appl Bio Mater ; 3(12): 8808-8819, 2020 Dec 21.
Artículo en Inglés | MEDLINE | ID: mdl-35019556

RESUMEN

The fixation of hydrogels to biological tissues is a major challenge conditioning the development of implants and surgical techniques. Here, coatings of procoagulant nanoparticles are devised which use the presence of blood to create adhesion between hydrogels and soft internal organs. Those nanostructured coatings are simply adsorbed at the hydrogel surfaces and can rapidly activate the formation of an interfacial blood clot acting as an adhesive joint. This concept is demonstrated on pig liver capsules with model poly(ethylene-glycol) membranes that are intrinsically poorly adhesive. In the absence of blood, ex vivo peeling tests show that coatings with aggregates of bare silica nanoparticles induce a 2- to 4-fold increase in adhesion energy as compared to the uncoated membrane (3 ± 2 J m-2). This effect is found to scale with the specific surface area of the coating. The highest adhesion energies produced by these nanoparticle-coated membranes (10 ± 5 J m-2) approach the value obtained with cyanoacrylate glue (33 ± 11 J m-2) for which tearing of the tissue is observed. Ex vivo pull-off tests show an adhesion strength of coated membranes around 5 ± 1 kPa, which is significantly reduced when operating in vivo (1.0 ± 0.5 kPa). Nevertheless, when blood is introduced at the interface, the in vivo adhesion strength can be improved remarkably with silica coatings, reaching 4 ± 2 kPa after 40 min contact. In addition, these silica-coated membranes can seal and stop the bleeding produced by liver biopsies very rapidly (<30 s). Such a combination of coagulation and particle bridging opens promising routes for better biointegrated hydrogel implants and improved surgical adhesives, hemostats, and sealants.

3.
J Phys Chem Lett ; 10(15): 4192-4196, 2019 Aug 01.
Artículo en Inglés | MEDLINE | ID: mdl-31305079

RESUMEN

We report the successful one-pot synthesis of adenosine mono-, di-, and triphosphate in the confined space of a mordenite zeolite. This is also the first report of ATP synthesized onto a porous mineral surface. The results revealed a plausible prebiotic route to ribonucleotides and highlighted the contribution of microporous minerals in the origins of life.


Asunto(s)
Adenosina Difosfato/síntesis química , Adenosina Monofosfato/síntesis química , Adenosina Trifosfato/síntesis química , Silicatos de Aluminio/química , Nanopartículas/química , Técnicas de Síntesis en Fase Sólida/métodos , Zeolitas/química , Adenina/química , Organofosfatos/química , Origen de la Vida , Porosidad , Ribosa/química , Propiedades de Superficie , Termodinámica , Factores de Tiempo
4.
Langmuir ; 30(1): 297-307, 2014 Jan 14.
Artículo en Inglés | MEDLINE | ID: mdl-24359449

RESUMEN

An ordered microporous carbon material was prepared by the nanocasting process using the EMC-2 zeolite (EMT structure type) as a hard template. X-ray diffraction (XRD) and transmission electron microscopy (TEM) revealed long-range ordering in the material that resulted from the negative replication of the host template. The carbon porous network replicating the zeolite structure was modeled by overlapped spherical voids with diameters determined from the XRD pattern that displayed up to six distinct peaks. The surface delimiting the 3D interconnected porosity of the solid has a complex morphology. The pore size distribution calculated from the XRD-derived structural model is characterized by a maximum at 1.04 nm related to the long-range-ordered microporous network. Complementary studies by immersion calorimetry revealed that most of the porosity was characterized by a size above 1.5 nm. These porous features were compared to data resulting from classical analysis (DR, DFT, BET, etc.) of the N2 (77 K) and CO2 (low and high pressure, 273 K) physisorption isotherms. The limitations of these approaches are discussed in light of the pore size distribution consistently determined by XRD and immersion calorimetry measurements.

5.
Talanta ; 79(3): 877-86, 2009 Aug 15.
Artículo en Inglés | MEDLINE | ID: mdl-19576459

RESUMEN

Numerous mercaptopropyl-functionalized silica spheres have been prepared by either post-synthesis grafting of MCM-41 and MCM-48 or self-assembly co-condensation of mercaptopropyltrimethoxysilane (MPTMS) or mercaptopropyltriethoxysilane (MPTES) and tetraethoxysilane (TEOS) precursors in hydroalcoholic medium in the presence of a cationic surfactant as templating agent and ammonia as catalyst. These materials of approximately the same particle size and morphology featured different functionalization levels, various degrees of structural order, and variable distribution of thiol groups in the mesopores. Their reactivity in solution has been studied using Hg(II) as model analyte. Total accessibility (on a 1:1 S:Hg stoichiometry basis) was demonstrated and quantified for well-ordered materials whereas less open and less organized structures with high degrees of functionalization were subject to less-than-complete loadings. Capacities measured at pH 2 were lower than at pH 4 because of distinct mercury-binding mechanisms. Kinetics associated to the uptake process were studied by in situ electrochemical monitoring of Hg(II) consumption from aqueous suspensions containing the various adsorbents. They indicate only little difference between materials of the MCM-41 and MCM-48 series at similar functionalization levels, fast mass transport in well-ordered mesostructures in comparison to the poorly or non-ordered ones (except at pH 2 where charge formation induced some restriction in materials characterized by long-range structural order), and even faster processes in the wormlike frameworks (characterized by shorter range structural order). Hg(II) binding to thiol-functionalized materials obtained by post-synthesis grafting was found to occur more rapidly in the early beginning of the uptake process as a result of a higher concentration of binding sites at the pore entrance in comparison to the more homogeneous distribution of these groups in the mesochannels of materials obtained by co-condensation.

6.
Acta Crystallogr C ; 63(Pt 11): m537-40, 2007 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-17989476

RESUMEN

The title compound, {(C(2)H(10)N(2))(2)[Mn(PO(4))(2)]}(n), contains anionic square-twisted chains of formula [Mn(PO(4))(2)](4-) constructed from corner-sharing four-membered rings of alternating MnO(4) and PO(4) units. The Mn and P atoms have distorted tetrahedral coordination and the Mn atom lies on a twofold axis. The linear manganese-phosphate chains are held together by hydrogen-bonding interactions involving the framework O atoms and the H atoms of the ethane-1,2-diammonium cations, which lie in the interchain spaces.

7.
Chem Commun (Camb) ; (9): 991-3, 2006 Mar 07.
Artículo en Inglés | MEDLINE | ID: mdl-16491186

RESUMEN

The present study demonstrates that for the nanocasting process with zeolites, a careful choice of the zeolite structure type (EMT) allows the formation of faithful carbon replica exhibiting up to three well resolved XRD peaks.

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