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1.
Langmuir ; 24(14): 7532-7, 2008 Jul 15.
Artículo en Inglés | MEDLINE | ID: mdl-18540641

RESUMEN

The current investigation is centered on the thermal decomposition (700 degrees C) of acetyl acetonates of Ni, Co, and Fe in a closed reactor that was conducted by employing an external magnetic field (MF) of 10T. Interestingly, reactions of Co and Ni acetyl acetonates under a 10T MF produce Co and Ni nanoparticles (NPs) coated with carbon, while Fe acetyl acetonate produces Fe3O4 uncoated with carbon. Additionally, it is observed that all the as-formed magnetic particles tend to align in one dimension along applied MF; thus, this process can be used to fabricate large arrays of magnetic nanoparticles. The effect of an applied MF to synthesize morphologically and compositionally different products from corresponding precursors with their mesoscopic organization is the key theme of the present paper, explained with a plausible mechanism.

2.
Inorg Chem ; 46(12): 4951-9, 2007 Jun 11.
Artículo en Inglés | MEDLINE | ID: mdl-17487966

RESUMEN

The current investigation is centered on the thermal decomposition of iron(II) acetyl acetonate, Fe(C5H7O2)2, in a closed cell at 700 degrees C, which is conducted under a magnetic field (MF) of 10 T. The product is compared with a similar reaction that was carried out without a MF. This article shows how the reaction without a MF produces spherical Fe3O4 particles coated with carbon. The same reaction in the presence of a 10 T MF causes the rejection of the carbon from the surface of pyramid-shaped Fe3O4 particles, increases the Fe3O4 particle diameter, forms separate carbon particles, and leads to the formation of an anisotropic (long cigarlike) orientation of Fe3O4 pyramids and C sheets. The macroscopic orientation of Fe3O4 pyramids+C sheets is stable even after the removal of an external MF. The suggested process can be used to fabricate large arrays of uniform wires comprised of some magnetic nanoparticles, and to improve the magnetic properties of nanoscale magnetic materials. The probable mechanism is developed for the growth and assembly behavior of magnetic Fe3O4 pyramids+C sheets under an external MF. The effect of an applied MF to synthesize morphologically different, but structurally the same, products with mesoscopic organization is the key theme of the present paper.


Asunto(s)
Carbono/química , Compuestos Férricos/química , Magnetismo , Conformación Molecular , Nanopartículas/química
3.
J Phys Chem B ; 110(27): 13420-4, 2006 Jul 13.
Artículo en Inglés | MEDLINE | ID: mdl-16821865

RESUMEN

The thermal decomposition of commercial silicone grease was carried out in a closed reactor (Swagelok) that was heated at 800 degrees C for 3 h, yielding a SiO2-carbon composite with a BET surface area of 369 m2/g. The bulk conductivity (5.72 x 10(-6) S x cm(-2)) of the SiO2-carbon composite was determined by impedance measurements. The as-prepared SiO2-carbon composite was further annealed at 500 degrees C in air for 2 h, which led to the formation of white paramagnetic silica particles (confirmed by ESR), possessing a surface area of 111 m2/g. The present synthetic technique requires unsophisticated equipment and a low-cost commercial precursor, and the reaction is carried out without a solvent, surfactant, or catalyst. The mechanism for the formation of a porous SiO2-carbon composite from the silicone grease is also presented.

4.
J Phys Chem B ; 110(23): 11237-40, 2006 Jun 15.
Artículo en Inglés | MEDLINE | ID: mdl-16771390

RESUMEN

This article reports on the synthesis of high surface area (563m2/g) beta-SiC nanorods by thermal decomposition of commercial silicone oil at a relatively low reaction temperature (800 degrees C) in a closed Swagelok cell. High yield (75%) of SiC nanorods are obtained in this one-stage, solvent-, catalyst-, and template-free synthesis technique that runs at a relative low temperature and employs cheap single-precursor. The morphological (TEM, HR-SEM), compositional (CHNS, EDX, SAEDX]), structural (XRD, HR-TEM, and ED), thermal (TGA) characterizations and surface area analysis are carried out for the obtained SiC nanorods. The possibility of hydrogen storage in this high surface area nano-SiC rods are also tested and reported for the first time.


Asunto(s)
Compuestos Inorgánicos de Carbono/química , Nanotubos , Compuestos de Silicona/química , Aceites de Silicona/química , Microscopía Electrónica de Rastreo , Microscopía Electrónica de Transmisión , Difracción de Rayos X
5.
Inorg Chem ; 44(26): 9938-45, 2005 Dec 26.
Artículo en Inglés | MEDLINE | ID: mdl-16363865

RESUMEN

This article reports on the fabrication of WO(3) nanorods using an efficient straightforward synthetic technique, without a catalyst, and using a single precursor. The thermal dissociation of WO(OMe)(4) at 700 degrees C in a closed Swagelok cell under an air/inert atmosphere yielded W(18)O(49) nanorods. Annealing of W(18)O(49) at 500 degrees C under an air atmosphere led to the formation of pure WO(3) nanorods. The obtained products are characterized by morphological (scanning electron microscopy and transmission electron microscopy), structural (X-ray diffraction analysis, high-resolution scanning electron microscopy, and Raman spectroscopy), and compositional [energy-dispersive X-ray and elemental (C, H, N, S) analysis] measurements. The mechanism of the formation of nonstoichiometric W(18)O(49) nanorods is supported by the measured analytical data and several control experiments.

6.
Langmuir ; 21(8): 3635-40, 2005 Apr 12.
Artículo en Inglés | MEDLINE | ID: mdl-15807613

RESUMEN

The method of ultrasound irradiation is used for anchoring metallic nanocrystals (Ag, Au, Pd, and Pt) onto the surface of polystyrene spheres. In former studies, almost all the sonochemically prepared, coated metallic nanomaterials were formed as amorphous nanoparticles (Pol, V. G.; et al. Langmuir 2002, 18, 3352; Pol, V. G.; et al. Chem. Mater. 2003, 15, 1111; Zhong, Z. Y.; et al. Chem. Mater. 1999, 11 (9), 2350; Pol, V. G.; et al. Chem. Mater. 2003, 15, 1378), which were coated on various substrates (silica spheres, carbon spherules, titania, and alumina). On the other hand, the noble metal nanoparticles deposited on polystyrene spheres via ultrasound irradiation yielded nanocrystalline Ag, Au, Pd, and Pt particles on the surface of polystyrene as as-synthesized materials. The sonochemical mechanism is proposed based on chemical interactions between the particles.

7.
Ultrason Sonochem ; 12(3): 205-12, 2005 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-15491883

RESUMEN

Porous nickel and cobalt oxides were prepared using NiSO4.6H2O and anhydrous Co(CH3COO)2, a precursor other than alkoxides and cetyltrimethylammonium bromide as organic surfactant. The sonication method has been used for such synthesis. The surfactants were removed by calcination, as well as by solvent extraction and it is extent was examined by IR spectroscopy. The trend of removal of surfactant was followed by TGA studies and the change in phases by DSC. The products were identified by XRD. Peak in low angle XRD indicates the porous nature of the oxides. The morphology of the pores was studied by transmission electron microscopy. The pores were found less ordered, having an average size of 4-6 nm. The Brunauer-Emmet-Teller surface areas of the as-prepared, as well as the treated samples are reported having H2 and H4 type hysteresis for Ni and Co, respectively.

8.
J Phys Chem B ; 109(19): 9495-8, 2005 May 19.
Artículo en Inglés | MEDLINE | ID: mdl-16852141

RESUMEN

A very simple, efficient, and economical synthetic technique, which produces fascinating fullerene-like Ni-C (graphitic) core-shell nanostructures at a relatively low temperature, is reported. The thermal dissociation of Ni acetylacetonate is carried out in a closed vessel cell (Swagelok) that was heated at 700 degrees C for 3 h. The encapsulation of ferromagnetic Ni nanospheres into the onion structured graphitic layers is obtained in a one-stage, single precursor reaction, without a catalyst, that possesses interesting magnetic properties. The magnetoresistance (MR) property of Ni nanospheres encapsulated in a fullerene-like carbon was measured, which shows large negative MR, of the order of 10%. The proposed mechanism for the formation of the Ni-C core-shell system is based on the segregation and the surface flux formed in the Ni and carbon particles during the reaction under autogenic pressure at elevated temperature.


Asunto(s)
Carbono/química , Fulerenos/química , Níquel/química , Campos Electromagnéticos , Calor , Indicadores y Reactivos , Magnetismo , Microscopía Electrónica de Transmisión , Nanotubos , Presión , Espectrometría Raman , Difracción de Rayos X
9.
J Phys Chem B ; 108(20): 6322-7, 2004 May 20.
Artículo en Inglés | MEDLINE | ID: mdl-18950118

RESUMEN

In this article, we present results of the RAPET dissociation of MoO(OMe)4 at 700 degrees C in a closed Swagelok cell. The reaction produces molybdenum dioxide nanoparticles (20 nm) coated with carbon (20 nm). We have also carried out the same reaction under an applied magnetic field of 10 T. This reaction yielded different products. It produces a mixture of comparatively larger (50 nm) molybdenum dioxide nanoparticles and separated uncoated carbon particles (20-30 nm).

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