Growth of boehmite nanofibers by assembling nanoparticles with surfactant micelles

It is known that boehmite (AlOOH) nanofibers formed in the presence of nonionic poly(ethylene oxide) (PEO) surfactant at 373 K. A novel approach is proposed in this study for the growth of the boehmite nanofibers: when fresh aluminum hydrate precipitate was added at regular interval to initial mixture of boehmite and PEO surfactant at 373 K, the nanofibers grow from 40 to 50 nm long to over 100 nm. It is believed that the surfactant micelles play an important role in the nanofiber growth: directing the assembly of aluminum hydrate particles through hydrogen bonding with the hydroxyls on the surface of aluminum hydrate particles. Meanwhile a gradual improvement in the crystallinity of the fibers during growth is observed and attributed to the Ostwald ripening process. This approach allows us to precisely control the size and morphology of boehmite nanofibers using soft chemical methods and could be useful for low temperature, aqueous syntheses of other oxide nanomaterials with tailorable structural specificity such as size, dimension and morphology.

Synthesis and characterization of boehmite nanofibers

Boehmite nanofibers of high quality were synthesized through a wet-gel conversion process without the use of a surfactant. The long nanofibers of boehmite with clear-cut edges were obtained by steaming the wet-gel precipitate at 170 ºC for 2 days under a pH 5. Hydrothermal treatment of the boehmite gels enabled self-assembly through directed crystal growth. Detailed characterization using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Infrared Emission Spectroscopy (IES) and Raman Spectroscopy is presented.

Mesoporous spinel MgAl2O4 prepared by in situ modification of boehmite sol particle surface: I Synthesis and characterization of the unsupported membranes

Mesoporous spinel membranes as ultrafiltration membranes were prepared through a novel sol-gel technique. By in situ modification of the sol particle surface during the sol-gel process, control of the material structure on a nanometer scale from the earliest stages of processing was realized. Nano-particles with a chocolate-nut-like morphology, i.e. spinel MgAl2O4 as a shell and gamma -Al2O3 as a core, were first revealed by HRTEM results. The formation of the spinel phase was confirmed by X-ray diffraction (XRD). N-2 adsorption-desorption results showed that the mesoporous membranes had a narrow pore size distribution. (C) 2001 Elsevier Science B.V. All rights reserved.

Synthesis and luminescence properties of water dispersible Eu3+-doped boehmite nanoparticles

Nanocrystallized boehmite gamma-AlOOH center dot nH(2)O had been synthesized by spray-drying (SD) of a solution of aluminium tri-sec-butoxide peptized by nitric acid. The sub-micronic spherical particles obtained had an average diameter of 500 nm and were built of 100 nm or less platelet-like sub-particles. The average crystallite size calculated from XRD was 1.6 nm following the b axis (i.e. one unit cell) and 3-4 nm perpendicular to b. As a result of the nanometric sizes of crystallites, there was a large surface free for water adsorption and it was found to be n = 1.18 +/- 0.24H(2)O per AlOOH. The SD spheres spontaneously dispersed in water at room temperature and formed stable-over months-suspensions with nanometre-size particles (25-85 nm). Luminescent europium-doped nanocrystallized boehmites AlOOH: Eu (Al0.98Eu0.02OOH center dot nH(2)O) were synthesized the same way by SD and demonstrated the same crystallization properties and morphologies as the undoped powders. It is inferred from the Eu3+ luminescence spectroscopy that partly hydrated europium species are immobilized on the boehmite nanocrystals where they are directly bonded to alpha(OH) groups of the AlOOH surface. The europium coordination is schematically written [Eu3+(OH)(alpha)(H2O)(7-alpha/2)]. The europium-doped boehmite from SD spontaneously dispersed in water: the luminescence spectroscopy proves that most of the Eu3+ ions were detached from the NPs during water dispersion. The AlOOH: Eu nanoparticles were modified by the amine acid asparagine (ASN). The modification aimed to render the NPs compatible for further bio-functionalization. After surface modification, the NPs easily dispersed in water; the luminescence spectra after dispersion prove that the Eu3+ ions were held at the boehmite surface.

Elaboration of boehmite nano-powders by spray-pyrolysis

Boehmite (gamma-AlOOH) synthesis have been investigated using a spray pyrolysis (SP) device starting from a stable sol of Al-tri-sec-butoxide peptized by nitric acid. Free spherical particles from 100 to 500 nm have been elaborated. Particles sub-structure is made of nano-crystalline boehmite with very small average crystallite size (one crystal cell along the b axis). The nano-crystalline boehmite synthesized by SP at low temperature (200 degrees C) is spontaneously dispersible in water without any surface treatment. Boehmite powder may be transformed to transition gamma-alumina by heat post-treatment. Powders of sub-micrometric and spherical gamma-alumina particles may also be synthesized by SP at 700 degrees C. (C) 2008 Elsevier B.V. All rights reserved.

Self-supported bacterial cellulose/boehmite organic-inorganic hybrid films

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Transparent bacterial cellulose-boehmite-epoxi-siloxane nanocomposites

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural changes induced by ultrasound during aging of the boehmite phase

Structural changes induced by ultrasound during the aging of the aluminum monohydroxide (boehmite) were studied by means of X-ray diffraction (XRD) and nitrogen adsorption. The BET surface area and the pore volume of the ultrasound stimulated hydroxide (HU) are about 40% less than those of the non-stimulated one (HS). The mean pore size practically does not change, while the mean crystallite size (L) is about 25% greater in the HU system. The increase of L alone is not enough to account for the surface area diminution, suggesting that the sonication also induces compaction by elimination of some porosity. The sonication of the precursor hydroxide does not seem to play an apparent role in the structural properties of the resulting calcinated γ-alumina. © 1997 Elsevier Science B.V.

Transparent bacterial cellulose-boehmite-epoxi-siloxane nanocomposites

Organic-inorganic composite membranes were prepared from membranes of the bio-polymer bacterial cellulose (BC) and organic-inorganic sal composed of nanoparticulate boehmite and epoxi modified siloxane. Bacterial cellulose membranes are obtained in a highly hydrated state (1% cellulose and 99% cellulose) from cultures of Gluconacetobacter xylinus and could be used in the never-dried or in the dried state. Depending on the use of dried or never-dried BC membranes two main kinds of composites were obtained. In the first one dried BC membranes coated with the hybrid sol have lead to transparent membranes displaying a hi-phase structure where the two components could be easily distinguished, with individual structures preserved. A decrease was observed for tensile strength (50.5 MPa) and Young's Modulus (2.8 GPa) when compared to pure BC membrane (112.5 MPa and 12.7 GPa). Elongation at break was observed to increase (2.5% against 1.5% observed for BC). When never-dried BC membranes were used transparent membranes were also obtained, however an improvement was observed for mechanical properties (tensile strength - 116 MPa and Young's Modulus - 13.7 GPa). A lower value was obtained for the elongation at break (1.3%). In the last case the interaction between the two-phases lead to changes in the cellulose crystallinity as shown by X rays diffraction results. Multifunctional transparent membranes displaying the cellulose structure in one side and the boehmite-siloxane structure at the opposite face could find special applications in opto-electronics or biomedical areas taking advantage of the different chemical nature of the two components. (C) 2012 Elsevier Ltd. All rights reserved.

Self-supported bacterial cellulose/boehmite organic-inorganic hybrid films

Self-supported organic-inorganic hybrid transparent films have been prepared from bacterial cellulose and boehmite. SEM results indicate that the BC membranes are covered by Boehmite and XRD patterns suggest structural changes on cellulose due to Boehmite addition. Thermal stability is accessed through TG curves and is dependent on Boehmite content. Transparency, as evaluated by UV-Vis absorption, increases with increasing content of boehmite suggesting application of these materials as transparent substrates for opto-electronic devices.

XPS study of the major minerals in bauxite: Gibbsite, bayerite and (pseudo-)boehmite

Synthetic corundum (Al2O3), gibbsite (Al(OH)(3)), bayerite (Al(OH)(3)), boehmite (AlO(OH)) and pseudoboehmite (AlO(OH)) have been studied by high resolution XPS. The chemical compositions based on the XPS survey scans were in good agreement with the expected composition. High resolution A12p scans showed no significant changes in binding energy, with all values between 73.9 and 74.4 eV. Only bayerite showed two transitions, associated with the presence of amorphous material in the sample. More information about the chemical and crystallographic environment was obtained from the 0 Is high resolution spectra. Here a clear distinction could be made between oxygen in the crystal structure, hydroxyl groups and adsorbed water. Oxygen in the crystal structure was characterised by a binding energy of about 530.6 eV in all minerals. Hydroxyl groups, present either in the crystal structure or on the surface, exhibited binding energies around 531.9 eV, while water on the surface showed binding energies around 533.0 eV. A distinction could be made between boehmite and pseudoboehmite based on the slightly lower ratio of oxygen to hydroxyl groups and water in pseudoboehmite. (c) 2005 Elsevier Inc. All rights reserved.