Title:
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Novel sol-gel synthesis and characterization of oxide nanopowders for solid oxide fuel cells
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In this research, three different sol-gel synthesis methods by using cost
effective materials, such as sugar + pectin, sodium alginate beads or sodium
alginate granules, have been investigated for nanopowders production in
Solid Oxide Fuel Cells (SOFCs) application. Materials (cerium gadolinium
oxide and nickel oxide) have been selected as model materials. Cerium
gadolinium oxide (CGO) is one of the most important electrolyte materials in
SOFC due to its high ionic conductivity at 500-800 "C, whilst nickel oxide
(NiO) can be reduced into nickel in SOFC fuels (H2 or CH4) as catalyst in
anode layer.
First of all, a novel sol-gel method has been developed for the production of
high purity nanopowders of Ce0.8Gd0.201.9 (CG02) solid solution using
maltose or sucrose as an organic chelating agent and pectin for gelation.
The results of this investigation indicate that the final particle size of
approximately 10 nm can be obtained after calcination of the dried gel at
, 500°C for 2 hours in ambient air. Powder X-ray diffraction (XRD) shows that
all samples are single phase cubic CGO powders. The mean crystallite sizes
calculated from XRD analysis using Rietveld refinement method agree with
the morphological features observed by transmission electron microscopy
(TEM). The nominal composition of CG02 has been found to be in excellent
agreement with that determined by energy dispersive X-ray spectroscopy
(EDS) and inductively coupled plasma - atomic emission spectrometry
analysis (ICP-AES). The ionic conductivities of Ceo.8Gdo.201.9 samples are
measured by AC-impedance which appears reasonably well with the
reference data which will qualify the use of this material for SOFC as solid
electrolyte and in the fabrication of composite electrodes.
On the other hand, another novel and generic sol-gel method has been
developed for the production of high purity metal oxide nanopowders using
sodium alginate (Na-ALG). This has been demonstrated successfully
employing NiO and CGO CG01 (Ce0.9Gd0.1O1.95) and CGO2 (Ce0.8Gd0.201.9)
as model materials in this instance. For NiO, the results of this investigation
indicate that the final particle size of -20 nm can be obtained after
calcination of the predried beads at 500°C for 3 hours in ambient air. XRD
shows that the obtained samples are single phase cubic NiO powders.
Furthermore, freeze dried and X-ray micro-tomography (XMT) technologies
are applied to observe the inside morphology of the Ni-ALG beads. XMT
shows that nickel ions have been uniformly cross-linked in the alginate
structure and remained stable after freeze drying evidenced by the bright
green color of the freeze dried beads. Finally, NiO nanopowders can also be
synthesized using Na-ALG granules.
Moreover, this alginate method has also been demonstrated successfully
employing CGO in two composites designated as CG01 (Ceo.9Gdo.101.95)
and CG02 (Ceo.aGdo.201.9), respectively. The results indicate that the
nanopowders having a final particle size of -7 nm can be obtained after
calcination of ion-exchanged alginate precursor at 500 degC for 2 hours in
ambient' air. The chemical structures of Na-ALG solution and CGO beads
are analyzed by Fourier transform infrared spectroscopy (FTIR) which
indicates that Ce3+/Gd3+ are ion-exchanged with Na+ after gelation. The
nominal compositions of CG01 and CG02 have been found to be in
excellent agreement with that determined by EDS and ICP-AES. The ionic
conductivities of these two samples are measured by AC-impedance which
appears reasonably well with the reference data which will also qualify the
use of this material for SOFC as solid electrolyte.
All of these new sol-gel methods are simple, environmentally friendly and
non-toxic routes for a large scale production of high purity single phase
nanopowders in a cost effective manner at significantly low temperatures.
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