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Figure 1
the film was kept exposed for 1 hour for gel film to form via hydrolysis and
polymerization. The film was dried via heat treatment at a temperature of
300o C for 2 hours. The Crystallization, densification and microstructure of
the films were then examined.
by
ferrite
a
powder
solution
was
evaporation
and a 0.25 M
X,
and
ALS
(ammonium
lauryl
heated on a hot plate with continuous stirring until it reaches its boiling
temperature such time that all liquid have already evaporated. A brown fume
that evolves during the process was obtained at the bottom of the beaker.
The powder was than calcined at 500oC and 550oC. the crystalline size of the
powder was then computed using the Scherrer formula.
Figure 2. Flow chart of supernatant assisted autocombustion synthesis.
SUPER CRITICAL HYDROTHERMAL SYNTHESIS
The
equal
mole
amount
(0.003
mol)
of
Bi(NO3)35H2O
and
was dissolved in 250 ml deionized water and was heated until homogenized.
It was than transferred to a reactor vessel. A stainless steel 316 with 180 mL
volume bath type reactor was used and was heated using an electrical
heater.
The hydrothermal reaction was performed in the reactor vessel at 500 o
C for 2 hours. After then, the reactor vessel was reduced to stop the reaction
with cold water so that the product will be collected through washing the
reactor with deionized water and cetrifugate to remove the reagent that
didnt reacted. Then the BiFeO nanoparticles were dreid at 40 o C for 24
hours.
The identity of the synthesized nanoparticled was then X-rayed for
diffraction measurements. The size and the shape of the obtained
nanoparticled was then studied using transmission electron microscopy.
stirring for 15 min. To adjust its pH to or greater than 10, 13.2 M solution of
ammonia was slowly dropped into the homogenous solution with constant
stirring, and a brown-colored precipitate will be formed. To remove NO3- and
Cl- ions from the precipitate, it was filtered and repeatedly was washed with
distilled water. The suspension was then transferred into a 40 ml Teflon-lined
stainless steel autoclave and to fill the capacity of 70%, mineralizer solutions
was added. Potassium hydroxide (KOH), lithium hydroxide (LiOH) and sodium
hydroxide (NaOH) were utilized for the preparation of mineralizer solutions.
The hydrothermal was performed with a reaction temperature of 180o C with
varied concentratios of the mineralizer (0.02-0.15 M) for 16 hours with
autogeneous pressure. The final products of the autoclave were filtered out
and were washed with distilled water and absolute ethanol several times to
remove residual soluble salts and unreacted ions after the autoclave was
cooled down naturally to room temperature. The obtained powders were
dried at 80C for 5 hours before characterization.
The phase structure of the as-synthesized BiFeO3powders was
characterized by X-ray powder diffraction with monochromated CuK
radiation ( = 1.5406 ) at 40 Kv and 50 Ma. The transmission electron
microscope (TEM), high-resolution transmission electron microscope (HRTEM) and selected area electron diffraction (SAED) images of the final
products were then observed using a JEOL 200 CX TEM with acceleration
voltage of 300 Kv.
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Retrieved from http://www.hindawi.com/journals/jnm/2011/797639/
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