using tributylphosphine, 10
13 nm Co nanoparticles weregenerated. Using hydrated nickel acetate as a metal precursor,nickel nanoparticles with particle sizes in the range 8
13 nmwere obtained. Co/Ni alloy nanoparticles were also producedusing a mixture of cobalt acetate and nickel acetate through asimilar synthetic procedure.
used ferromagneticresonance (FMR) techniques to investigate the detailed mag-netic characteristics of cobalt nanoparticles with differentcrystalline structures.
The structural characterization of anordered assembly of cobalt nanoparticles using high-resolutiontransmission electron microscopy was reported by Wang
They synthesized multiply twinned fcc cobalt nanocrystals fromthe thermal decomposition of dicobalt octacarbonyl in thepresence of a surfactant mixture composed of oleic acid andtributylphosphine. An HRTEM image of the nanoparticlesrevealed complicated interference patterns.
Reverse micelles, which are water-in-oil droplets stabilizedby a monolayer of surfactant, have been applied as nanoscalereactors for the synthesis of various nanoparticles.
and later the Pileni group reported on the synthesis of relativelyuniform cobalt nanoparticles by the reduction of cobalt saltinside reverse micelles.
synthesized cobaltnanoparticles with particle size in the range 1.8
4.4 nm byreducing CoCl
in reverse micelles formed usingdidodecyldimethylammonium bromide (DDAB). The Pilenigroup reported the synthesis of cobalt nanoparticles from thereaction between a micellar solution containing NaAOT(sodium bis(2-ethylhexyl)sulfosuccinate) and Co(AOT)
dissolved in NaAOT solution.
Collisions followed byexchange between micellar droplets induce chemical reaction of cobalt ions and sodium borohydride to generate cobalt nano-particles. The as-synthesized nanoparticles were poorly crystal-line while XRD, after heating at 500
C, revealed thecharacteristic pattern of fcc cobalt. The average particle sizemeasured using TEM data was 6 nm with a particle sizedistribution
= 9%. A size selection process involving theextraction of nanoparticles from reverse micelles significantlyreduced the polydispersity of the particle size distribution andthese uniform particles self-assembled to generate two-dimen-sionally hexagonally ordered arrays.
Relatively very little work has been done to synthesizeuniform iron nanoparticles. Suslick
reported the synthesisof iron nanoparticles from the sonochemical decomposition of iron pentacarbonyl in the presence of polyvinylpyrrolidone(PVP) or oleic acid.
The sonochemical decomposition of volatile organometallic compounds has been applied to synthe-size various nanostructured materials.
Transmission electronmicrographs showed that the iron particles ranged in size from3 to 8 nm. Electron diffraction revealed that the particles as-formed are amorphous, and that after
electron beamheating they crystallized to bcc iron. These iron nanoparticleswere readily oxidized to FeO when exposed to air. Gedankenand coworkers reported the synthesis of amorphous cobaltnanoparticles by sonicating Co(CO)
(NO) in decane solution inthe presence of oleic acid.
10 nm sized amor-phous nanoparticles were produced. One drawback of thesonochemical process in the synthesis of nanoparticles is itsinability to control particle size.Very recently, our research group synthesized monodisperseiron nanoparticles from the high temperature (300
C) aging of an iron
oleic acid metal complex, which was prepared by thethermal decomposition of iron pentacarbonyl in the presence of oleic acid at 100
We were able to synthesize monodispersenanoparticles with sizes ranging from 4 to 20 nm without usingany size selection process. Initially, the iron oleate complex wasprepared by reacting Fe(CO)
and oleic acid at 100
C. Ironnanoparticles were then generated by aging the iron complex at300
C. A TEM image of the iron nanoparticles revealed that thenanoparticles were monodisperse and the electron diffractionpattern showed that the nanoparticles were nearly amorphous.The XRD pattern of the sample after being heat-treated in anargon atmosphere at 500
C revealed a bcc
-iron structure. Theparticle size could be controlled from 4 to 11 nm by usingdifferent molar ratios of iron pentacarbonyl to oleic acid. Fig.3(a) and (b) show TEM images of iron nanoparticles withparticle sizes of 7 and 11 nm, respectively, which were preparedusing 1
2 and 1
3 molar ratios of Fe(CO)
oleic acid. In orderto produce nanoparticles larger than 11 nm, a reaction mixturewith a 1
4 molar ratio of Fe(CO)
and oleic acid was usedduring the synthesis. However, the particle size of the resultingnanoparticles was still around 11 nm. We could produce ironnanoparticles with particle sizes bigger than 11 nm by addingmore iron oleate complex to previously prepared 11 nm ironnanoparticles, and then aging at 300
C. Using this syntheticprocedure, we were able to tune the particle sizes of thenanoparticles from 11 to 20 nm.Using a similar synthetic procedure, we prepared moderatelymonodisperse cobalt nanoparticles and successfully appliedthem to recyclable catalysts for Pauson
Khand reactions, whichinvolve the cycloaddition of alkynes, alkenes and carbonmonoxide to synthesize cyclopentenones.
We also usedaqueous colloidal cobalt nanoparticles stabilized by sodiumdodecyl sulfate, which were synthesized by the reverse micellemethod described above, for use as recyclable aqueous-phasePauson
Nanoparticles of alloys of cobalt and iron
synthesized monodisperse iron
platinum nano-particles by the simultaneous reduction of platinum acet-ylacetonate (Pt(acac)
) and the thermal decomposition of ironpentacarbonyl (Fe(CO)
) in the presence of oleic acid and oleylamine.
The composition was adjusted by changing the molarratio of the two precursors. Using a 3
2 molar ratio of Fe(CO)
nanoparticles were produced, while using4
1 mixtures Fe
nanoparticles were formed. The particlesize could be varied from 3 to 10 nm by adding more precursorsto previously synthesized 3 nm particles, which acted as nuclei.When the solvent was evaporated slowly, three-dimensionalsuperlattices are generated, and by controlling the chain lengthsof the stabilizing surfactants, inter-particle spacing could betuned. For example, 6 nm Fe
nanoparticles were arranged
TEM images of iron nanoparticles: (a) three-dimensional array of 7nm Fe nanoparticles and (b) 11 nm Fe nanoparticles.
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