Synthesis of Nanostructured Spherical Aluminum OxidePowders by Plasma Engineering
T. LAHA, K. BALANI, A. AGARWAL, S. PATIL, andS. SEALIrregularly shaped aluminum oxide particles were plasma atomized resulting in narrow size range dis-tribution of spherical nanostructured powders. Cooling rates, on the order of 10
K/s, wereobtained from the different quenching medias,
. air, water, and liquid nitrogen. Plasma-engineeredpowder particles developed nanosize crystallites, while solidification provided insight into the mor-phological feasibility in refinement of grain size. X-ray diffraction (XRD) methods have been usedto quantify the crystallite size obtained with different quenching media. Raman peak shift validatedthe X-ray analysis in anticipating the grain refinement with increasing cooling rates. Salient struc-tural morphology characteristics and a detailed understanding of spheroidized plasma-sprayed alu-mina powders were analyzed through scanning electron microscopy (SEM) studies. Formation of nanograins, novel metastable phases, and amorphous structure were endorsed by transmission elec-tron microscopy (TEM) investigations.
materials exhibit superior prop-erties such as excellent strength, toughness, and hardness,as obvious from the presence of refined grains.
The nano-structured coatings/structures experience superior and novelproperties; thus, the importance of achieving such tremen-dous improvement in performance cannot be neglected byresearchers. Plasma spraying is one of the methods used toform nanocomposite structure, but it must overcome obstruct-ing and difficult processing challenges.
The first chal-lenge is that the low mass and poor flow characteristicsrestrict the smooth flow of individual nanoparticles inthespray nozzle during thermal spraying.
In addition, nano-sized powders tend to agglomerate and form clogs in theplasma gun nozzle, hindering the smoothness of the flowand thereby imparting nonuniform coating. The other chal-lenge is to retain the nanograins in the powder because grainscoarsen, experiencing the high temperatures in the plasmaflame. Several techniques are being developed to getnanocoating/composites by plasma such as employment of spray dried agglomerates of nanopowders, blending andspraying of bimodal powders with controlled plasma para-meters, explosion of loose nanoagglomerates in plasmaflame,
In this study, we are trying to modify thefeedstock powder by two ways simultaneously,
. spher-oidization and nanocrystallization/grain refinement of sprayparticles. It is anticipated that synthesis of nanostructuredceramic spheres by plasma spray technique would result indevelopment of an ideal free-flowing powder feedstock tosynthesize nanostructured coatings, and small complex partswith improved physical properties. Spheroidization byplasma spraying has been studied earlier,
but the nov-elty of this article lies in the idea of using different quench-ing media (
. air, water, and liquid nitrogen) to achievenanostructured grains in individual spherical powder parti-cles through the plasma spraying process. Al
(alumina)powder has been selected for the present study becausespherical nanostructured alumina powder is an excellentstarting material for near-net-shape forming, spray powdersfor coatings and soft abrasives, surface adsorbents in chem-ical industries, biocompatible coatings, and as carriers forcatalyst.
This powder is also being used potentially inthermal insulation as well as in inertial confinement fusionof nuclear materials.
Thermal plasma spraying has been used extensively withinmany industries for a variety of applications because of itsversatility to synthesize fine metal, alloy, ceramic, polymer,and composite powders. Plasma spheroidizing is a modifiedform of atomization technique, where the temperature reachesmore than 15,000 K in plasma flame with gas velocities reach-ing speeds of 1 to 3 Mach.
Because of the short resi-dence time of the particle in the plasma, impurity limits inthe product are generally low.
The added beauty of theprocess is the use of inert carrier gases minimizing the chem-ical reaction of the processed powder, which possesses highersurface energy than the starting powder, due to its refinedsize. Processing of ceramics such as alumina powdersbecomes much easier since the temperatures achieved inplasma are much higher than the melting point of any knownmaterial. The surface tension on the molten particles, upondisintegration, fragments it into spheroids of fine particlesadded with quenching from water, and liquid nitrogen helpsto nucleate and retain the nanocrystalline/grain structure of the particle. Plasma-spheroidized powder experiences rapidcooling, resulting in a high nucleation rate for solidified par-ticles, without any significant time for grain growth.
Commercially available aluminum oxide powder (99.8pctpurity) of irregular shape in the 15- to 45-
m particle size
METALLURGICAL AND MATERIALS TRANSACTIONS AVOLUME 36A, FEBRUARY 2005—301
T. LAHA and K. BALANI, Graduate Research Assistants, and A.AGARWAL, Assistant Professor, are with the Department of Mechanical& Materials Engineering, Florida International University, Miami, FL 33174.Contact e-mail: email@example.com S. PATIL, Graduate Research Assistant,and S. SEAL, Associate Professor, are with the Department of Mechanical,Materials and Aerospace Engineering, University of Central Florida, Orlando,FL 32186.Manuscript submitted March 29, 2004.