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Synthesis of Nanostructured Spherical Aluminum OxidePowders by Plasma Engineering

Synthesis of Nanostructured Spherical Aluminum OxidePowders by Plasma Engineering

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Synthesis of Nanostructured Spherical Aluminum OxidePowders by Plasma Engineering
Synthesis of Nanostructured Spherical Aluminum OxidePowders by Plasma Engineering

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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
6
to 10
8
K/s, wereobtained from the different quenching medias,
viz
. 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.
I.INTRODUCTION
N
ANOSTRUCTURED
materials exhibit superior prop-erties such as excellent strength, toughness, and hardness,as obvious from the presence of refined grains.
[1]
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.
[2–6]
The first chal-lenge is that the low mass and poor flow characteristicsrestrict the smooth flow of individual nanoparticles inthespray nozzle during thermal spraying.
[2]
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,
etc
.
[2–6]
In this study, we are trying to modify thefeedstock powder by two ways simultaneously,
viz
. 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,
[7,8,9]
but the nov-elty of this article lies in the idea of using different quench-ing media (
viz
. air, water, and liquid nitrogen) to achievenanostructured grains in individual spherical powder parti-cles through the plasma spraying process. Al
2
O
3
(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.
[10]
This powder is also being used potentially inthermal insulation as well as in inertial confinement fusionof nuclear materials.
[11]
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.
[12,13]
Because of the short resi-dence time of the particle in the plasma, impurity limits inthe product are generally low.
[7]
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.
II.EXPERIMENTAL PROCEDURE
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 2005301
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: agarwala@fiu.edu 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.
 
302VOLUME 36A, FEBRUARY 2005METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 1—Low-magnification SEM micrograph of as-received irregularlyshaped alumina powder.Fig. 2—Schematic of plasma spraying for powder spheroidizing.
range was procured from Saint Gobain Ceramics Materials(Figure 1). Plasma spheroidization experiments were carriedout under a variety of plasma conditions altering the primary,secondary, and carrier gas flow rate for different quenchingmedias, whereas the input current and voltage remained fixed.The alumina powders were plasma sprayed using a Praxairplasma SG 100 gun (Praxair, Danbury, CT) at 40 V and 800A,where the powders carried by argon gas were fed internallythrough a Praxair model 1264 powder feeder. Gas flow ratesof primary (Ar), secondary (He), and carrier gas (Ar) are inthe range of 15 to 35 Psi, 80 to 120 Psi, and 40 to 55 Psi,respectively. The optimized results are being presented in thisarticle. A schematic of the process is shown in Figure2. Theflight distance and diameter of the powder collector are denotedas
h
and
, respectively, in the schematic.Alumina powders were internally fed through the SG 100gun for providing a longer stay (dwell time) to maximizethe higher temperatures observed during the transit in theplasma flame. Hence, these ceramic powders experience ahigh degree of superheat in the plasma gun, which in turngives rise to the formation of resolidified morphology, asexplained in a later section.In order to compare the feasibility and degree of grain sizerefinement, three different cooling media,
air 
(room tem-perature),
water 
(room temperature), and
liquid nitrogen
(77 K) were used, thereby providing different degrees of cooling rates. The plasma-sprayed powders were collectedat the bottom of a vertical cylindrical steel container (29.2-cmheight and 16.4-cm diameter) with proper cooling arrange-ment. An extra open-ended steel cylinder (45.7-cm heightand
16.3-cm diameter) was placed on the powder-collect-ing container during air cooling in order to increase the flighttime of the molten ceramic particles,
i.e
., to avoid the splatformation of molten powders by impinging on the bottomsurface of the container. The collected powders, quenchedin water and liquid nitrogen, were dried by keeping thepowders in a box furnace at a temperature of 70 °C for2 hours. Henceforth, the quenched powders, synthesized bythe plasma spraying process, will also be called
 plasma-engineered powders
in this article. Scanning electronmicroscopy (SEM) characterization was carried out using ascanning electron microscope. As-received powders andplasma-engineered spherical powders have been investigatedby X-ray diffraction (XRD) for phase study and grain sizemeasurement using Mo
radiation (
0.70930 Å). Ramanspectra were obtained using a Ti-sapphire crystal target witha laser wavelength of 785 nm. The high-resolution trans-mission electron microscopy (HRTEM) images of the as-prepared particles were obtained with a PHILIPS* (Tecnai
*PHILIPS is a trademark of Philips Electronic Instruments Corp.,Mahwah, NJ.
Series) transmission electron microscope at 300 keV. Samplepreparation for TEM analysis was done by suspending pow-ders in acetone, where they were ultrasonicated for 10 min-utes, after which a copper grid was dipped in the solution. Thecopper grid was dried in air for 10 minutes and inserted in avacuum chamber for an hour before inserting the sample intheTEM chamber.
III.RESULTS AND DISCUSSION
A.
 Microstructural Evaluation of Plasma-Atomized Powders
The SEM micrograph shows an irregular morphology of as-received alumina powders (Figure 1) displaying powderparticles in the 15- to 45-
m size range. The overall mor-phologies of the powders after plasma spraying in air, water,and liquid nitrogen are shown in Figures 3 through 5, respec-tively. It is evident from the figures that most of the powdersbecame spherical after plasma spraying. A higher surfacearea to volume ratio leads to formation of spherical-shapedpowders facilitating faster heat energy dissipation. Hence,the tendency of spheroidization of the plasma-sprayed pow-ders was controlled by the high cooling rate of the thermalspraying process. The cooling rate during the solidificationof molten particles is calculated from the crystallite sizeshown later in this article. The plasma-engineered powdersin air, water, and liquid nitrogen are in the size ranges of 15 to 35
m, 10 to 35
m, and 10 to 25
m, respectively.
 
METALLURGICAL AND MATERIALS TRANSACTIONS AVOLUME 36A, FEBRUARY 2005303
Fig. 3—Low-magnification SEM micrograph of plasma-engineered spher-ical alumina powders, quenched in air.Fig. 4—Low-magnification SEM micrograph of spherical alumina pow-ders, plasma engineered in water.Fig. 5—Low-magnification SEM micrograph of spherical alumina pow-ders, plasma engineered in liquid nitrogen.
The presence of smaller spherical powder particles (2 to 5
m)can also be observed in all three cases. This is attributed tothe fragmentation of the molten particles moving at highspeed (
Mach 2) that became smaller sized spherical pow-ders after solidification. It can be noticed that some of thepowder particles became elliptical or oval shaped in all threecases of different cooling rates. This is because of the uneventhermal treatment of the powder particles during the inter-action with the plasma. The uneven thermal treatment resultsdue to the incongruity of plasma zone temperature and thedisparity in the interaction time of powders with the plasma.The different sized as-received powders also contributed tothe formation of oval-shaped powders, where the completemelting of the larger sized powders has not occurred.Incongruent flame flow causes partial melting of surfaces,which thereby leads to asymmetrical melting of edges andhence to the conical morphology of sprayed powder. The highspeed of the particle in the plasma flame smoothens the edgesand trims it to the shape of a comet undergoing more melt-ing at the front surfaces due to friction from air resistance. Itmay obviously be expected that larger particles melt in an
Fig. 6—Appearance of alien face attributed to different powder particle sizeand differential melting of sprayed particles, quenched in liquid nitrogen.
asymmetric way at the surfaces, whereas the smaller particlescan undergo complete melting and then get redeposited.A typical image is captured in Figure 6 as
an alien face
,where the small (
2 to 4
m) spray particles quenched inliquid nitrogen are resolidified and stuck to a partially meltedlarger particle (30 to 40
m). It might happen that larger,partially melted particles form a conical morphology aftertheir surface experiences differential flame flow in the streamand thereby generate
 face
of the alien. Fragmentation of larger particles by the gas stream impact or resolidificationof smaller melted particles spreading onto already solidifiedparticle form
eyes
, completing the formation of an alien face.The high-magnification SEM micrographs of plasma-sprayed powders are shown in Figures 7 through 10. Cellu-lar morphology is visible in the air-quenched plasma-sprayedpowders (Figure 7), whereas a flat and smooth resolidifiedstructure with some cellularity is obtained in the water-quenched sprayed powders (Figure 8). Even larger particles(compared to water- and air-quenched particles) in liquidnitrogen–quenched alumina powders resulted in the dendritic

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