Vapor Deposition Process for the Manufacture of Coated Particles
a technology of vapor deposition and coating particles, which is applied in the direction of chemical vapor deposition coating, coating, liquid surface applicator, etc., can solve the problems of large-scale batch process significant inefficiencies, large process equipment and maintenance costs, and high production costs in batch process, so as to achieve enhanced throughput, reduce production costs, and reduce production costs
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example 1
[0101]80.0 g of 250 nm TiO2 particles is put into the powder reservoir of a reactor as shown in FIG. 3. The reactive precursor reservoir 33 is 1.5″ (3.8 cm) in diameter; the diameters of powder reservoir 32 and purge zone 36 each flares out to 3″ (7.6 cm). Prior to sealing the reactor, the ball valves are opened and all of the powder falls through to the bottom section. This demonstrates that the reactor dimensions are large enough to prohibit powder from necking during sealed operation. The volumes of powder reservoir 32 and purge zone 36 are each about twice that of reactive precursor reservoir 33.
[0102]The reactor is sealed and pumped down to a vacuum level of about 200 mTorr using a rotary vane vacuum pump. Heating tapes are used to heat the reactor and its contents to ˜77° C. Trimethylaluminum (TMA), preheated to 90° C., is introduced into reactive precursor reservoir 33 until the pressure is approximately 75 Torr. Ball valve 34 is opened and the pressures in powder reservoir 3...
example 2
[0107]Example 1 is repeated, this time using 50.0 g of high surface area TiO2 nanoparticles (79 m2 / g) as the starting powder. The precursors (TMA and H2O) are individually preheated to temperatures such that their respective vapor pressures equal approximately 30 Torr. The dosing times are 2 seconds for each precursor. At the onset of the dose time, the pressure immediately shoots up to approximately 25 Torr, and rise to 30-35 Torr over the dosing period. The amount of precursor administered to the system in each dose is slightly sub-stoichiometric. The sequential dosing and purging of the TMA and H2O are repeated for five cycles. The powder is removed and analyzed for Al2O3 using ICP-AES. The ALD growth rate is 0.5 Å / cycle, again indicated that the reactants are somewhat underdosed.
example 3
[0108]The reactor of FIG. 3 is modified to accommodate a three-zone dosing section for each precursor, whereby one-third of the reactive precursor is applied to the powder in each of the three zones. The three zones are arranged one above the other, and each are separated by a ball valve such a valve 34. This proceeded identically to that described in Example 2, except that both the TMA and the water are introduced to the powder over the three zones in three equivalently timed sub-dose regimes. This process is continued for 5 cycles, and the resulting growth rate is double the rate obtained in Example 2.
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