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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

Inactive Publication Date: 2015-09-17
PNEUMATICOAT TECH LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The invention provides a simplified apparatus for vapor deposition processes that can be performed in a semi-continuous manner. This apparatus allows for a higher throughput of coated particles, resulting in higher quality products that can be produced for similar or lower capital costs. The apparatus can be used in processes such as atomic layer deposition and chemical vapor deposition, and can be easily adapted to high production rates or different thicknesses of coatings. Overall, the invention improves production efficiency and allows for greater control over the coating process.

Problems solved by technology

Batch processes have significant inefficiencies when operated at large scale, for several reasons.
Equipment failures and maintenance add to this downtime.
Process equipment tends to be very large and expensive in batch processes.
The need to operate these processes under vacuum adds greatly to equipment costs, especially as equipment size increases.
Because of this, equipment costs for batch processes tend to increase faster than operating capacity.
Another problem that occurs as the process equipment becomes larger is that it becomes more difficult to maintain uniform reaction conditions throughout the vessel.
It is also difficult to adequately fluidize a large mass of particles, specifically nanoparticles.
Issues such as these can lead to inconsistencies and defects in the coated product.
This represents yet another problem for a batch operation.
The batch particle ALD process inherently incurs additional down-time due to more frequent periodic cleaning requirements, and the reaction vessels cannot be used for multiple film types when cross-contamination could be problematic.
With larger vessels, localized process conditions, including internal bed heating, pressure gradients, mechanical agitation to break up nanoparticle aggregates, and diffusion limitations amongst others, become more difficult to control.
There is a practical maximum reaction vessel size when performing ALD processes on fine and ultra-fine particles, which limits the annual throughput for a single batch reactor operating continually, where the time duration of the process producing a given amount of coated materials equals the up-time plus down-time.
There is a practical maximum allowable capital expense to fabricate a particle ALD production facility, which effectively limits the number of batch reactors that operate identical processes in parallel.
With these constraints, there are practical throughput limitations that prohibit the integration of some particle ALD processes at the industrial scale.
For a traditional batch CVD process, the primary methods of controlling reactions are limited to reactant exposure time and operating conditions such as process temperatures and pressures.
The batch particle CVD process inherently has limited opportunity to prevent unwanted gas-phase side reactions.

Method used

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  • Vapor Deposition Process for the Manufacture of Coated Particles
  • Vapor Deposition Process for the Manufacture of Coated Particles
  • Vapor Deposition Process for the Manufacture of Coated Particles

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

A process for conducting vapor phase deposition is disclosed. The process separates a series of reactions through a sequence of reaction reservoirs. In some particular embodiments, the reactor includes a reactive precursor reservoir beneath a powder reservoir separated by valve means. A reactive precursor is charged into the reactive precursor reservoir and a powder is charged into the powder reservoir. The pressures are adjusted so that the pressure in the reactive precursor reservoir is higher than that of the powder reservoir. The valve means is opened, and the vapor phase reactant fluidized the powder and coats its surface. The powder falls into the reactive precursor reservoir. The apparatus permits vapor phase deposition processes to be performed semi-continuously.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]This application is a divisional of U.S. patent application Ser. No. 13 / 069,452, filed Mar. 23, 2011, which claims priority benefit of U.S. Provisional Patent Application No. 61 / 316,410, filed 23 Mar. 2010, all of which are incorporated herein by reference in their entirety.BACKGROUND OF THE INVENTION[0002]The incorporation of particles from millimeter-scale down to nanometers in size is ubiquitous in end-use products produced in industrial-scale quantities. A significant percentage of the particles used across all industries require that the surfaces be coated with a shell, layer, film, or other coating, ranging from sub-nanometer to hundreds of micrometers in thickness. For a variety of reasons, each sector or industry has determined that the incorporation of coated particles into the end-use product provides enough value-add in the performance of the product that the cost associated with each coating process is justified. Vapor deposit...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C23C16/44C23C16/442C23C16/455
CPCC23C16/4417C23C16/442C23C16/45525C23C16/402C04B41/009C04B41/4584C04B41/5031C04B41/5035C04B41/5041C04B41/5049C04B41/81C04B41/87C23C16/403C23C16/405C23C16/407C23C16/45555
Inventor KING, DAVID M.WEIMER, ALAN W.LICHTY, PAUL
Owner PNEUMATICOAT TECH LLC