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Chemical vapor deposition and powder formation using thermal spray

a technology of chemical vapor deposition and thermal spray, which is applied in the field of powder formation and thin film deposition, can solve the problems of inability to meet the requirements of chemical production, so as to improve the ratio of a given compound, improve the effect of coating and reducing the amount of vapor

Inactive Publication Date: 2005-01-27
HUNT ANDREW T +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

"The present invention provides a method and apparatus for depositing coatings and nanophase materials using plasma torch and CCVD techniques. The method involves using a solution fluid near or above its critical pressure and temperature, which is then heated just prior to being released through a nozzle or restriction. This results in a very fine atomization of the solution, with the precursor molecules reacting or dissolving prior to the atomization process. The method can be used to deposit coatings from various metalorganics and inorganic precursors. The resulting powder size can be decreased by decreasing the concentration of the initial solution, decreasing the time in the hot gases, decreasing the size of the droplets formed, and increasing the vapor pressure of the reagent. The method also allows for the formation of high-speed gas-vapor streams, improving film quality and deposition efficiency. The noncombustible fluids can be used as the solvent for the precursors, and the deposition can be performed at reduced pressures or in a controlled atmosphere. The technical effects of the invention include improved deposition efficiency, reduced powder size, and improved film quality."

Problems solved by technology

Many of these fluids are not stable as liquids at STP, and must be combined in a pressure cylinder or at a low temperature.
Conversely, if in-line filters become clogged or precipitant is found remaining in the main container, an incompatibility under those conditions may have occurred.

Method used

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  • Chemical vapor deposition and powder formation using thermal spray
  • Chemical vapor deposition and powder formation using thermal spray
  • Chemical vapor deposition and powder formation using thermal spray

Examples

Experimental program
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Effect test

example i

[0106] To illustrate the coating deposition capability of the process of the present invention, simple oxide coatings were formed on a metal substrate. SiO2 was deposited onto water cooled aluminum foil from a solution of tetraethoxysilane [Si(OC2H5)4] dissolved in isopropanol to 2.1 wt % Si, additional isopropanol (3.2 ml) and propane (51 ml) were added for an overall silicon concentration of 0.06 M. The gas temperature for deposition was 1190° C. The needle used to nebulize the precursor, as seen in FIG. 3, was 304 stainless steel with OD=0.012 inches and ID=0.004 inches. The resistance over the electrical flow length of the needle was about 1.6 W. Small pilot flames formed from combusted ethane and oxygen were used throughout the deposition to maintain the flame. The solution was pumped to the needle at 3 ml / min and nebulized by controlling the amount of current through the needle. In this example, the current was 2.65 A. The solution pressure from pumping during a deposition can...

example ii

[0108] In addition to coatings formed on metal substrates, such as the oxide deposited on aluminum in Example I, coatings have also been formed on plastic substrates. Platinum was deposited onto Teflon at a gas temperature of 200 to 260° C. from a 0.005M solution of platinum-acetylacetonate [Pt(CH3COCHCOCH3).2], toluene and methanol. The deposition apparatus used was similar to that used for Example I, except two separate pilot lights were used and the oxygen was supplied via a coaxial tube surrounding the reagent solution. The solution flow rate was 2 ml / min with a pressure of 1500 psi and a needle current of approximately 3.3 A. The oxygen flowed at a pressure of 20 psi and a rate of 4750 ml / min. The resulting adherent film was smooth, dense and uniform. X-ray diffraction (“XRD”) confirmed the formation of platinum with a (111) preferred growth direction.

[0109] This example also illustrates that the coatings produced by the process of the present invention are not exclusively oxi...

example iii

[0110] The coatings developed by the present invention are not limited to formation on planar substrates. Films have been deposited on ceramic fiber tows using the apparatus of the present invention. LaPO4 was deposited onto an alumina fiber tow from a solution of triethylphosphate [C2H.5O3PO4] dissolved in toluene to 1.7 wt % P, lanthanum 2-ethylhexanoate dissolved in toluene to 1 wt % La, additional toluene (16 ml) and propane (273 ml). The resulting solution had concentrations of 0.0010 M P and 0.0013M La. The solution flowed at a rate of 3 ml / min with a pressure of 410 psi during the deposition and was nebulized with a needle current of 2.36 A. The flow rate of oxygen to the solution flame was 4750 ml / min at a pressure of 30 psi.

[0111] The 400 fibers in the tow were coated at the same time. Each fiber was approximately 12 mm in diameter. The tow was slowly moved through the deposition zone of the flame two times. Only two passes through the flame (where the tow was rotated 180 ...

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Abstract

A method for chemical vapor deposition using a very fine atomization or vaporization of a reagent containing liquid or liquid-like fluid near its supercritical temperature, where the resulting atomized or vaporized solution is entered into a flame or a plasma torch, and a powder is formed or a coating is deposited onto a substrate. The combustion flame can be stable from 10 torr to multiple atmospheres, and provides the energetic environment in which the reagent contained within the fluid can be reacted to form the desired powder or coating material on a substrate. The plasma torch likewise produces the required energy environment, but, unlike the flame, no oxidizer is needed so materials stable in only very low oxygen partial pressures can be formed. Using either the plasma torch or the combustion plasma, coatings can be deposited and powders formed in the open atmosphere without the necessity of a reaction chamber, but a chamber may be used for various reasons including process separation from the environment and pressure regulation.

Description

RELATED CASES [0001] This application is a continuation of U.S. patent application Ser. No. 09 / 921,437 filed Mar. 8, 2001, which is a divisional of U.S. patent application Ser. No. 09 / 293,867 filed Apr. 16, 1999, (now abandoned), which is a divisional of U.S. patent application Ser. No. 08 / 691,853, filed Aug. 2, 1996, now U.S. Pat. No. 5,997,956, which claims the benefit of U.S. Provisional Application Ser. No. 60 / 002,084, filed Aug. 4, 1995, the contents of all of which are hereby incorporated in their entirety by this reference.II. FIELD OF THE INVENTION [0002] This invention relates to methods of powder formation and thin film deposition from reagents contained in liquid or liquid-like fluid solutions, whereby the fluid solution, near its supercritical point temperature, is released into a region of lower pressure causing a superior, very fine atomization or vaporization of the solution. Gasses are entrained or fed into the dispersed solution and rapidly flow into a flame or plas...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B05D1/02B22F9/28H05H1/24C01B13/34C23C16/44C23C16/448C23C16/453
CPCB22F9/28C01B13/34C23C16/4486C23C16/453Y10T428/265B05D1/08B05D2401/90Y10T428/25Y10T428/256Y02T50/67Y02P20/54Y02T50/60
Inventor HUNT, ANDREW T.HORNIS, HELMUT G.
Owner HUNT ANDREW T
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