Method and apparatus for making uniform and ultrasmall nanoparticles

• US 9,216,398 B2
• Filed: 01/27/2014
• Issued: 12/22/2015
• Est. Priority Date: 04/19/2005
• Status: Active Grant

• Current Assignee: Umicore AG & Company KG (Umicore S.A.)
• Original Assignee: SDC Materials,Inc.
• Inventors: Layman, Frederick P., Biberger, Maximilian A.
• Primary Examiner(s): Mayekar, Kishor
• Application Number:
  US14/165,438
• Publication Number:
  US 20140209451A1
• Time in Patent Office: 694 Days
• Field of Search: None
• US Class Current: 1/1
• CPC Class Codes: A61L 2/18 Liquid substances or solutions comprising solids or dissolved gases
• CPC Class Codes: B01J 19/0013 Controlling the temperature of the process
• CPC Class Codes: B01J 19/088 giving rise to electric discharges for heating purposes H05B7/00; for the production of ozone C01B13/11, H01T19/00
• CPC Class Codes: B01J 2/16 by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
• CPC Class Codes: B01J 2219/0805 giving rise to electric discharges
• CPC Class Codes: B01J 2219/0879 Solid
• CPC Class Codes: B01J 2219/0894 Processes carried out in the presence of a plasma
• CPC Class Codes: B01J 25/00 Catalysts of the Raney type
• CPC Class Codes: B01J 25/02 Raney nickel
• CPC Class Codes: B01J 35/56 Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
• CPC Class Codes: B01J 37/0018 Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
• CPC Class Codes: B01J 37/0027 Powdering
• CPC Class Codes: B01J 37/06 Washing B01J37/0009, B01J37/0018 take precedence
• CPC Class Codes: B01J 37/349 making use of flames, plasmas or lasers
• CPC Class Codes: B22F 2202/13 Use of plasma
• CPC Class Codes: B22F 2203/13 pressure
• CPC Class Codes: B22F 2999/00 Aspects linked to processes or compositions used in powder metallurgy
• CPC Class Codes: B22F 9/12 starting from gaseous material
• CPC Class Codes: F28C 3/16 the particulate material forming a bed, e.g. fluidised, on vibratory sieves
• CPC Class Codes: F28D 15/00 Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies F28D17/00, F28D19/00, F28D20/00 take precedence
• CPC Class Codes: F28D 7/024 : the conduits of only one medium being helically coiled tubes, the coils having a cylindrical configuration
• CPC Class Codes: F28D 7/08 : the conduits being otherwise bent, e.g. in a serpentine or zig-zag F28D7/10 takes precedenceF28D7/0016 and F28D7/0033 take precedence
• CPC Class Codes: F28F 27/00 : Control arrangements or safety devices specially adapted for heat-exchange or heat-transfer apparatus control arrangements in general G05
• CPC Class Codes: Y10S 623/92 : Method or apparatus for preparing or treating prosthetic
• CPC Class Codes: Y10S 623/923 : Bone
• CPC Class Codes: Y10T 137/0391 : Affecting flow by the addition of material or energy
• CPC Class Codes: Y10T 137/2076 : Utilizing diverse fluids
• CPC Class Codes: Y10T 156/15 : Combined or convertible surface bonding means and/or assembly means

Abstract

A system comprising: a plasma production chamber configured to produce a plasma; a reaction chamber vaporize a precursor material with the plasma to form a reactive mixture; a quench chamber having a frusto-conical surface and a quench region formed within the quench chamber between an ejection port of the reaction chamber and a cooled mixture outlet, wherein the quench region configured to receive the reactive mixture from the ejection port, to cool the reactive mixture to form a cooled mixture, and to supply the cooled mixture to the cooled mixture outlet; and a conditioning fluid injection ring disposed at the ejection port and configured to flow a conditioning fluid directly into the reactive mixture as the reactive mixture flows through the ejection port, thereby disturbing the flow of the reactive mixture, creating turbulence within the quench region and cooling the reactive mixture to form a cooled mixture comprising condensed nanoparticles.

Claims

1. A method of producing nanoparticles, the method comprising:

vaporizing a precursor material with a plasma stream within a reaction chamber, thereby forming a reactive mixture stream comprising the vaporized precursor material entrained within the plasma stream;

flowing the reactive mixture stream through an ejection port of the reaction chamber and into a quench region of a quench chamber having a frusto-conical surface that narrows as it extends away from the ejection port of the reaction chamber, wherein the ejection port is located within a frusto-conical-shaped portion of the quench chamber;

flowing a conditioning fluid through an injection ring disposed at the ejection port of the reaction chamber into the reactive mixture stream as the reactive mixture stream flows through the ejection port of the reaction chamber, thereby disturbing the flow of the reactive mixture stream and creating turbulence within the quench region;

quenching the reactive mixture stream within the quench region to form a cooled mixture stream comprising condensed nanoparticles; and

flowing the cooled mixture stream through a cooled mixture outlet of the quench chamber.

2. The method of claim 1, further comprising supplying the conditioning fluid into the quench region in an annular formation along a path different from the flow of the conditioning fluid through the conditioning fluid injection ring via an annular supply portion formed between the reaction chamber and the frusto-conical surface of the quench chamber.

3. The method of claim 2, wherein the annular supply portion comprises a plurality of supply ports disposed in an annular formation around the reaction chamber.

4. The method of claim 2, wherein the annular supply portion comprises one continuous supply port disposed in an annular formation around the reaction chamber.

5. The method of claim 1, wherein the conditioning fluid injection ring flows the conditioning fluid into the reactive mixture stream at an angle substantially perpendicular to the flow of the reactive mixture stream.

6. The method of claim 1, wherein the conditioning fluid is a super-cooled gas.

7. The method of claim 1, wherein the conditioning fluid is liquid nitrogen.

8. The method of claim 1, wherein the conditioning fluid is liquid helium.

9. The method of claim 1, wherein the plasma stream is produced within a plasma production chamber by energizing a working gas.

10. The method of claim 9, further comprising flowing the precursor material into the plasma production chamber via a precursor supply port on the plasma production chamber prior to its vaporization.

11. The method of claim 1, further comprising flowing the precursor material into the reaction chamber via a precursor supply port on the reaction chamber prior to its vaporization.

12. The method of claim 1, further comprising maintaining the enthalpy of the reactive mixture stream for a period of time within an enthalpy maintenance region within the reaction chamber, wherein the reaction chamber comprises an insulating material.

13. The method of claim 12, wherein the reaction chamber comprises a ceramic material.

14. The method of claim 1, further comprising:

flowing the cooled mixture stream from the quench region to a collection device via a conduit having substantially the same diameter as the cooled mixture outlet; and

separating condensed nanoparticles from the cooled mixture stream using the collection device.

15. The method of claim 1, wherein the conditioning fluid is argon.

16. A method of producing nanoparticles comprising:

applying a plasma stream to a precursor material within a reaction chamber, thereby forming a reactive mixture stream comprising vaporized precursor material entrained within the plasma stream;

flowing the reactive mixture stream through an ejection port of the reaction chamber and into a frusto-conical-shaped quench chamber, wherein the ejection port is located within the frusto-conical-shaped quench chamber; and

flowing a conditioning fluid into the reactive mixture stream as the reactive mixture stream flows through the ejection port to disturb the flow of the reactive mixture stream and to cool the reactive mixture stream to form a cooled mixture stream comprising condensed nanoparticles.

17. The method of claim 16, wherein the conditioning fluid flows through an injection ring disposed at the ejection port into the reactive mixture stream at an angle substantially perpendicular to the flow of the reactive mixture stream out through the ejection port.

18. The method of claim 17, wherein the injection ring induces a high degree of turbulence within the conditioning fluid and the reactive mixture stream.

19. The method of claim 17, wherein the injection ring comprises one or more injection ports.

20. The method of claim 16, wherein the plasma stream is produced within a plasma production chamber.

21. The method of claim 20, further comprising supplying the precursor material into the plasma production chamber prior to its vaporization.

22. The method of claim 16, further comprising supplying the precursor material into the reaction chamber prior to its vaporization.