System and process for chemical vapor deposition

Patent metadata

Field	Value
Publication number	US-10337101-B2
Application number	US-201615376867-A
Country	US
Kind code	B2
Filing date	Dec 13, 2016
Priority date	Dec 13, 2016
Publication date	Jul 2, 2019
Grant date	Jul 2, 2019

Abstract

A chemical vapor deposition method comprises flowing a carrier liquid through a reactor. A fluid comprising one or more reactants is introduced into the carrier liquid. The fluid is at a first temperature and first pressure and is sufficiently immiscible in the carrier liquid so as to form a plurality of microreactors suspended in the carrier liquid. Each of the microreactors comprise a discrete volume of the fluid and have a surface boundary defined by an interface of the fluid with the carrier liquid. The fluid is heated and optionally pressurized to a second temperature and second pressure at which a chemical vapor deposition reaction occurs within the microreactors to form a plurality of chemical vapor deposition products. The plurality of chemical vapor deposition products are separated from the carrier liquid. A system for carrying out the method of the present disclosure is also taught.

First claim

What is claimed is:

1. A method comprising:
flowing a carrier liquid through a reactor;
introducing a fluid comprising one or more reactants into the carrier liquid, the fluid being at a first temperature and first pressure and being sufficiently immiscible in the carrier liquid so as to form a plurality of microreactors suspended in the carrier liquid, each of the microreactors comprising a discrete volume of the fluid surrounded by the carrier liquid and having a surface boundary defined by an interface of the fluid with the carrier liquid;
heating and optionally pressurizing the fluid to a second temperature and second pressure at which a chemical vapor deposition reaction occurs within the microreactors to form a plurality of chemical vapor deposition products, the surface boundary acting as a substrate for the chemical vapor deposition reaction; and
separating the plurality of chemical vapor deposition products from the carrier liquid.

2. The method of claim 1 , wherein the fluid comprising one or more reactants is predominately a gas at the first temperature and first pressure.

3. The method of claim 1 , wherein the fluid comprising one or more reactants is predominately a liquid at the first temperature and first pressure and is predominately a gas at the second temperature and second pressure.

4. The method of claim 1 , wherein the deposition reaction comprises reacting the one or more reactants at the surface boundary of the microreactor to form a shell.

5. The method of claim 4 , further comprising maintaining a discrete volume of the fluid to be sufficiently constant during the deposition reaction so as to avoid fracturing of the microreactors.

6. A method comprising:
flowing a carrier liquid through a reactor;
introducing a fluid comprising one or more reactants into the carrier liquid, the fluid being at a first temperature and first pressure and being sufficiently immiscible in the carrier liquid so as to form a plurality of microreactors suspended in the carrier liquid, each of the microreactors comprising a discrete volume of the fluid and having a surface boundary defined by an interface of the fluid with the carrier liquid;
heating and optionally pressurizing the fluid to a second temperature and second pressure at which a chemical vapor deposition reaction occurs within the microreactors to form a plurality of chemical vapor deposition products; and
separating the plurality of chemical vapor deposition products from the carrier liquid,
wherein maintaining the discrete volume to be sufficiently constant comprises at least one of: 1) increasing a hydrostatic pressure at the surface boundary of the microreactors while heating the fluid and 2) decreasing the hydrostatic pressure while cooling the fluid.

7. The method of claim 4 , wherein the discrete volume of the fluid changes during the deposition reaction so as to fracture the microreactors.

8. The method of claim 1 , wherein the one or more reactants comprise a first reactant and a second reactant.

9. The method of claim 8 , wherein the first reactant reacts at the second temperature to form an outer layer of a shell and the second reactant reacts at a third temperature that is higher than the second temperature to deposit an inner layer on an inner surface of the outer layer.

10. The method of claim 1 , wherein a solid catalyst is provided at the surface boundary of the microreactor.

11. The method of claim 10 , wherein the solid catalyst is in the form of a nanoparticle.

12. A method comprising:
flowing a carrier liquid through a reactor;
introducing a fluid comprising one or more reactants into the carrier liquid, the fluid being at a first temperature and first pressure and being sufficiently immiscible in the carrier liquid so as to form a plurality of microreactors suspended in the carrier liquid, each of the microreactors comprising a discrete volume of the fluid and having a surface boundary defined by an interface of the fluid with the carrier liquid;
heating and optionally pressurizing the fluid to a second temperature and second pressure at which a chemical vapor deposition reaction occurs within the microreactors to form a plurality of chemical vapor deposition products; and
separating the plurality of chemical vapor deposition products from the carrier liquid,
wherein a solid catalyst is provided at the surface boundary of the microreactor and the chemical vapor deposition products are carbon nanotubes.

13. The method of claim 1 , wherein the carrier liquid comprises one or more compounds chosen from molten salts, alkanes and mixtures thereof.

14. The method of claim 1 , where the one or more reactants comprise a compound chosen from a hydrocarbon, silane, O 2 , WF 6 , AlCl 3 , Copper(II) bis(hexafluoroacetylacetonate), (CH 3 ) 3 Al, Fe(CO) 5 , [(CH 3 ) 2 N] 4 Hf, W(CO) 6 , C 5 H 4 CH 3 Pt(CH 3 ) 3 , and combinations thereof.

15. The method of claim 1 , further comprising cooling the plurality of chemical vapor deposition products to a third temperature that is sufficiently below the second temperature so that chemical vapor deposition terminates.

16. The method of claim 1 , further comprising allowing the microreactors to rise to a surface of the carrier liquid, thereby releasing waste fluid from the microreactors.

17. The method of claim 6 , wherein the carrier liquid comprises one or more compounds chosen from molten salts, alkanes and mixtures thereof.

18. The method of claim 6 , where the one or more reactants comprise a compound chosen from a hydrocarbon, silane, O 2 , WF 6 , AlCl 3 , Copper(II) bis(hexafluoroacetylacetonate), (CH 3 ) 3 Al, Fe(CO) 5 , [(CH 3 ) 2 N] 4 Hf, W(CO) 6 , C 5 H 4 CH 3 Pt(CH 3 ) 3 , and combinations thereof.

19. The method of claim 18 , wherein the deposition reaction comprises reacting the one or more reactants at the surface boundary of the microreactor to form a shell.

20. The method of claim 12 , wherein the carrier liquid comprises one or more compounds chosen from molten salts, alkanes and mixtures thereof.

Assignees

• Boeing Co

Inventors

• Humfeld Keith Daniel
• Cherry De'Andre James

Classifications

• C23C16/01 Primary

  on temporary substrates, e.g. substrates subsequently removed by etching · CPC title

• C23C16/4557

  Heated nozzles · CPC title

• C23C16/4418

  Methods for making free-standing articles (C23C16/01 takes precedence) · CPC title

• C23C16/26

  Deposition of carbon only · CPC title

• C23C16/402

  Silicon dioxide · CPC title