Chemical vapor deposition reactor with preheating, reaction, and cooling zones

• US 9,816,185 B2
• Filed: 05/08/2017
• Issued: 11/14/2017
• Est. Priority Date: 03/22/2016
• Status: Expired due to Fees

• Current Assignee: King Fahd University Of Petroleum And Minerals
• Original Assignee: King Fahd University Of Petroleum And Minerals
• Inventors: Rabbani, Fahad Ali, Malaibari, Zuhair Omar, Atieh, Muataz Ali
• Primary Examiner(s): MCCRACKEN, DANIEL
• Application Number:
  US15/589,400
• Publication Number:
  US 20170275760A1
• Time in Patent Office: 190 Days
• Field of Search: 4234473
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: B82Y 40/00 Manufacture or treatment of nanostructures
• CPC Class Codes: C01B 2202/06 Multi-walled nanotubes
• CPC Class Codes: C01B 2202/10 Filled nanotubes
• CPC Class Codes: C01B 2202/32 Specific surface area
• CPC Class Codes: C01B 32/16 Preparation
• CPC Class Codes: C01B 32/162 characterised by catalysts
• CPC Class Codes: C01F 7/304 of organic aluminium compounds
• CPC Class Codes: C04B 41/4531 by C.V.D.
• CPC Class Codes: C23C 16/01 on temporary substrates, e.g. substrates subsequently removed by etching
• CPC Class Codes: C23C 16/30 Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
• CPC Class Codes: C23C 16/4417 Methods specially adapted for coating powder
• CPC Class Codes: C23C 16/4486 by producing an aerosol and subsequent evaporation of the droplets or particles
• CPC Class Codes: C23C 16/46 characterised by the method used for heating the substrate C23C16/48, C23C16/50 take precedence
• CPC Class Codes: C23C 16/463 Cooling of the substrate
• CPC Class Codes: Y10S 977/744 having atoms interior to the carbon cage
• CPC Class Codes: Y10S 977/752 Multi-walled
• CPC Class Codes: Y10S 977/843 Gas phase catalytic growth, i.e. chemical vapor deposition
• CPC Class Codes: Y10S 977/846 internal modifications, e.g. filling, endohedral modifications

Abstract

A vertical chemical vapor deposition (CVD) reactor and a method for synthesizing metal oxide impregnated carbon nanotubes. The CVD reactor includes a preheating zone portion and a reaction zone portion, and preferably an additional cooling zone portion and a product collector. The method includes (a) subjecting a liquid reactant solution comprising an organic solvent, a metallocene, and a metal alkoxide to atomization in the presence of a gas flow comprising a carrier gas and a support gas to form an atomized mixture, and (b) heating the atomized mixture to a temperature of 200° C.-1400° C., wherein the heating forms a metal oxide and at least one carbon source compound, wherein the metallocene catalyzes the formation of carbon nanotubes from the at least one carbon source compound and the metal oxide is incorporated into or on a surface of the carbon nanotubes to form the metal oxide impregnated carbon nanotubes.

Claims

1. A vertical chemical vapor deposition reactor, comprising:

a preheating zone portion;

a preheating element interposed between a top and bottom of the preheating zone portion that defines the preheating zone portion, wherein the preheating element is configured to heat the preheating zone portion to a preheating temperature;

a first inlet located at the top of the preheating zone portion and an ultrasonic atomizing nozzle operatively connected to the first inlet configured to release carrier, support, and/or reactant gases and at least one liquid reactant solution into the preheating zone portion;

a reaction zone portion located below the preheating zone portion;

a heater interposed between a top and a bottom of the reaction zone portion that defines the reaction zone portion, wherein the heater is configured to heat the carrier, support, and/or reactant gases and the at least one liquid reactant solution to a reaction temperature that is higher than the preheating temperature;

a cooling zone portion located below the reaction zone portion; and

a product collector located below the cooling zone portion configured to collect a solid chemical vapor deposition reaction product;

wherein the preheating zone portion, the reaction zone portion, the cooling zone portion, and the product collector are fluidly connected.

2. The vertical chemical vapor deposition reactor of claim 1, wherein the product collector is removably attached to a bottom of the cooling zone portion.

3. The vertical chemical vapor deposition reactor of claim 1, wherein the preheating zone portion, the reaction zone portion, and the cooling zone portion are cylindrically shaped, and wherein a diameter of the reaction zone portion is larger than a diameter of the preheating zone portion.

4. The vertical chemical vapor deposition reactor of claim 1, wherein the preheating zone portion, the reaction zone portion, and the cooling zone portion are cylindrically shaped, and wherein a diameter of the reaction zone portion is larger than a diameter of the preheating zone portion and the cooling zone portion.

5. The vertical chemical vapor deposition reactor of claim 1, wherein the first inlet is operatively connected to a pump that is connected to a liquid reactant solution container or mixer.

6. The vertical chemical vapor deposition reactor of claim 1, further comprising an outlet located at a bottom of the cooling zone portion configured to remove at least one reaction waste product from the cooling zone portion.

7. The vertical chemical vapor deposition reactor of claim 6, further comprising a second inlet located at the top of the preheating zone portion configured to introduce an evacuation gas into the preheating zone portion to displace and remove the at least one reaction waste product.

8. The vertical chemical vapor deposition reactor of claim 1, wherein the preheating element is disposed outside of the preheating zone portion.

9. The vertical chemical vapor deposition reactor of claim 1, wherein the heater is disposed outside of the reaction zone portion.

10. The vertical chemical vapor deposition reactor of claim 1, further comprising insulation disposed outside and around the preheating zone portion, the reaction zone portion, and the cooling zone portion.

11. The vertical chemical vapor deposition reactor of claim 10, wherein the insulation is graphite foam or quartz wool.