IP Library Granted Patent US 9,051,186
Granted Patent B2
US 9,051,186 · App. 13/791,549 · Granted Jun 9, 2015

Silicon carbide synthesis from agricultural waste

Inventors: Syed B Qadri (Fairfax Station, VA); Ame W Fliflet (Alexandria, VA); M Ashraf Iman (Great Falls, VA); Bhakta B Rath (Oakton, VA); Edward P Gorzkowski, III (Odenton, MD)
Assignee: The United States of America, as represented by the Secretary of the Navy
C01B31/36B82Y40/00C01P2004/16C01P2004/64B82Y30/00
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Quick Facts
Patent No.
US 9,051,186
App. No.
13/791,549
Granted
Jun 9, 2015
Kind
B2
Abstract

This disclosure concerns a method of making silicon carbide involving adding one from the group of rice husk material, sorghum, peanuts, maple leaves, and/or corn husk material to a container, creating a vacuum or an inert atmosphere inside the container, applying conventional heating or microwave heating, heating rapidly, and reacting the material and forming silicon carbide (SiC).

Claims (30)

1. A method of making SiC comprising:

adding one selected from the group consisting of rice husk material, sorghum, nuts, nut shells, maple leaves, fruit pits, and corn husk material to a container;

wherein the container is a covered boron nitride crucible;

creating a vacuum or an inert atmosphere inside the container;

applying heat;

heating rapidly the one selected from the group consisting of rice husk material, sorghum, nuts, nut shells, maple leaves, fruit pits, and corn husk material;

wherein the step of heating is accomplished by using a millimeter-wave beam and wherein the frequency of the millimeter-wave beam is about 83 GHz, the total beam power is about 5 kW, and the power density is about 0.3 kW/cm 2 ; and

reacting the one selected from the group consisting of rice husk material, sorghum, nuts, nut shells, maple leaves, fruit pits, and corn husk material and forming silicon carbide;

wherein the silicon carbide is nanoparticles and nanorods of SiC in a pure form.

2. The method of claim 1 further comprising the step of:

heating the one selected from the group consisting of rice husk material, sorghum, nuts, nut shells, maple leaves, fruit pits, and corn husk material to a temperature of about 1400-1500° C.

3. The method of claim 2 further comprising the step of:

maintaining the temperature of about 1400-1500° C. for about 1 to about 10 minutes.

4. The method of claim 3 further comprising the step of:

cooling the container.

5. The method of claim 4 wherein the vacuum is a modest vacuum environment which prevents oxidation and silica formation.

6. A method of producing nanorods and nanoparticles of silicon carbide comprising:

milling rice husks into a fine rice husk powder;

mixing the fine rice husk powder with a Polyvinyl alcohol (PVA) binder in a ratio of 0.95 rice husk to 0.05 PVA by weight;

pressing fine rice husk powder into a pellet;

directing a millimeter-wave beam to the pellet and thereby increasing the localized temperature;

heating the pellet to a temperature of about 1900° C.;

maintaining the temperature of the pellet at about 1900° C.; and

cooling the pellet which thereby forms nanorods and nanoparticles of silicon carbide and other products.

7. The method of claim 6 wherein the steps of heating the pellet, maintaining the heat, and cooling the pellet involve a total time of about 10 minutes.

8. The method of claim 7 wherein the frequency of the millimeter-wave beam is 83 GHz, the total beam power is about 5 kW, and the power density is about 0.3 kW/cm 2 with the microwave radiation directed at the pellet.

9. The method of claim 8 further comprising the step of:

using electron microscopy on a JEOL JSM-7001FLV SEM to characterize the structure of the silicon carbide and using TEM to further analyze the nanostructure wherein samples were prepared by transferring a few drops of alcohol containing the nanorods and nanoparticles of silicon carbide to a carbon coated fine mesh Cu-grid and were imaged using Phillips CM 30 and JEOL 2200 FX transmission electron microscopes.

10. The method of claim 9 further comprising the step of utilizing a SPEX jar mill in a Polycarbonate jar with Polytetrafluoroethylene milling media.

11. The method of claim 10 wherein the pellets are about 0.5 inch pellets pressed using a Carver press and die set.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 13, 2013
From: QADRI, SYED B.; FLIFLET, ARNE W.; IMAM, M. ASHRAF; RATH, BHAKTA B.; GORZKOWSKI, EDWARD P.
To: NAVY, U.S.A. AS REPRESENTED BY THE SECRETARY OF THE
Reel/Frame 030007/0860 →
Continuity (2)
Provisional Application 61622588 · Apr 11, 2012
Related Publication 20130272947A1 · Oct 17, 2013