IP Library Granted Patent US 7,524,481
Granted Patent B2
US 7,524,481 · App. 10/220,688 · Granted Apr 28, 2009

Reactors for producing inorganic fullerene-like tungsten disulfide hollow nanoparticles and nanotubes

Assignee: Yeda Research and Development Co., Ltd.
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Quick Facts
Patent No.
US 7,524,481
App. No.
10/220,688
Granted
Apr 28, 2009
Kind
B2
Abstract

The present invention is related to an apparatus for the production of inorganic fullerene-like (IF) nanoparticles and nanotubes. The apparatus comprises a chemical reactor, and is further associated with a feeding set up and with a temperature control means for controlling the temperature along the reaction path inside the reactor so as to maintain the temperature to be substantially constant. The invention is further directed to a method for the synthesis of IF-WO3 nanoparticles having spherical shape and having a size up to 0.5 mu m and nanotubes having a length of up to several hundred mu m and a cross-sectional dimension of up to 200 nanometer.

Claims (17)

1. A synthetic method of production of WS 2 fullerene-like nanoparticles and nanostructures from WO 3 metal oxide powder and H 2 and H 2 S reacting gases, said method comprising the steps of:

(i) feeding a first mixture of a reacting tungsten oxide powder and an inert gas with a predetermined feeding rate downwardly into the top of a vertical flow line extending into the inside of a vertical chemical reactor such that a lower end of the vertical flow line is located inside the vertical chemical reactor, and providing a flow of a mixture of the H 2 and H 2 S reacting gases along said vertical chemical reactor, so as to allow interaction of the flowing tungsten oxide powder and the reacting gases in a reaction path located in the vertical chemical reactor;

(ii) controlling temperature inside the chemical reactor so as to provide a predetermined temperature profile along the reaction path; and

(iii) collecting the formed WS 2 nanostructures at a bottom portion of the vertical reactor,

the method thereby providing a solid-gas reaction between the reacting gases and the tungsten oxide powder during the flow through and along the reaction path, resulting in the formation of WO 3-x , clusters coated by at least one layer of WS 2 , and further exchange of oxides by sulfides in inner parts of the clusters, thereby causing formation of WS 2 nanostructures.

2. The method according to claim 1 , wherein the feeding rate of the reacting tungsten oxide powder is selected in accordance with the dimensions of the chemical reactor, thereby obtaining the WS 2 nanostructures in the form of IF-nanoparticles, or a combination of IF-nanoparticles and nanotubes.

3. The method according to claim 2 , wherein the feeding rate ranges between about 3 mg/min to about 120 mg/min, the concentration of the H 2 gas being from about 0.2% (w/v) to about 7% (w/v) and the concentration of the H 2 S gas being from about 0.1% (w/v) to about 6% (w/v).

4. The method according to claim 3 , wherein the formed nanostructures contain a combination of nanoparticles and nanotubes.

5. The method according to claim 2 , wherein the feeding rate ranges between about 3 mg/min to about 40 mg/min, with the concentration of the H 2 and H 2 S gases ranging from about 0.2% to about 4% (w/v).

6. The method according to claim 5 , wherein the formed IF-WS 2 nanostructures contain nanoparticles, each having a substantially perfect spherical shape and having a size up to 0.5 μm.

7. The method according to claim 2 , wherein the feeding rate ranges between about 40 mg/min and about 120 mg/min, with the concentration of the H 2 and H 2 S gases from about 3% to about 7% (w/v).

8. The method according to claim 7 , wherein the formed WS 2 nanostructures contain a combination of IF-nanoparticles and nanotubes, the nanotubes each having a cross-sectional dimension of up to 200 nanometer.

9. The method according to claim 2 , wherein the feeding rate ranges between about 3 mg/min to about 40 mg/min, with the concentration of the H 2 gas from about 0.2% to about 4% and the concentration of the H 2 S gas from about 0.2% to about 4% (w/v)

10. The method according to claim 9 , wherein the formed WS 2 nanostructures contain a combination of nanoparticles and nanotubes, the nanotubes having a length of up to several hundred μm and a cross-sectional dimension of up to 200 nanometer.

11. The method according to claim 1 , wherein said temperature within the reaction path is maintained at a constant temperature within the range of about 750° C. to about 850° C.

12. The method according to claim 1 , wherein the flow of the mixture of the H 2 and H 2 S reacting gases in said feeding step (i) is in a downward direction into the top of the vertical chemical reactor.

13. The method according to claim 1 , wherein the flow of the mixture of the H 2 and H 2 S reacting gases in said feeding step (i) is in an upward direction from the bottom of the vertical chemical reactor, thereby creating a fluidized bed of said powder in said reacting gases.

Assignments (5)
CORRECTIVE ASSIGNMENT TO CORRECT THE NATURE OF THE CONVEYANCE, SHOULD BE A TERMINATION AND RELEASE PREVIOUSLY RECORDED ON REEL 054221 FRAME 854. ASSIGNOR(S) HEREBY CONFIRMS THE TERMINATION AND RELEASE. Recorded Nov 2, 2020
From: NANOTECH INDUSTRIAL SOLUTIONS, INC.
To: EVONIK VENTURE CAPITAL GMBH, AS AGENT
Reel/Frame 054276/0332 →
SECURITY INTEREST Recorded Oct 30, 2020
From: NANOTECH INDUSTRIAL SOLUTIONS, INC.
To: EVONIK VENTURE CAPITAL, GMBH, AS AGENT
Reel/Frame 054221/0854 →
SECURITY INTEREST Recorded Dec 15, 2016
From: NANOTECH INDUSTRIAL SOLUTIONS, INC.
To: EVONIK VENTURE CAPITAL GMBH, AS AGENT
Reel/Frame 040992/0046 →
CORRECTIVE ASSIGNMENT TO CORRECT THE COVER SHEET - ADDRESS OF RECEIVING PARTY AND EXECUTION DATES PREVIOUSLY RECORDED ON REEL 015006 FRAME 0152. ASSIGNOR(S) HEREBY CONFIRMS THE ADDRESS OF RECEIVING PARTY IS THE WEIZMANN INSTITUTE OF SCIENCE; AND ASSIGNMENT WAS EXECUTED IN MARCH OF 2004. Recorded Sep 16, 2004
From: TENNE, RESHEF; FELDMAN, YISHAY; ZAK, ALLA; ROSENTSVEIG, RITA
To: YEDA RESEARCH AND DEVELOPMENT CO. LTD.
Reel/Frame 015135/0021 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 19, 2004
From: TENNE, RESHEF; FELDMAN, YISHAY; ZAK, ALLA; ROSENTSVEIG, RITA
To: YEDA RESEARCH AND DEVELOPMENT COMPANY LTD.
Reel/Frame 015006/0152 →
Priority Claims (1)
IL 134891 · Mar 6, 2000 · national
Continuity (1)
Related Publication 20040105808A1 · Jun 3, 2004