IP Library Granted Patent US 11,634,341
Granted Patent B2
US 11,634,341 · App. 16/928,543 · Granted Apr 25, 2023

Nanolog and nanoparticles and method of formation

Inventors: Anna Kossoy (Rehovot, IL); Vladimir Aguf (Rehovot, IL); Alexander Margolin (Nes Ziona, IL)
Assignee: NANOTECH INDUSTRIAL SOLUTIONS
C01G41/00B01J23/30B01J27/047B01J35/002B01J35/0013B01J35/023B01J35/026B01J37/0215B01J37/08B01J37/20C01G41/02C04B14/36C04B28/04C08K3/30C08L23/06C08L77/02C08L79/08H01M4/5815B01J2523/69B82B3/0052B82Y30/00B82Y40/00C01P2002/72C01P2004/03C01P2004/04C01P2004/12C01P2004/16C01P2004/50C01P2004/61C01P2004/90C08K2003/3009C08K2201/003C08K2201/004H01M10/0525
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Quick Facts
Patent No.
US 11,634,341
App. No.
16/928,543
Granted
Apr 25, 2023
Kind
B2
Abstract

A nanostructure is provided that in one embodiment includes a cluster of cylindrical bodies. Each of the cylindrical bodies in the cluster are substantially aligned with one another so that their lengths are substantially parallel. The composition of the cylindrical bodies include tungsten (W) and sulfur (S), and each of the cylindrical bodies has a geometry with at least one dimension that is in the nanoscale. Each cluster of cylindrical bodies may have a width dimension ranging from 0.2 microns to 5.0 microns, and a length greater than 5.0 microns. In some embodiments, the cylindrical bodies are composed of tungsten disulfide (WS 2 ). In another embodiment the nanolog is a particle comprised of external concentric disulfide layers which encloses internal disulfide folds and regions of oxide. Proportions between disulfide and oxide can be tailored by thermal treatment and/or extent of initial synthesis reaction.

Claims (28)

1. A method of forming a nanostructure comprising:

reducing a particle size of tungsten oxide powder to produce a precursor material having a reduced particle size of less than 2 microns, wherein said reducing the particle size comprises grinding coarse WO 3 to fine size so that 50% of the powder will be below 1 μm;

heating the precursor material in a chamber to a reaction temperature in an inert atmosphere;

introducing hydrogen sulfide containing gas into the chamber after the reaction temperature has been reached to provide reduction and sulfidization reactions with the precursor material to provide a sulfided reactant structure; and

separating the sulfided reactant reaction into a powder containing clusters of cylindrical bodies composed of tungsten (W) and sulfur (S), wherein each of the cylindrical bodies has a geometry with at least one dimension that is in the nanoscale, and said each cluster of cylindrical bodies may have a width dimension ranging from 0.2 microns to 5.0 microns, and a length greater than 5.0 microns.

2. The method of claim 1 , wherein said reducing the particle size comprises grinding coarse WO 3 to said fine size so that 50% of the powder will be below 1 μm with a majority grain size being around 1 μm.

3. The method of claim 1 , wherein the reduced particle size is selected to provide a dimension for the clusters of cylindrical bodies.

4. The method of claim 3 , wherein heating the precursor material to the reaction temperature includes increases of a temperature of the chamber from ambient to said reaction temperature ranging from 750° C. to 950° C. while streaming a nitrogen gas (N 2 ) atmosphere through the chamber at atmospheric pressure.

5. The method of claim 1 , wherein said introducing hydrogen sulfide containing gas into the chamber after the reaction temperature has been reached comprises exchanging the nitrogen gas atmosphere with an atmosphere comprising 30% to 50% hydrogen sulfide (H 2 S) gas, and 30% to 50% hydrogen (H 2 ) gas.

6. The method of claim 5 , wherein said introducing hydrogen sulfide containing gas into the chamber comprises a mixture of N 2 /H 2 /H 2 S with ratio 1:2:2 for at least 1 hour.

7. The method of claim 5 , wherein the time period of said introducing hydrogen sulfide containing gas is selected to provide an oxide core within the cylindrical bodies, or to provide a hollow core within the cylindrical bodies.

8. A method of claim 5 , wherein forming the precursor material comprises:

reducing a particle size of WO 3 powder to produce a WO 3 precursor material having a reduced particle size of less than 2 microns;

heating the precursor material in a chamber to a reaction temperature ranging from 400° C. to 700° C. in an inert atmosphere;

introducing a reaction atmosphere including 5% to 45% hydrogen gas and 55% to 95% nitrogen gas into the chamber after the reaction temperature has been reached for a reaction time of less than 1 hour, wherein the WO 3 precursor material is converted to a reaction product of WO 2.9 ; and

separating the reaction product of WO 2.9 into a powder containing nanospheres composed of WO 2.9 .

9. The method of claim 8 , wherein the reduced particle size is greater than 0.3 microns.

10. The method of claim 8 , wherein the reaction temperature ranges from 500° C. to 600° C.

11. A method of forming a nanostructure comprising:

reducing a particle size of tungsten oxide powder to produce a precursor material having a reduced particle size of less than 2 microns, wherein the reduced particle size is selected to provide a dimension for the clusters of cylindrical bodies;

heating the precursor material in a chamber to a reaction temperature in an inert atmosphere;

introducing hydrogen sulfide containing gas into the chamber after the reaction temperature has been reached to provide reduction and sulfidization reactions with the precursor material to provide a sulfided reactant structure; and

separating the sulfided reactant reaction into a powder containing clusters of cylindrical bodies composed of tungsten (W) and sulfur (S), wherein each of the cylindrical bodies has a geometry with at least one dimension that is in the nanoscale, and said each cluster of cylindrical bodies may have a width dimension ranging from 0.2 microns to 5.0 microns, and a length greater than 5.0 microns.

12. A method of forming a nanostructure comprising:

reducing a particle size of tungsten oxide powder to produce a precursor material having a reduced particle size of less than 2 microns;

heating the precursor material in a chamber to a reaction temperature in an inert atmosphere;

introducing hydrogen sulfide containing gas into the chamber after the reaction temperature has been reached to provide reduction and sulfidization reactions with the precursor material to provide a sulfided reactant structure, wherein said introducing hydrogen sulfide containing gas into the chamber after the reaction temperature has been reached comprises exchanging the nitrogen gas atmosphere with an atmosphere comprising 30% to 50% hydrogen sulfide (H 2 S) gas, and 30% to 50% hydrogen (H 2 ) gas, wherein said introducing hydrogen sulfide containing gas into the chamber comprises a mixture of N 2 /H 2 /H 2 S with ratio 1:2:2 for at least 1 hour; and

separating the sulfided reactant reaction into a powder containing clusters of cylindrical bodies composed of tungsten (W) and sulfur (S), wherein each of the cylindrical bodies has a geometry with at least one dimension that is in the nanoscale, and said each cluster of cylindrical bodies may have a width dimension ranging from 0.2 microns to 5.0 microns, and a length greater than 5.0 microns.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 14, 2020
From: KOSSOY, ANNA; AGUF, VLADIMIR; MARGOLIN, ALEXANDER
To: NANOTECH INDUSTRIAL SOLUTIONS, INC.
Reel/Frame 053204/0782 →
Continuity (3)
Continuation 16075286
Provisional Application 62291229 · Feb 4, 2016
Related Publication 20210002144A1 · Jan 7, 2021