Layer-by-layer sorting of rhenium disulfide via high-density isopycnic density gradient ultracentrifugation

Patent metadata

Field	Value
Publication number	US-10702803-B2
Application number	US-201715800666-A
Country	US
Kind code	B2
Filing date	Nov 1, 2017
Priority date	Nov 1, 2016
Publication date	Jul 7, 2020
Grant date	Jul 7, 2020

Abstract

Separation of rhenium disulfide nanomaterials and related fluid density gradient media.

First claim

We claim:

1. A method for separating planar nanomaterials by thickness, the method comprising:
centrifuging a rhenium disulfide nanomaterial composition in contact with an aqueous fluid medium comprising a density gradient and an adjuvant component providing said medium a buoyant density greater than the buoyant density of said rhenium disulfide nanomaterial composition, wherein the rhenium disulfide nanomaterial composition comprises one or more surface active components and a polydisperse population of planar rhenium disulfide nanomaterials which is polydisperse at least with respect to thickness and has a mean thickness on the order of nanometers; and
separating the rhenium disulfide nanomaterial composition into two or more separation fractions each comprising a subpopulation of planar rhenium disulfide nanomaterials from the polydisperse population, wherein the subpopulation of planar rhenium disulfide nanomaterials in at least one of the two or more separation fractions has a mean thickness that is less than the mean thickness of the polydisperse population.

2. The method of claim 1 , wherein the planar nanomaterials comprise mono- and bilayer rhenium disulfide nanomaterials.

3. The method of claim 1 , wherein the one or more surface active components comprise a planar organic group.

4. The method of claim 3 , wherein the one or more surface active components is sodium cholate.

5. The method of claim 1 , wherein said aqueous fluid medium comprises iodixanol and an adjuvant component to increase the buoyant density of said medium.

6. The method of claim 5 , wherein said adjuvant component is CsCl.

7. A method for separating rhenium disulfide nanomaterials by thickness, the method comprising:
sonicating a rhenium disulfide material in a first fluid medium to provide a rhenium disulfide nanomaterial composition;
centrifuging the rhenium disulfide nanomaterial composition in contact with an aqueous second fluid medium comprising a density gradient and an adjuvant component providing said medium a buoyant density greater than the buoyant density of said rhenium disulfide nanomaterial composition, wherein the rhenium disulfide nanomaterial composition comprises one or more surface active components and a polydisperse population of planar rhenium disulfide nanomaterials comprising monolayer, bilayer, trilayer and n-layer rhenium disulfide nanomaterials, where n is an integer in the range of 4 to 10; and
separating the rhenium disulfide nanomaterial composition into two or more separation fractions each comprising a subpopulation of planar rhenium disulfide nanomaterials from the polydisperse population, wherein the subpopulation in at least one of the two or more separation fractions comprises greater than about 50% of the monolayer rhenium disulfide nanomaterials, bilayer rhenium disulfide nanomaterials, trilayer rhenium disulfide nanomaterials, or combinations thereof.

8. The method of claim 7 , wherein the subpopulation in at least one of the two or more separation fractions comprises greater than about 50% of the monolayer or bilayer rhenium disulfide nanomaterials, or a combination thereof.

9. The method of claim 7 , wherein the one or more surface active components comprise a compound having a planar organic group.

10. The method of claim 8 , wherein the one or more surface active components is sodium cholate.

11. The method of claim 7 , wherein the subpopulation in one of the separation fractions comprises greater than about 50% of the monolayer rhenium disulfide.

12. The method of claim 7 , wherein said second aqueous fluid medium comprises iodixanol and CsCl.

13. The method of claim 12 , wherein the subpopulation in one of the separation fractions comprises greater than about 50% of the monolayer rhenium disulfide and is deposited on the substrate.

14. The method of claim 13 , wherein the substrate and rhenium disulfide deposited thereon are incorporated into an electronic device.

15. The method of claim 7 , wherein a subpopulation of at least one of the two or more separation fractions is deposited on a substrate.

16. A method for separating monolayer rhenium disulfide nanomaterials, the method comprising:
centrifuging a rhenium disulfide nanomaterial composition in contact with an aqueous fluid medium comprising iodixanol and CsCl, said medium having a density gradient, wherein the rhenium disulfide nanomaterial composition comprises sodium cholate and a polydisperse population of planar rhenium disulfide nanomaterials comprising monolayer, bilayer and trilayer rhenium disulfide nanomaterials; and
separating the rhenium disulfide nanomaterial composition into two or more separation fractions each comprising a subpopulation of planar rhenium disulfide nanomaterials from the polydisperse population, wherein the subpopulation in one of the two or more separation fractions comprises greater than about 50% of the monolayer rhenium disulfide nanomaterials.

17. The method of claim 16 , wherein a subpopulation of at least one of the two or more separation fractions is deposited on a substrate.

18. The method of claim 17 , wherein the subpopulation in one of the separation fractions comprises greater than about 50% of the monolayer rhenium disulfide and is deposited on the substrate.

19. The method of claim 18 , wherein the substrate and rhenium disulfide deposited thereon are incorporated into an electronic device.

20. The method of claim 16 , wherein said fluid medium and said sodium cholate are removed from a said separation fraction.

21. A method of using an increased buoyant density limit for separating planar nanomaterials by thickness, the method comprising:
providing a composition comprising a nanomaterial and one or more surface active components, said composition comprising a polydisperse population of planar nanomaterials comprising monolayer, bilayer, trilayer and n-layer nanomaterials, where n is an integer selected from 4-about 10, said composition having a buoyant density;
providing an aqueous fluid medium comprising a density gradient, said medium having a maximum buoyant density;
introducing a component to said medium, said component having a maximum density limit greater than said composition buoyant density, to provide said medium a buoyant density greater than said composition buoyant density;
centrifuging said nanomaterial composition in contact with said aqueous fluid medium; and
separating said nanomaterial composition into two or more separation fractions each comprising a subpopulation of planar nanomaterials from the polydisperse population, wherein the subpopulation of planar nanomaterials in at least one of the two or more separation fractions comprises a greater population of the monolayer nanomaterials, bilayer nanomaterials, or a combination thereof as compared to adjacent separation fractions;
wherein said nanomaterial is rhenium disulfide.

22. The method of claim 21 wherein the planar nanomaterials comprise mono- and bi-layer rhenium disulfide nanomaterials.

23. The method of claim 21 wherein the one or more surface active components comprise a planar organic group.

24. The method of claim 23 wherein the one or more surface active components is sodium cholate.

25. The method of claim 21 wherein said aqueous fluid medium comprises iodixanol.

26. The method of claim 25 wherein said component introduced to said fluid medium is CsCl.

27. T

Assignees

• Univ Northwestern

Inventors

• Hersam Mark C
• Kang Joohoon

Classifications

• C01G47/00 Primary

  Compounds of rhenium · CPC title

• B03D3/00

  Differential sedimentation · CPC title

• C01P2004/20

  extending in two dimensions, e.g. plate-like · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title