Method of purifying nanodiamond powder and purified nanodiamond powder

Patent metadata

Field	Value
Publication number	US-9446956-B2
Application number	US-201514594002-A
Country	US
Kind code	B2
Filing date	Jan 9, 2015
Priority date	Jun 28, 2012
Publication date	Sep 20, 2016
Grant date	Sep 20, 2016

Abstract

A method of purifying a nanodiamond powder includes preparing the nanodiamond powder, heating the nanodiamond powder at between 450° C. and 470° C. in an atmosphere including oxygen, performing a hydrochloric acid treatment on the heated nanodiamond powder, and performing a hydrofluoric acid treatment on the nanodiamond powder obtained after performing the hydrochloric acid treatment.

First claim

What is claimed is:

1. Nanodiamond powder comprising sp 3 carbon, wherein
a content of sp 2 carbon is less than 0.01 wt %; and
a content of S (sulfur), Fe (iron), Al (aluminum) and Si (silicon) is each less than 0.01 wt %, wherein the nanodiamond powder comprises clusters of a nanodiamond particle, and an average diameter of the cluster is less than 102 nm.

2. The nanodiamond powder according to claim 1 , wherein
a content of W (tungsten), Ta (tantalum), Cr (chromium), Mn (manganese), Ag (silver), Ca (calcium), Cu (copper), and Ti (titanium) is each less than 0.01 wt %.

3. The nanodiamond powder according to claim 2 , wherein the content of W (tungsten), Ta (tantalum), Cr (chromium), Mn (manganese), Ag (silver), Ca (calcium), Cu (copper), and Ti (titanium) is each determined by EDAX.

4. The nanodiamond powder according to claim 1 , wherein
carbon and oxygen are present; and
S (sulfur), W (tungsten), Ta (tantalum), Fe (iron), Cr (chromium), Mn (manganese), Al (aluminum), Ag (silver), Ca (calcium), Cu (copper), Ti (titanium), and Si (silicon) are not substantially present, wherein presence is determined by EDAX.

5. The nanodiamond powder according to claim 4 , wherein the content of S (sulfur), W (tungsten), Ta (tantalum), Fe (iron), Cr (chromium), Mn (manganese), Al (aluminum), Ag (silver), Ca (calcium), Cu (copper), Ti (titanium), and Si (silicon) is each determined by EDAX.

6. The nanodiamond powder according to claim 1 , wherein the content of S (sulfur), Fe (iron), Al (aluminum) and Si (silicon) is each determined by EDAX.

7. The nanodiamond powder according to claim 1 , wherein the content of sp 2 carbon is determined by EELS.

8. The nanodiamond powder according to claim 1 , wherein an average diameter of particles is less than 10 nm.

9. The nanodiamond powder according to claim 1 , wherein a color of the powder is white or colorless.

10. The nanodiamond powder according to claim 1 , wherein a color of the powder is blue.

11. The nanodiamond powder according to claim 1 , obtained by a process comprising:
preparing the nanodiamond powder;
heating the nanodiamond powder at between 450° C. and 470° C. in an atmosphere including oxygen to reduce a content of sp 2 carbon;
after heating the nanodiamond powder to reduce the content of sp 2 carbon, performing a hydrochloric acid treatment on the heated nanodiamond powder; and
performing a hydrofluoric acid treatment on the nanodiamond powder obtained after the hydrochloric acid treatment,
wherein a content of S (sulfur), Fe (iron), Al (aluminum) and Si (silicon) is each reduced.

12. The nanodiamond powder according to claim 1 , obtained by a process comprising:
performing a density gradient separation process to separate the nanodiamond powder according to one or more of particle size and number of particle clusters.

13. Nanodiamond powder comprising clusters of a nanodiamond particle comprising sp 3 carbon, wherein
an average diameter of clusters is less than 45.2 nm;
a content of sp 2 carbon is less than 0.01 wt %; and
a content of S (sulfur), Fe (iron), Al (aluminum) and Si (silicon) is each less than 0.01 wt %.

14. The nanodiamond powder according to claim 13 , wherein an average diameter of particles is less than 10 nm.

15. The nanodiamond powder according to claim 13 , wherein a color of the powder is white or colorless.

16. The nanodiamond powder according to claim 13 , wherein a color of the powder is blue.

17. The nanodiamond powder according to claim 13 , wherein
a content of W (tungsten), Ta (tantalum), Cr (chromium), Mn (manganese), Ag (silver), Ca (calcium), Cu (copper), and Ti (titanium) is each less than 0.01 wt %.

18. The nanodiamond powder according to claim 17 , wherein the content of W (tungsten), Ta (tantalum), Cr (chromium), Mn (manganese), Ag (silver), Ca (calcium), Cu (copper), and Ti (titanium) is each determined by EDAX.

19. The nanodiamond powder according to claim 13 , wherein
carbon and oxygen are present; and
S (sulfur), W (tungsten), Ta (tantalum), Fe (iron), Cr (chromium), Mn (manganese), Al (aluminum), Ag (silver), Ca (calcium), Cu (copper), Ti (titanium), and Si (silicon) are not substantially present, wherein presence is determined by EDAX.

20. The nanodiamond powder according to claim 19 , wherein the content of S (sulfur), W (tungsten), Ta (tantalum), Fe (iron), Cr (chromium), Mn (manganese), Al (aluminum), Ag (silver), Ca (calcium), Cu (copper), Ti (titanium), and Si (silicon) is each determined by EDAX.

21. The nanodiamond powder according to claim 13 , wherein the content of S (sulfur), Fe (iron), Al (aluminum) and Si (silicon) is each determined by EDAX.

22. The nanodiamond powder according to claim 13 , wherein the content of sp 2 carbon is determined by EELS.

23. The nanodiamond powder according to claim 13 , obtained by a process comprising:
preparing the nanodiamond powder;
heating the nanodiamond powder at between 450° C. and 470° C. in an atmosphere including oxygen to reduce a content of sp 2 carbon;
after heating the nanodiamond powder to reduce the content of sp 2 carbon, performing a hydrochloric acid treatment on the heated nanodiamond powder; and
performing a hydrofluoric acid treatment on the nanodiamond powder obtained after the hydrochloric acid treatment,
wherein a content of S (sulfur), Fe (iron), Al (aluminum) and Si (silicon) is each reduced.

24. The nanodiamond powder according to claim 13 , obtained by a process comprising:
performing a density gradient separation process to separate the nanodiamond powder according to one or more of particle size and number of particle clusters.

Assignees

• Canon Kk
• Univ Arizona
• Univ Arizona

Inventors

• Gangopadhyay Palash
• Norwood Robert A
• Miles Alexander Ashton
• Kato Jun
• Virji Shabnam
• Miyawaki Mamoru

Classifications

• C30B25/165

  the flow of the reactive gases · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C30B25/00

  Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth · CPC title

• C30B29/04

  Diamond · CPC title