IP Library › Granted Patent US 11,158,845
Granted Patent B2
US 11,158,845 · App. 16/478,327 · Granted Oct 26, 2021

Low temperature, high yield synthesis of nanomaterials and composites from Zintl phases

Inventors: Michael J. Wagner (Rockville, MD); Nathan A. Banek (Arlington, VA)
Assignee: The George Washington University
H01M4/134H01M4/133H01M4/463H01M4/466H01M10/0525
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Quick Facts
Patent No.
US 11,158,845
App. No.
16/478,327
Granted
Oct 26, 2021
Kind
B2
Abstract

The present disclosure relates to an improved process for the synthesis of nanomaterials and composites from Zintl phases. The nanomaterials and composites are useful, for example, as ion storage materials.

Claims (49)

1. A process for preparing an ion storage material, the process comprising:

a) reacting a Zintl compound with an aluminum compound, optionally in the presence of a support material;

b) optionally isolating the resulting product; and

c) optionally purifying the isolated product,

wherein step a) is conducted:

i) by mechanical milling;

ii) in a solvent; or

iii) in a molten salt comprising the aluminum compound in combination with one or more alkali metal halides, alkali earth metal halides, or any combination thereof.

2. The process according to claim 1 , wherein the the Zintl compound is a compound comprising a) a Group 1 metal, a Group 2 metal, or any combination thereof, and b) a post transition metal or metalloid, or any combination thereof.

3. The process according to claim 1 , wherein

the Group 1 and/or Group 2 metal is selected from Li, Na K, Rh, Cs, Be, Mg, Cu, Sr, Ba, and any combination thereof; and

the post transition metal or metalloid is selected from B, Si, Ga, Ge, As, In, Sn, Sb, Te, Tl, Pb, Bi, and any combination thereof.

4. The process according to claim 1 , wherein the Group 1 and/or Group 2 metal is Mg and the post transition metal or metalloid is Si.

5. The process according to claim 1 , wherein the Zintl compound is Mg 2 Si.

6. The process according to claim 1 , wherein the aluminum compound is selected from halides, oxides, alkoxides, hydroxides, sulfates, sulfites, nitrates, nitrites, phosphates, and phosphites of aluminum, hydrates of any of the foregoing, and any combination thereof.

7. The process according to claim 1 , wherein the aluminum compound is an aluminum halide.

8. The process according to claim 1 ,, wherein the aluminum compound is AlCl 3 , AlBr 3 , AlI 3 , or any combination thereof.

9. The process according to claim 1 , wherein the support material, if present, is selected from carbonaceous materials, metals, glasses, oxides, nitrides, borides, and any combination thereof.

10. The process according to claim 1 , wherein the support material, if present, is a carbonaceous material selected from carbon spheres, graphite, carbon nanotubes, carbon nanofibers, carbon fibers, hard and soft carbons, activated carbons, carbon blacks, amorphous carbons, soots, graphene, fullerenes, coal, coke, fossil fuel derived materials, biomass, biochar, charcoal, chars, and any combination thereof.

11. The process according to claim 1 , wherein the support material, if present, is selected from a multiwall graphene nanoshell (MGNS), graphite, and any combination thereof.

12. The process according to claim 1 , wherein step a) is conducted at a temperature ranging between about 50° C. and about 600° C.

13. The process according to claim 1 , wherein step c) comprises adding an inorganic acid.

14. The process according to claim 1 , wherein step c) comprises adding hydrochloric acid.

15. The process according to claim 1 , wherein the ion storage material comprises between 0 and about 20 wt. % Al.

16. The process according to claim 1 , wherein step a) is conducted at a temperature ranging between about 50° C. and about 200° C.

17. The process according to claim 1 , wherein step a) is conducted at a temperature ranging between about 100° C. and about 200° C.

18. The process according to claim 1 , wherein step a) is conducted at a temperature ranging between about 120° C. and about 180° C.

19. The process according to claim 1 , wherein step a) is conducted at a temperature of about 125° C. or about 180° C.

20. The process according to claim 1 , wherein the ion storage material comprises between 0 and about 15 wt. % Al.

21. The process according to claim 1 , wherein the ion storage material comprises between 0 and about 10 wt. % Al.

22. The process according to claim 1 , wherein the ion storage material comprises between 0 and about 5 wt. % Al.

23. The process according to claim 1 , wherein the ion storage material comprises between 0 and about 4 wt. % Al.

24. The process according to claim 1 , wherein the ion storage material comprises between about 0 and about 3 wt. % Al.

25. The process according to claim 1 , wherein the ion storage material comprises between about 0 and about 2 wt. % Al.

26. The process according to claim 1 , wherein the ion storage material comprises between about 0 and about 1 wt. % Al.

27. The process according to claim 1 , wherein the ion storage material comprises or between about 1 and about 3 wt. % Al.

28. The process according to claim 1 , wherein step a) is conducted by mechanical milling.

29. The process according to claim 1 , wherein step a) is conducted in a solvent.

30. The process according to claim 1 , wherein step a) is conducted in a molten salt comprising the aluminum compound in combination with one or more alkali metal halides, alkali earth metal halides, or any combination thereof.

31. A process for preparing an ion storage material, the process comprising:

a) reacting a Zintl compound with an aluminum compound, optionally in the presence of a support material;

b) optionally isolating the resulting product; and

c) optionally purifying the isolated product;

wherein step a) is conducted in a solvent selected from aromatic hydrocarbons, nonaro atic hydrocarbons, amines, aprotic solvents, and any combination thereof.

32. A process for preparing an ion storage material, the process comprising:

a) reacting a Zintl compound with an aluminum compound, optionally in the presence of a support material;

b) optionally isolating the resulting product; and

optionally purifying the isolated product;

wherein step a) is conducted in a solvent selected from cyclohexane, toluene, or a combination thereof.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 30, 2019
From: WAGNER, MICHAEL J.; BANEK, NATHAN A.
To: THE GEORGE WASHINGTON UNIVERSITY
Reel/Frame 049911/0677 →
Continuity (2)
Provisional Application 62450392 · Jan 25, 2017
Related Publication 20200014024A1 · Jan 9, 2020