Mechanochemical synthesis of alane

Patent metadata

Field	Value
Publication number	US-10273156-B2
Application number	US-201515118788-A
Country	US
Kind code	B2
Filing date	Feb 12, 2015
Priority date	Feb 12, 2014
Publication date	Apr 30, 2019
Grant date	Apr 30, 2019

Abstract

In some examples, a method of forming alane (AlH 3 ), the method comprising reacting one of: 1) a MAlH 4 , wherein M is an alkali metal; 2) alkali-metal hydride, MH; or 3) alkali-metal with one or more aluminum halides (AlX 3 , where X is a halogen), via a mechanochemical process, to form the alane, wherein the reaction is substantially solvent free and carried out in an environment with a temperature between approximately 250 K and approximately 330 K.

First claim

The invention claimed is:

1. A method of forming alane (AlH 3 ), the method comprising reacting one of: 1) a MAlH 4 , wherein M is an alkali metal; 2) an alkali metal hydride, MH; or 3) an alkali metal with one or more aluminum halides (AlX 3 , where X is a halogen), via a mechanochemical process, to form the alane,
wherein the reaction is solvent free and carried out in an environment with a temperature between approximately 250 K and approximately 330 K,
wherein the reaction is carried out in a pressure of hydrogen or a pressure of an inert gas, wherein the pressure of the hydrogen or the pressure of the inert gas is greater than or equal to a critical pressure for the reaction, and
wherein the pressure of hydrogen or the pressure of the inert gas is greater than atmospheric pressure.

2. The method of claim 1 , wherein no heat is added externally or removed by cooling during the reaction.

3. The method of claim 1 , wherein the temperature of the environment is between approximately 283 K and approximately 313 K.

4. The method of claim 1 , wherein the reaction is carried out at the pressure of the hydrogen less than approximately 350 bar.

5. The method of claim 1 , wherein the reaction is carried out at the pressure of the inert gas less than approximately 350 bar.

6. The method of claim 5 , wherein the inert gas comprises helium, neon, argon, krypton, xenon, or a mixture thereof.

7. The method of claim 5 , wherein the inert gas comprises a saturated or unsaturated linear, branched or cyclic hydrocarbon that contains from 1 to 5 carbon atoms per molecule.

8. The method of claim 5 , wherein the inert gas comprises a gas that does not chemically react with any of the reactants and with the formed AlH 3 .

9. The method of claim 1 , wherein the reaction is carried out in the presence of excess MAlH 4 .

10. The method of claim 9 , wherein the amount of MAlH 4 varies between approximately 3.01 and approximately 10 moles per mole of the aluminum halide.

11. The method of claim 1 , wherein no metallic Al is formed by the reaction.

12. The method of claim 1 , wherein the reaction yields are greater than approximately 50% alane.

13. The method of claim 12 , wherein the reaction yields are greater than approximately 90% alane.

14. The method of claim 1 , wherein the mechanochemical process comprises at least one of ball milling, jet milling, or screw extrusion.

15. The method of claim 1 , wherein the reaction is carried out at the pressure of hydrogen or the inert gas that is greater than or equal to the critical pressure for the reaction, wherein the critical pressure for the reaction is a threshold pressure at or above which metallic aluminum does not form in quantities that can be detected by standard analytical tools.

16. The method of claim 1 , wherein the critical pressure is dependent on at least one of milling energy, milling speed, molecular weight of the inert gas, and powder to milling media ratio.

17. The method of claim 1 , wherein the one of the MAlH 4 , the alkali metal hydride, MH, or the alkali metal is in a stoichiometric excess.

18. The method of claim 1 , further comprising controlling a milling speed and a ball to powder ratio of the mechanochemical process to obtain the critical pressure greater than the atmospheric pressure.

Assignees

• Univ Iowa State Res Found Inc

Inventors

• Gupta Shalabh
• Pecharsky Vitalij K
• Kobayashi Takeshi
• Pruski Marek
• Hlova Ihor

Classifications

• C01B6/06 Primary

  Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof · CPC title

• C01B3/0026

  Metals or metal hydrides · CPC title

• Y02E60/32

  Hydrogen storage · CPC title