US 11,881,579 B2
Cation energy storage device and methods
G. Tayhas R. Palmore, Providence, RI (US); and Dan Liu, Providence, RI (US)
Assigned to Brown University, Providence, RI (US)
Filed by Brown University, Providence, RI (US)
Filed on May 27, 2022, as Appl. No. 17/826,997.
Application 17/826,997 is a continuation of application No. 16/862,286, filed on Apr. 29, 2020, granted, now 11,374,211.
Application 16/862,286 is a continuation of application No. 15/564,711, granted, now 10,673,065, issued on Jun. 2, 2020, previously published as PCT/US2016/026496, filed on Apr. 7, 2016.
Claims priority of provisional application 62/144,021, filed on Apr. 7, 2015.
Prior Publication US 2023/0031332 A1, Feb. 2, 2023
This patent is subject to a terminal disclaimer.
Int. Cl. H01M 4/136 (2010.01); H01M 10/054 (2010.01); H01M 4/36 (2006.01); H01M 4/58 (2010.01); C01B 25/37 (2006.01); H01M 4/62 (2006.01); C01B 25/45 (2006.01); C01B 25/38 (2006.01); C01B 25/445 (2006.01); H01M 10/0525 (2010.01); H01M 10/052 (2010.01)
CPC H01M 4/136 (2013.01) [C01B 25/375 (2013.01); C01B 25/38 (2013.01); C01B 25/445 (2013.01); C01B 25/45 (2013.01); H01M 4/366 (2013.01); H01M 4/5825 (2013.01); H01M 4/62 (2013.01); H01M 4/625 (2013.01); H01M 10/054 (2013.01); H01M 10/0525 (2013.01); H01M 10/052 (2013.01)] 18 Claims
 
1. A composition comprising a material having an alluaudite crystal structure;
wherein the alluaudite crystal structure is made by a method comprising the steps of:
(1) dissolving reactants (A) (NH4)2Fe(SO4)2-6H2O, (B) H3PO4, and (C) NaOH in water with a 1:1:3 molar ratio (A:B:C), thereby forming a cathode solution; and
(2) heating the cathode solution, whereby said reactants crystallize in a monoclinic C 2/c space group consisting of pure alluaudite crystal; and
wherein the alluaudite crystal structure comprises formula (I):
Na1.702Fey(PO4)z  (formula I);
wherein y is greater than or equal to 3 and less than or equal to 3.5, and wherein z is greater than or equal to 1 and less than or equal to 3.
 
13. A method of making a material having an alluaudite crystal structure capable of providing an energy storage capacity of up to about 160 mAh/g, the method comprising the steps of:
(1) dissolving reactants (A) (NH4)2Fe(SO4)2-6H2O, (B) H3PO4, and (C) NaOH in water with a 1:1:3 molar ratio (A:B:C), thereby forming a cathode solution; and
(2) heating the cathode solution, whereby said reactants crystallize in a monoclinic C 2/c space group consisting of pure alluaudite crystal; and
wherein the alluaudite crystal structure comprises formula (I):
Na1.702Fey(PO4)z  (formula I);
wherein y is greater than or equal to 3 and less than or equal to 3.5, and wherein z is greater than or equal to 1 and less than or equal to 3.