Methods of forming a cathode material from a tutton's salt

Patent metadata

Field	Value
Publication number	US-2025346498-A1
Application number	US-202519203510-A
Country	US
Kind code	A1
Filing date	May 9, 2025
Priority date	May 10, 2024
Publication date	Nov 13, 2025
Grant date	—

Abstract

A method of preparing a cathode precursor material comprising combining a Tutton's salt exhibiting the chemical formula (NH4)2M(SO4)2·6H2O, wherein M comprises one or more metals, and water to form a Tutton's salt solution, adding a chelating agent to the Tutton's salt solution to form a Tutton's salt/chelating agent solution, and heating the Tutton's salt/chelating agent solution to form a cathode precursor material comprising a mixed metal composition of the Tutton's salt. Additional methods are disclosed.

First claim

What is claimed is:

1 . A method of preparing a cathode precursor material, the method comprising:
combining a Tutton's salt exhibiting the chemical formula (NH 4 ) 2 M(SO 4 ) 2 ·6H 2 O, wherein M comprises one or more metals, and water to form a Tutton's salt solution; adding a chelating agent to the Tutton's salt solution to form a Tutton's salt/chelating agent solution; and heating the Tutton's salt/chelating agent solution to form a cathode precursor material comprising a mixed metal composition of the Tutton's salt.

2 . The method of claim 1 , wherein combining a Tutton's salt exhibiting the chemical formula (NH 4 ) 2 M(SO 4 ) 2 ·6H 2 O comprises dissolving the Tutton's salt in ethylene glycol and water.

3 . The method of claim 1 , further comprising obtaining the Tutton's salt from one or more metal waste sources.

4 . The method of claim 1 , wherein M comprises one or more transition metals.

5 . The method of claim 1 , wherein M is one or more of Ni, Co, and Mn.

6 . The method of claim 1 , wherein adding a chelating agent to the Tutton's salt solution comprises adding one or more of ethylenediaminetetraacetic acid, citric acid, fulvic acid, phytic acid, gluconic acid, nitrilotriacetic acid, lactic acid, acetic acid, malic acid, oxalic acid, tartaric acid, lactic acid, picolinic acid, ascorbic acid, and formic acid to the Tutton's salt solution.

7 . The method of claim 1 , wherein heating the Tutton's salt solution comprises heating the Tutton's salt solution to a temperature of from about 100° C. to about 250° C.

8 . The method of claim 1 , wherein heating the Tutton's salt solution comprises precipitating the mixed metal composition of the Tutton's salt.

9 . The method of claim 1 , further comprising:
adding one or more metal sulfate salts to the Tutton's salt solution to adjust relative metal amounts of the cathode precursor material.

10 . A method of preparing a cathode precursor material, the method comprising:
combining a Tutton's salt comprising the chemical formula (NH 4 ) 2 M(SO 4 ) 2 ·6H 2 O, wherein M comprises nickel and cobalt in water to form a Tutton's salt solution; adding oxalic acid to the Tutton's salt solution to form a Tutton's salt/oxalic acid solution; and heating the Tutton's salt/oxalic acid solution to form a cathode precursor material comprising nickel and cobalt.

11 . The method of claim 10 , wherein heating the Tutton's salt/oxalic acid solution to form a cathode precursor material comprises forming the cathode precursor material comprising the chemical formula Ni x Mn y Co (1-x-y) (OH) 2 .

12 . The method of claim 10 , further comprising:
combining the cathode precursor material with a lithium source and heating to form lithium-metal particles.

13 . The method of claim 12 , wherein combining the cathode precursor material with a lithium source comprises combining the cathode precursor material with one or more of LiOH and Li 2 CO 3 .

14 . The method of claim 12 , wherein heating to form lithium-metal particles comprises heating to a temperature of from about 400° C. to about 950° C.

15 . The method of claim 12 , wherein forming lithium-metal particles comprises forming particles of LiNi x Mn y Co (1-x-y) O 2 .

16 . The method of claim 12 , wherein heating to form lithium-metal particles comprises forming the lithium-metal particles comprising lithium-Ni:Mn:Co particles comprising Ni:Mn:Co at a ratio of 8:1:1 Ni:Mn:Co or 6:2:2 Ni:Mn:Co.

17 . A method of preparing a cathode precursor material, the method comprising:
dissolving a Tutton's salt in water or in ethylene glycol and water to form a Tutton's salt solution; adding a chelating agent comprising one or more of citric acid and oxalic acid to the Tutton's salt solution to form a Tutton's salt/chelating agent solution; and heating the Tutton's salt/chelating agent solution to form a cathode precursor material comprising a mixed metal composition.

18 . The method of claim 16 , wherein dissolving a Tutton's salt comprises dissolving a Tutton's salt prepared from a metal feedstock recovered from spent lithium-ion batteries.

19 . The method of claim 17 , wherein heating the Tutton's salt/chelating agent solution to form a cathode precursor material comprising a mixed metal composition comprises heating the Tutton's salt/chelating agent solution to form a cathode precursor material comprising nickel, cobalt, and manganese.

20 . The method of claim 19 , further comprising:
combining the cathode precursor material with a lithium source to form lithium-metal particles; and disposing the lithium-metal particles on a substrate to form a cathode material comprising nickel, cobalt, manganese, and lithium.

Assignees

• Battelle Energy Alliance Llc

Inventors

• Klaehn John R
• Dufek Eric J
• Aldana Luis A Diaz
• Lister Tedd E
• Shi Meng
• Chen Bor-Rong
• Barnes Pete L

Classifications

• C01G53/50

  of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2 · CPC title

• C01G53/82

  Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements · CPC title

• H01M4/505

  of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy · CPC title

• C01G53/506 Primary

  with the molar ratio of nickel with respect to all the metals other than alkali metals higher than or equal to 0.8, e.g. Li(MzNixCoyMn1-x-y-z)O2 with x ≥ 0.8 · CPC title

• H01M4/525

  of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy · CPC title