Electrochemical slurry compositions and methods for preparing the same

• US 9,484,569 B2
• Filed: 03/15/2013
• Issued: 11/01/2016
• Est. Priority Date: 06/13/2012
• Status: Active Grant

• Current Assignee: 24M Technologies, Inc.
• Original Assignee: 24M Technologies, Inc.
• Inventors: Doherty, Tristan, Duduta, Mihai, Limthongkul, Pimpa, Butros, Asli, Cross, James C. III
• Primary Examiner(s): Ryan, Patrick
• Assistant Examiner(s): Anthony, Julian
• Application Number:
  US13/832,861
• Publication Number:
  US 20130337319A1
• Time in Patent Office: 1,327 Days
• US Class Current: 1/1
• CPC Class Codes: C22B 26/12 Obtaining lithium
• CPC Class Codes: H01G 11/30 characterised by their material
• CPC Class Codes: H01G 11/38 Carbon pastes or blends; Binders or additives therein
• CPC Class Codes: H01G 11/46 Metal oxides
• CPC Class Codes: H01G 11/86 specially adapted for electrodes carbonisation or activation of carbon for the manufacture of electrodes H01G11/34
• CPC Class Codes: H01M 10/0525 Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
• CPC Class Codes: H01M 2004/021 Physical characteristics, e.g. porosity, surface area
• CPC Class Codes: H01M 2004/028 Positive electrodes
• CPC Class Codes: H01M 4/02 Electrodes composed of, or comprising, active material
• CPC Class Codes: H01M 4/0411 by extrusion
• CPC Class Codes: H01M 4/131 Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
• CPC Class Codes: H01M 4/136 Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
• CPC Class Codes: H01M 4/1391 of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
• CPC Class Codes: H01M 4/1397 of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
• CPC Class Codes: H01M 4/505 of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
• CPC Class Codes: H01M 4/525 of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
• CPC Class Codes: H01M 4/5825 Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
• CPC Class Codes: Y02E 60/10 Energy storage using batteries
• CPC Class Codes: Y02E 60/13 Energy storage using capacitors

Abstract

Embodiments described herein generally relate to semi-solid suspensions, and more particularly to systems and methods for preparing semi-solid suspensions for use as electrodes in electrochemical devices such as, for example batteries. In some embodiments, a method for preparing a semi-solid electrode includes combining a quantity of an active material with a quantity of an electrolyte to form an intermediate material. The intermediate material is then combined with a conductive additive to form an electrode material. The electrode material is mixed to form a suspension having a mixing index of at least about 0.80 and is then formed into a semi-solid electrode.

Claims

1. A method of preparing a semi-solid electrode, the method comprising:

combining a quantity of an active material with a quantity of an electrolyte and a conductive additive to form an electrode material;

mixing the electrode material to form a suspension having a mixing index of at least about 0.80;

controlling a temperature of the electrode material during mixing to control evaporation of the electrolyte therefrom;

forming the electrode material into a semi-solid electrode;

forming a second electrode; and

forming an electrochemical cell by combining the semi-solid electrode and the second electrode.

2. The method of claim 1, wherein the electrode material is a stable suspension when it is formed into the semi-solid electrode.

3. The method of claim 1, wherein the electrode material is mixed until the suspension has a mixing index of at least about 0.90.

4. The method of claim 3, wherein the electrode material is mixed until the suspension has a mixing index of at least about 0.95.

5. The method of claim 4, wherein the electrode material is mixed until the suspension has a mixing index of at least about 0.975.

6. The method of claim 1, further comprising:

mixing the electrode material until the electrode material has an electronic conductivity of at least about 10<sup>−

6</sup> S/cm.

7. The method of claim 6, wherein the electrode material is mixed until the electrode material has an electronic conductivity of at least about 10⁻

5 S/cm.

8. The method of claim 7, wherein the electrode material is mixed until the electrode material has an electronic conductivity of at least about 10⁻

4 S/cm.

9. The method of claim 8, wherein the electrode material is mixed until the electrode material has an electronic conductivity of at least about 10⁻

3 S/cm.

10. The method of claim 9, wherein the electrode material is mixed until the electrode material has an electronic conductivity of at least about 10⁻

2 S/cm.

11. The method of claim 1, further comprising:

mixing the electrode material until the electrode material has an apparent viscosity of less than about 100,000 Pa-s at an apparent shear rate of 1,000 s<sup>−

1</sup>.

12. The method of claim 11, wherein the electrode material is mixed until the electrode has an apparent viscosity of less than about 10,000 Pa-s at an apparent shear rate of 1,000 s⁻

1.

13. The method of claim 12, wherein the suspension is mixed until the suspension has an apparent viscosity of less than about 1,000 Pa-s at an apparent shear rate of 1,000 s⁻

1.

14. The method of claim 1, wherein the quantity of the active material is about 20% to about 75% by volume of the electrode material.

15. The method of claim 14, wherein the quantity of the active material is about 40% to about 75% by volume of the electrode material.

16. The method of claim 15, wherein the quantity of the active material is about 60% to about 75% by volume of the electrode material.

17. The method of claim 1, wherein the quantity of the electrolyte is about 25% to about 70% by volume of the electrode material.

18. The method of claim 17, wherein the quantity of the electrolyte is about 30% to about 50% by volume of the electrode material.

19. The method of claim 18, wherein the quantity of the electrolyte is about 20% to about 40% by volume of the electrode material.

20. The method of claim 1, wherein the quantity of the conductive material is about 0.5% to about 25% by volume of the electrode material.

21. The method of claim 20, wherein the quantity of the conductive material is about 1% to about 6% by volume of the electrode material.

22. The method of claim 1, wherein the mixing index is evaluated with a sample volume that is a cube of a formed semi-solid electrode thickness±

10%.

23. The method of claim 1, wherein the mixing index is evaluated with a sample volume of 0.12 mm³±

10%.

24. The method of claim 1, wherein the controlling includes decreasing the temperature of the electrode material during mixing.

25. The method of claim 24, wherein the controlling includes decreasing the temperature of the electrode material to lower than 10 degrees Celsius during mixing.

26. A method of preparing a semi-solid electrode, the method comprising:

combining a quantity of an active material with a quantity of an electrolyte and a conductive additive to form an electrode material;

mixing the electrode material to form a stable suspension having a mixing index of at least about 0.80 and an electronic conductivity of at least about 10<sup>−

6</sup> S/cm; and

controlling a temperature of the electrode material during mixing to control rate of evaporation of the electrolyte therefrom.

27. The method of claim 26, wherein the quantity of the active material is about 20% to about 75% by volume of the stable suspension, the quantity of the conductive additive is about 0.5% to about 25% by volume of the stable suspension, and the quantity of the electrolyte is about 25% to about 70% by volume of the stable suspension.

28. The method of claim 27, wherein the mixing supplies a specific mixing energy of about 90 J/g to about 150 J/g to the electrode material.

29. The method of claim 26, wherein the mixing supplies a specific mixing energy of at least about 90 J/g to the electrode material.

30. The method of claim 29, wherein the mixing supplies a specific mixing energy of at least about 100 J/g to the electrode material.

31. The method of claim 30, wherein the mixing supplies a specific mixing energy of about 100 J/g to about 120 J/g to the electrode material.

32. A method of preparing a semi-solid electrode, the method comprising:

combining an active material, an electrolyte, and a conductive additive in a vessel of a mixer;

mixing the active material, the electrolyte, and the conductive additive in the mixer to form an electrode material suspension having a mixing index of at least about 0.80; and

forming the electrode material into a semi-solid electrode,

wherein the mixing imparts a specific mixing energy to the active material, the electrolyte, and the conductive additive so as to control evaporation of the electrolyte therefrom.

33. The method of claim 32, wherein the vessel of the mixer is cooled to a temperature of lower than 10 degrees Celsius during mixing.

34. The method of claim 32, wherein the mixer is a high shear mixer.

35. The method of claim 32, wherein the mixer is a planetary mixer.

36. The method of claim 32, wherein the mixer is a centrifugal planetary mixer.

37. The method of claim 32, wherein the mixer is a sigma mixer.

38. The method of claim 32, wherein the mixer is a CAM mixer.

39. The method of claim 32, wherein the mixer is a roller mixer.