IP Library › Granted Patent US 12,327,871
Granted Patent B2
US 12,327,871 · App. 17/271,244 · Granted Jun 10, 2025

Polymer precursors for solid state electrolytes

Inventors: Richard M. Laine (Ann Arbor, MI); Eleni Temeche (Ann Arbor, MI); Xinyu Zhang (Ann Arbor, MI)
Assignee: The Regents of The University of Michigan
H01M4/62C01B21/082H01M4/131H01M4/1391H01M10/0562H01M50/403H01M50/414H01M50/434H01M50/437H01M50/449H01M50/451H01M50/497H01M2300/0068
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Quick Facts
Patent No.
US 12,327,871
App. No.
17/271,244
Granted
Jun 10, 2025
Kind
B2
Abstract

A method of synthesizing a precursor for making a polymer, glass, or ceramic material is provided. The method includes reacting OPCl 3 with NH 3 or MNH 2 , where M is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form O═P(NH2) 3 . The method then includes either: (i) reacting the O═P(NH 2 ) 3 with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor; or (ii) heating the O═P(NH 2 ) 3 to form a branched or cyclomeric compound, and reacting the branched or cyclomeric compound with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor. The precursor is an oligomer or a polymer. Uses for the precursor and the polymer, glass, or ceramic material as binders, sintering aids, adhesives, and electrolytes in battery components are also provided.

Claims (40)

1. A method of synthesizing a precursor for making a polymer, glass, or ceramic material, the method comprising:

reacting OPCl 3 with NH 3 or MNH 2 , where M is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form O═P(NH 2 ) 3 ; and either

i. reacting the O═P(NH 2 ) 3 with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor; or

ii. heating the O═P(NH 2 ) 3 to form a branched or cyclomeric compound; and

reacting the branched or cyclomeric compound with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor.

2. The method according to claim 1 , wherein the method comprises i. and the reacting the O═P(NH 2 ) 3 with the M1NH 2 is performed at a temperature of greater than or equal to about −50° C. to less than or equal to about 200° C. to form the precursor as the oligomer.

3. The method according to claim 2 , further comprising:

heating the oligomer to a temperature greater than or equal to about 40° C. to less than or equal to about 300° C. to increase the molecular weight of the oligomer.

4. The method according to claim 1 , wherein the method comprises i. and the reacting the O═P(NH 2 ) 3 with the M1NH 2 is performed at a temperature of greater than about 20° C. to less than or equal to about 500° C. to form the precursor as the polymer.

5. The method according to claim 4 , further comprising:

heating the polymer to a temperature greater than or equal to about 50° C. to less than or equal to about 400° C. to increase the ceramic yield of the polymer.

6. The method according to claim 1 , wherein the method comprises ii. and the reacting is performed at a temperature of greater than or equal to about 30° C. to less than or equal to about 150° C.

7. The method according to claim 1 , wherein the method comprises ii. and is performed on a surface of, and optionally in pores of, a solid-state battery component selected from the group consisting of a cathode, an anode, a solid electrode, and combinations thereof.

8. The method according to claim 1 , wherein the precursor has the formula M1 a M2 b P m H n N x O y S z , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof; M2 is Al, S, Se, C, Si, Ge, Sn, Zn, or combinations thereof; 1≤a≤10; 0≤b≤10; 0≤m≤50; and 0 ≤n≤60; 0≤x≤50; 0≤y≤20; and 0≤z≤20.

9. The method according to claim 8 , wherein the precursor is PON, Li x PON, Na x PON, SiPON, Li x SiPON, Na x SiPON, LiNaSiPON, or MgSiPON, where x is 1, 1.5, 3, or 6.

10. A method of making an ion-conducting polymer-precursor composite material, comprising:

adding the precursor formed according to the method of claim 1 to a solution comprising an ion-conducting polymer and a solvent to form a polymer-precursor solution;

casting the polymer-precursor solution on a plate; and

removing the solvent from the polymer-precursor solution to form the ion-conducting polymer-precursor composite material.

11. The method according to claim 10 , wherein the ion-conducting polymer is polyethylene oxide (PEO), polypropylene oxide (PPO), an ion-conducting carboxylate polymer, copolymers thereof, or mixtures thereof.

12. The method according to claim 10 , wherein the solvent is acetonitrile.

13. The method according to claim 10 , wherein the precursor is PON, Li x PON, Na x PON, SiPON, Li x SiPON, Na x SiPON, LiNaSiPON, or MgSiPON, where x is 1, 1.5, 3, or 6.

14. The method according to claim 10 , further comprising:

incorporating the ion-conducting polymer-precursor composite material into a solid-state battery as a solid composite electrolyte.

15. A method of synthesizing a precursor for making a polymer, glass, or ceramic material, the method comprising:

reacting OPCl 3 with NH 3 or MNH 2 , where M is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form O═P(NH 2 ) 3 , wherein the reacting is performed in a polar, aprotic solvent at a temperature of greater than or equal to about −50° C. to less than or equal to about 200° C.; and either

i. reacting the O═P(NH 2 ) 3 with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor; or

ii. heating the O═P(NH 2 ) 3 to form a branched or cyclomeric compound; and reacting the branched or cyclomeric compound with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor,

wherein the precursor is an oligomer or a polymer.

16. A method of making a polymer, glass, or ceramic material, the method comprising:

forming a precursor that is an oligomer or polymer by reacting OPCl 3 with NH 3 or MNH 2 , where M is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form O═P(NH 2 ) 3 ; and

either

i. reacting the O═P(NH 2 ) 3 with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor; or

ii. heating the O═P(NH 2 ) 3 to form a branched or cyclomeric compound; and reacting the branched or cyclomeric compound with M1NH 2 , where M1 is Li, Na, K, Mg, Ca, Ba, or combinations thereof, to form the precursor;

heating the precursor to a temperature of greater than or equal to about ambient temperature to less than or equal to about 1000° C. to form the polymer, glass, or ceramic material.

17. The method according to claim 16 , further comprising, prior to the heating:

applying the precursor that is an oligomer or polymer to at least a portion of a surface of a battery component selected from the group consisting of a cathode, an anode, a solid electrolyte, and combinations thereof,

wherein the applying is performed by a process selected from the group consisting of doctor blading, spreading, brushing, spin casting, pouring, pipetting, printing, spray coating, dip coating, and combinations thereof.

18. The method according to claim 16 , further comprising:

combining the precursor with at least one of an electrode active material, with a separator material, or with a solid-state electrolyte material to generate at least one of a composite electrode material, a composite separator material, or a composite solid-state electrolyte material.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 3, 2021
From: LAINE, RICHARD; TEMECHE, ELENI; ZHANG, XINYU
To: THE REGENTS OF THE UNIVERSITY OF MICHIGAN
Reel/Frame 055477/0430 →
Continuity (2)
Provisional Application 62725731 · Aug 31, 2018
Related Publication 20210340011A1 · Nov 4, 2021
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