IP Library Granted Patent US 12,744,239
Granted Patent B2
US 12,744,239 · App. 18/349,770 · Granted Sep 22, 2026

Methods of making lithium ion conducting sulfide glass

Inventors: Steven J. Visco (Berkeley, CA); Yevgeniy S. Nimon (Danville, CA); Bruce D. Katz (Moraga, CA); Vitaliy Nimon (San Francisco, CA)
Assignee: PolyPlus Battery Company
H01M10/0562H01M10/0525H01M50/406H01M2300/0068
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Quick Facts
Patent No.
US 12,744,239
App. No.
18/349,770
Granted
Sep 22, 2026
Kind
B2
Abstract

A lithium ion-conductive solid electrolyte including a freestanding inorganic vitreous sheet of sulfide-based lithium ion conducting glass is capable of high performance in a lithium metal battery. Such an electrolyte is also manufacturable, and readily adaptable for battery cell and cell component manufacture, in a cost-effective, scalable manner using an automated machine based system, apparatus and methods based on inline spectrophotometry to assess and inspect the quality of such vitreous solid electrolyte sheets and associated components. Suitable manufacturing methods can involve providing a sulfur precursor, providing a boron precursor material having lithium as a second constituent, combining the sulfur and boron precursor materials to form a precursor mixture, melting the mixture, and cooling the melt to form a solid lithium ion conducting glass. The glass may have a Li+ conductivity of at least 10 −5 S/cm. The boron precursor material may be synthesized by reducing boron oxide to boron metal by heating the boron oxide in direct contact with lithium metal.

Claims (29)

1 . A method of making a lithium ion conducting sulfide glass, the method comprising:

i) providing a sulfur precursor material comprising sulfur as a main constituent element;

ii) providing a boron precursor material comprising boron as a first constituent element and lithium as a second constituent, the boron precursor material formed by making a lithium boron alloy or intermetallic via chemical reduction of a boron compound to elemental boron by lithium metal;

iii) combining the sulfur and boron precursor materials to form a precursor mixture;

iv) melting the mixture; and

v) cooling the melt to form a solid lithium ion conducting glass having Li + conductivity greater than or equal to 10 −5 S/cm.

2 . The method of claim 1 wherein the boron precursor material essentially consists of boron and lithium as constituent elements.

3 . The method of claim 1 wherein the boron precursor material is essentially devoid of magnesium as an impurity element.

4 . The method of claim 1 , wherein the lithium metal derives from a lithium precursor material that comprises lithium as a main constituent element; and further wherein the combining further includes adding the lithium precursor material to the precursor mixture.

5 . The method of claim 4 wherein the lithium precursor material is lithium metal.

6 . The method of claim 4 wherein the lithium precursor material is a lithium sulfide compound.

7 . The method of claim 6 wherein the lithium precursor material is Li 2 S.

8 . The method of claim 1 , wherein the sulfur precursor material is elemental sulfur.

9 . The method of claim 1 , wherein the boron precursor material is an alloy of lithium and boron, Li x B.

10 . The method of claim 9 wherein x is less than or equal to 1.

11 . The method of claim 9 wherein x is greater than 1.

12 . The method of claim 1 wherein the boron compound is boron oxide.

13 . A method of making a lithium ion conducting sulfide glass, the method comprising:

i) providing a sulfur precursor material comprising sulfur as a main constituent element;

ii) synthesizing a boron precursor material by reducing a boron compound to boron metal of greater than 99% purity by heating the boron compound in direct contact with lithium metal, wherein the boron precursor comprises boron as a first constituent element;

iii) combining the sulfur and boron precursor materials to form a precursor mixture;

iv) melting the precursor mixture; and

v) cooling the melt to form a solid lithium ion conducting glass.

14 . The method of claim 13 wherein the boron precursor material comprises boron as a first constituent element and lithium as a second constituent element.

15 . The method of claim 13 wherein the reducing the boron compound to boron metal is performed in the absence of magnesium metal.

16 . The method of claim 13 wherein the boron compound is boron oxide.

17 . The method of claim 16 wherein the sulfur precursor material is elemental sulfur.

18 . The method of claim 17 wherein the boron precursor material is an alloy of lithium and boron, Li x B.

19 . The method of claim 13 further comprising providing a lithium precursor material that comprises lithium as a main constituent element; and further wherein the combining includes adding the lithium precursor material to the precursor mixture.

Continuity (19)
Continuation 16509385 · Jul 11, 2019
Continuation In Part 16174058 · Oct 29, 2018
Continuation In Part 15726302 · Oct 5, 2017
Continuation 15380989 · Dec 15, 2016
Continuation In Part 14954812 · Nov 30, 2015
Continuation In Part 14954816 · Nov 30, 2015
Provisional Application 62344349 · Jun 1, 2016
Provisional Application 62342155 · May 26, 2016
Provisional Application 62271180 · Dec 22, 2015
Provisional Application 62222408 · Sep 23, 2015
Provisional Application 62196247 · Jul 23, 2015
Provisional Application 62171561 · Jun 5, 2015
Provisional Application 62165791 · May 22, 2015
Provisional Application 62149250 · Apr 17, 2015
Provisional Application 62146809 · Apr 13, 2015
Provisional Application 62126319 · Feb 27, 2015
Provisional Application 62111048 · Feb 2, 2015
Provisional Application 62086641 · Dec 2, 2014
Related Publication 20240088433A1 · Mar 14, 2024
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