Methods of making and inspecting a web of vitreous lithium sulfide separator sheet and lithium electrode assemblies

Patent metadata

Field	Value
Publication number	US-2017229731-A1
Application number	US-201615380989-A
Country	US
Kind code	A1
Filing date	Dec 15, 2016
Priority date	Dec 2, 2014
Publication date	Aug 10, 2017
Grant date	—

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 by providing a high degree of lithium ion conductivity while being highly resistant to the initiation and/or propagation of lithium dendrites. Such an electrolyte is also itself manufacturable, and readily adaptable for battery cell and cell component manufacture, in a cost-effective, scalable manner. An automated machine based system, apparatus and methods assessing and inspecting the quality of such vitreous solid electrolyte sheets, electrode sub-assemblies and lithium electrode assemblies can be based on spectrophotometry and can be performed inline with fabricating the sheet or web (e.g., inline with drawing of the vitreous Li ion conducting glass) and/or with the manufacturing of associated electrode sub-assemblies and lithium electrode assemblies and battery cells.

First claim

1 . A method of making a battery cell separator layer, the method comprising:
i) providing a dense solid inorganic glass electrolyte sheet having first and second opposing principal side surfaces; and ii) spectrophotometrically inspecting the sheet for defects or flaws.

2 . The method of claim 1 , wherein the spectrophotometrically inspecting the glass sheet further comprises characterizing and evaluating any defects or flaws present at or within 10 μm of one or more of the first principal side surface and the second principal side surface of the solid electrolyte glass sheet.

3 . The method of claim 1 , wherein the dense glass sheet is freestanding.

4 . The method of claim 1 , wherein the first and second opposing surfaces are uncoated, and in direct contact with the ambient environment.

5 . The method of claim 1 , wherein the spectrophotometric inspection is based on a comparison of incident and transmitted light intensities at various wavelengths.

6 . A method of making a battery cell component, the method comprising:
i) providing an electrode subassembly comprising:
a dense solid inorganic glass electrolyte sheet as an ionically conductive separator layer having first and second opposing principal side surfaces; and
a material layer coated on the first principal side surface; and
ii) spectrophotometrically inspecting the subassembly for defects or flaws. wherein the interface between the dense glass sheet and the material layer is spectrophotometrically inspected for flaws or inclusions at the interface.

7 . The method of claim 6 , wherein the material layer is reflective of light.

8 . The method of claim 7 , wherein the material layer is a metal that is not lithium metal.

9 . The method of claim 7 , wherein the spectrophotometric inspection is based on reflected light intensities at various wavelengths.

10 . A method of making a battery cell, the method comprising:
i) providing an electrode assembly comprising:
a dense solid inorganic glass electrolyte sheet as an ionically conductive separator layer having first and second opposing principal side surfaces; and
a material layer comprising electroactive lithium disposed on the first principal side surface; and
ii) spectrophotometrically inspecting the electrode assembly for defects or flaws at the interface between the lithium metal layer and the glass sheet.

11 . The method of claim 1 , wherein the spectrophotometric inspection involves light attenuation.

12 . The method of claim 11 , wherein the light is in the visible region.

13 . The method of claim 10 , wherein the material layer is lithium metal.

14 . The method of claim 10 , wherein the material layer is a lithium alloy.

15 . The method of claim 11 , wherein the light attenuation is used to characterize and evaluate concentrations of any scattering centers in the bulk of the glass sheet and at the interface between the glass sheet and the material layer,.

16 . The method of claim 10 , wherein changes in reflectivity of the interface are monitored in order to identify areas of low Li reactivity at the interface.

17 . The method of claim 10 , wherein the method involves monitoring reactions at the interface in real time.

18 . The methods of claim 1 , wherein the spectrophotometric inspection is an automated inspection comprising:
i. providing a source of light of a specified wavelength, or the wavelength selectable from a range of wavelengths; ii. providing sensors for measuring intensity of the light; iii. providing a computer that interfaces with the sensors for collecting light intensity data; iv. shining the light at the solid electrolyte glass sheet for transmission or reflection measurements; v. measuring the transmitted or reflected light intensity using said sensors; and vi. storing data from said sensors using said computer.

19 . The method of claim 18 , wherein the spectrophotometric inspection is performed inline with the fabrication of the inorganic solid electrolyte glass sheet, and/or subassembly, and/or electrode assembly.

20 . The method of claim 19 , wherein the spectrophotometric inspection comprises spectrophotometrically inspecting the first and/or second principal side surface of the inorganic solid electrolyte glass sheet at a first glass sheet inspection station, and conveying the glass sheet to a second inspection station for inspecting the interface between the glass sheet and a material layer on the first principal side surface of the glass sheet.

21 . A method of making a battery cell separator layer, the method comprising:
i) providing at least two precursor ingredients for making a Li ion conducting sulfide glass in a reaction vessel; ii) subjecting the precursor ingredients to a mechanical operation that mechanically induces a self-propagating reaction to form an amorphous solid powder; iii) heating the amorphous solid powder to a temperature sufficient to melt the amorphous powder; iv) cooling the melt to form a Li ion conducting sulfide glass.

22 . The method of claim 21 , wherein at least one precursor ingredient is not an amorphous material.

23 . The method of claim 21 , wherein at least one precursor ingredient is polycrystalline.

24 . The method of claim 21 , wherein the amorphous solid powder formed in operation iii) is a Li ion conducting sulfide glass.

25 . The method of claim 24 , wherein the Li ion conducting glass is processed to form a vitreous Li ion conducting sheet.

26 . The method of claim 25 , wherein the vitreous Li ion conducting glass sheet is combined with a lithium metal layer to form a lithium electrode assembly.

27 . The method of claim 26 , wherein the Li ion conducting sheet is subject to a compressive stress.

28 . The method of claim 27 , wherein the compressive stress is at least 10 MPa.

29 . A lithium electrode assembly comprising a vitreous Li ion conducting sulfide glass sheet and a lithium metal layer, wherein the sulfide glass sheet is subject to a compressive stress.

30 . The lithium electrode assembly of claim 29 , wherein the compressive stress is at least 10 MPa.

Assignees

• Polyplus Battery Co Inc

Inventors

• Visco Steven J
• Nimon Yevgeniy S
• De Jonghe Lutgard C
• Katz Bruce D
• Nimon Vitaliy

Classifications

• G01N2021/8967

  Discriminating defects on opposite sides or at different depths of sheet or rod · CPC title

• H01M4/1395

  of electrodes based on metals, Si or alloys · CPC title

• H01M2300/0068

  inorganic · CPC title

• G01N21/31

  Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry {(G01N21/72 takes precedence)} · CPC title

• H01M10/0566

  Liquid materials · CPC title