Device for analyzing film on surface of electrode for rechargeable lithium battery and method of analyzing film on surface of electrode for rechargeable lithium battery using same

Patent metadata

Field	Value
Publication number	US-9267904-B2
Application number	US-201213597229-A
Country	US
Kind code	B2
Filing date	Aug 28, 2012
Priority date	Apr 30, 2012
Publication date	Feb 23, 2016
Grant date	Feb 23, 2016

Abstract

A device for analyzing a film on a surface of an electrode for a rechargeable lithium battery includes: an inert chamber capable of maintaining an inert atmosphere including controlled amounts of moisture and oxygen and including an inner space for pretreating a sample including the film on the surface of the electrode; a first analyzer coupled to the inert chamber through a connection tube, the first analyzer being configured to receive the sample and being configured to provide composition and thickness information of the film; an inert holder configured to be assembled around the sample in the inert chamber and configured to maintain the inert atmosphere around the sample; and a second analyzer mounted with the inert holder therein and configured to provide shape information of the film. A method of analyzing a film on a surface of an electrode using the device is also disclosed.

First claim

What is claimed is:

1. A method of analyzing a film on a surface of an electrode for a rechargeable lithium battery comprising:
pretreating a sample comprising the film on the surface of the electrode in an inert chamber and controlling the amount of moisture and oxygen in an inert atmosphere in the inert chamber;
transporting the sample into a first analyzer to obtain composition and thickness information of the film in the first analyzer;
transporting the sample into the inert chamber and assembling an inert holder around the sample in the inert chamber;
ion etching the sample in the first analyzer before transporting the sample to the inert chamber; and
transporting the inert holder to a second analyzer to obtain shape information of the film in the second analyzer,
wherein the first analyzer is an X-ray Photoelectron Spectrometer (XPS),
wherein the second analyzer is a high resolution scanning electron microscope,
wherein an ion beam having a tilted angle relative to the surface of the sample is emitted during the ion etching,
wherein the ion beam has an accelerating voltage in a range of about 0.3 kV to about 0.5 kV and a current condition in a range of about 0.2 μA to about 0.5 μA, and
wherein the ion etching is performed until the electrode material under the film approaches about 50 to about 70 atom % based on the total amount of the electrode material prior to the ion etching.

2. The method of claim 1 , wherein the second analyzer emits an electron beam having an accelerating voltage in a range of about 0.5 kV to about 1.0 kV and a current condition in a range of about 1 pA to about 15 pA.

3. The method of claim 1 , wherein the pretreating the sample further comprises combining the sample with a supporting substrate or the inert holder.

4. The method of claim 1 , wherein the transporting the sample into the first analyzer comprises transporting the sample through a connection tube between the inert chamber and the first analyzer; and
wherein the inert atmosphere of the inert chamber and the connection tube has moisture in a range of 0 ppm to about 0.1 ppm and oxygen in a range of 0 ppm to about 0.5 ppm.

Assignees

• Lee Seon-Hong
• You Ho-Gon
• Song Joo-Han
• Jung In-Ho
• Kim Jake
• Samsung Sdi Co Ltd

Inventors

• Lee Seon-Hong
• You Ho-Gon
• Song Joo-Han
• Jung In-Ho
• Kim Jake

Classifications

• G01N23/2273 Primary

  Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS] · CPC title

• H01M10/42

  Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells (H01M10/60 takes precedence) · CPC title

• H01M4/13

  Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof · CPC title

• H01J37/28

  with scanning beams {(H01J37/268, H01J37/292, H01J37/2955 take precedence)} · CPC title

• H01M2004/021

  Physical characteristics, e.g. porosity, surface area · CPC title