# US 2008/0187835 A1 · Non-aqueous electrolyte secondary battery, examination method and manufacturing method for negative electrode thereof, and examination apparatus and manufacturing apparatus for negative electrode thereof

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- Number: US 2008/0187835 A1
- Document ID: US20080187835A1
- Status: Published application
- Kind: A1
- Application number: 12/024,155
- Filed: 2008-02-01
- Published: 2008-08-07
- Earliest claimed: 2007-02-01
- Inventors: Hideharu TAKEZAWA; Takayuki Shirane; Shinya Fujimura; Sadayuki Okazaki; Kazuyoshi Honda
- Web page: https://patentgrep.com/patent/US20080187835A1

## CPC

- G01N 23/223: by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
- C23C 14/10: Glass or silica
- C23C 14/545: {using measurement on deposited material}
- C23C 14/562: {for coating elongated substrates}
- H01M 4/0421: {involving vapour deposition}
- H01M 4/1395: of electrodes based on metals, Si or alloys
- G01N 2223/076: X-ray fluorescence
- H01M 4/134: Electrodes based on metals, Si or alloys
- H01M 4/58: of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- Y02E 60/10: Energy storage using batteries
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A method for examining a negative electrode of a non-aqueous electrolyte secondary battery includes irradiating an active material layer including silicon or a silicon compound having a known composition, which is capable of electrochemically absorbing and releasing lithium ions on a current collector made of a metal including at least any one of copper, nickel, titanium and iron, with an X-ray; and measuring an attenuation amount of any one of a CuKα ray, a NiKα ray, a TiKα ray, and a FeKα ray, which is a fluorescent X-ray of the metal included in the current collector in fluorescent X-rays generated from the active material layer.

## Claims

### Claim 1

A method for examining a negative electrode of a non-aqueous electrolyte secondary battery, the method comprising:
irradiating an active material layer including silicon or a silicon compound having a known composition, which is capable of electrochemically absorbing and releasing lithium ions on a current collector made of a metal including at least any one of copper, nickel, titanium and iron, with an X-ray;
measuring an attenuation amount of any one of a CuKα ray, a NiKα ray, a TiKα ray, and a FeKα ray, which is a fluorescent X-ray of the metal included in the current collector in fluorescent X-rays generated from the active material layer in order to estimate a deposit amount of silicon or the silicon compound per unit area of the current collector.

### Claim 2 (depends on 1)

The method for examining a negative electrode of a non-aqueous electrolyte secondary battery according to claim 1, further comprising calculating the deposit amount of silicon or the silicon compound per unit area of the current collector from the measured attenuation amount.

### Claim 3

A method for manufacturing a negative electrode of a non-aqueous electrolyte secondary battery, the method comprising:
forming an active material layer made of silicon or a silicon compound having a known composition, which is capable of electrochemically absorbing and releasing lithium ions, on a current collector made of a metal including at least any one of copper, nickel, titanium and iron by a gas phase method using silicon;
irradiating the active material layer with an X-ray;
measuring an attenuation amount of any one of a CuKα ray, a NiKα ray, a TiKα ray, and a FeKα ray, which is a fluorescent X-ray of the metal included in the current collector in fluorescent X-rays generated from the active material layer; and
adjusting a condition for forming the active material layer so as to match the deposit amount of silicon or the silicon compound in the active material layer to a predetermined value based on the measured attenuation amount.

### Claim 4 (depends on 3)

The method for manufacturing a negative electrode of a non-aqueous electrolyte secondary battery according to claim 3, wherein when the deposit amount is matched to a predetermined amount, by controlling a generation rate of vapor of silicon, the deposit amount of silicon or the silicon compound in the active material layer is matched to the predetermined amount.

### Claim 5 (depends on 3)

The method for manufacturing a negative electrode of a non-aqueous electrolyte secondary battery according to claim 3,
wherein when an oxidation number of silicon is changed in the active material layer in a stepwise manner in a direction of deposition, an attenuation amount of any one of a CuKα ray, a NiKα ray, a TiKα ray, and a FeKα ray, which is measured in each step, is measured and a condition for forming the active material layer is adjusted in each step.

### Claim 6 (depends on 3)

A non-aqueous electrolyte secondary battery, comprising:
a negative electrode formed by the method for manufacturing a negative electrode of a non-aqueous electrolyte secondary battery according to claim 3;
a positive electrode facing the negative electrode; and
an electrolyte interposed between the negative electrode and the positive electrode.

### Claim 7

An apparatus for examining a negative electrode of a non-aqueous electrolyte secondary battery, comprising:
an X-ray generating section for irradiating an active material layer including silicon or a silicon compound having a known composition, which is capable of electrochemically absorbing and releasing lithium ions, on a current collector made of a metal including at least any one of copper, nickel, titanium and iron, with an X-ray; and
a measuring section for measuring an attenuation amount of any one of a CuKα ray, a NiKα ray, a TiKα ray, and a FeKα ray, which is a fluorescent X-ray of the metal included in the current collector in fluorescent X-rays generated from the active material layer in order to estimate a deposit amount of silicon or the silicon compound.

### Claim 8 (depends on 7)

The apparatus for examining a negative electrode of a non-aqueous electrolyte secondary battery according to claim 7, further comprising a calculation section for calculating the deposit amount of silicon or the silicon compound per unit area of the current collector from the attenuation amount measured in the calculation section.

### Claim 9

An apparatus for manufacturing a negative electrode of a non-aqueous electrolyte secondary battery, comprising:
a formation section for forming an active material layer made of silicon or a silicon compound having a known composition, which is capable of electrochemically absorbing and releasing lithium ions, on a surface of a current collector made of a metal including at least any one of copper, nickel, titanium and iron by a gas phase method using silicon;
an X-ray generating section for irradiating the active material layer with an X-ray;
a measuring section for measuring an attenuation amount of any one of a CuKα ray, a NiKα ray, a TiKα ray, and a FeKα ray, which is a fluorescent X-ray of the metal included in the current collector in fluorescent X-rays generated from the active material layer; and
a control section for adjusting the formation section so as to match the deposit amount of silicon or the silicon compound in the active material layer to a predetermined value based on the measured attenuation amount.

### Claim 10 (depends on 9)

The apparatus for manufacturing a negative electrode of a non-aqueous electrolyte secondary battery according to claim 9, wherein the control section controls a generation rate of vapor of silicon in the formation section, thereby matching the deposit amount of silicon or the silicon compound in the active material layer to a predetermined value.

### Claim 11 (depends on 9)

The apparatus for manufacturing a negative electrode of a non-aqueous electrolyte secondary battery according to claim 9,
wherein the formation section changes an oxidation number of silicon in the active material layer in a stepwise manner in a direction of deposition, and
the control section measures an attenuation amount of any one of a CuKα ray, a NiKα ray, a TiKα ray, and a FeKα ray, which is measured in each step, and adjusts a condition for forming the active material layer in each step.