Method of measuring quantity of moisture in electrode, method of manufacturing electrode for lithium-ion secondary battery, moisture quantity measuring apparatus, and method of measuring moisture quantity

Patent metadata

Field	Value
Publication number	US-2018136177-A1
Application number	US-201615735397-A
Country	US
Kind code	A1
Filing date	Jun 1, 2016
Priority date	Jun 12, 2015
Publication date	May 17, 2018
Grant date	—

Abstract

A method of measuring a quantity of moisture in an electrode includes at least three steps as follows: disposing an electrode, which is a measurement target sample, inside a container provided with a gas introduction pipe and a gas discharge pipe; heating the electrode by supplying inert gas heated to a predetermined temperature in advance to the inside of the container through the gas introduction pipe, and vaporizing moisture adsorbed to the electrode; and collecting the moisture vaporized from the electrode, together with the inert gas through the gas discharge pipe and determining the quantity of the collected moisture. In addition, a moisture quantity measuring apparatus includes a container that has a gas introduction pipe and a gas discharge pipe, a heating unit, and a moisture quantity measuring unit that collects moisture vaporized from a sample, through the gas discharge pipe and determines the quantity of collected moisture.

First claim

1 . A method of measuring a quantity of moisture in an electrode comprising:
a step of disposing an electrode, which is a measurement target sample, inside a container provided with a gas introduction pipe and a gas discharge pipe; a step of heating the electrode by supplying inert gas heated to a predetermined temperature in advance to the inside of the container through the gas introduction pipe, and vaporizing moisture adsorbed to the electrode; and a step of collecting the moisture vaporized from the electrode, together with the inert gas through the gas discharge pipe and determining the quantity of the collected moisture.

2 . The method of measuring a quantity of moisture in an electrode according to claim 1 ,
wherein the step of vaporizing moisture includes a step of heating the electrode by supplying first inert gas heated to a predetermined temperature in advance to the inside of the container through the gas introduction pipe, and vaporizing primary region water adsorbed to the electrode, and a step of further heating the electrode by supplying second inert gas heated to a temperature higher than the temperature of the first inert gas to the inside of the container through the gas introduction pipe, and vaporizing secondary region water adsorbed to the electrode after the step of vaporizing primary region water.

3 . The method of measuring a quantity of moisture in an electrode according to claim 2 ,
wherein the step of determining the quantity of moisture includes a step of determining the quantity of the primary region water and a step of determining the quantity of the secondary region water.

4 . The method of measuring a quantity of moisture in an electrode according to claim 2 ,
wherein in the step of vaporizing primary region water, the first inert gas is heated to a range from equal to or higher than 150° C. to equal to or lower than 220° C.

5 . The method of measuring a quantity of moisture in an electrode according to claim 2 ,
wherein in the step of vaporizing secondary region water, the second inert gas is heated to a range from equal to or higher than 250° C. to equal to or lower than 350° C.

6 . The method of measuring a quantity of moisture in an electrode according to claim 1 ,
wherein in the step of vaporizing moisture, (T 2 −T 1 ) ranges from equal to or higher than 0° C. to equal to or lower than 50° C. when the temperature of directly heating the container is T 1 [° C.] and the temperature of the inert gas is T 2 [° C.].

7 . The method of measuring a quantity of moisture in an electrode according to claim 1 ,
wherein in the step of determining the quantity of the collected moisture, the quantity of moisture is determined by a Karl Fischer's moisture quantity determination method.

8 . The method of measuring a quantity of moisture in an electrode according to claim 1 ,
wherein the inert gas includes one or more selected from nitrogen gas, helium gas, and argon gas.

9 . (canceled)

10 . A method of manufacturing an electrode for a lithium-ion secondary battery, comprising:
a step of producing an electrode including an electrode active material; and a step of measuring the quantity of moisture in the electrode by using the method of measuring a quantity of moisture in an electrode according to claim 1 .

11 . The method of manufacturing an electrode for a lithium-ion secondary battery according to claim 10 , further comprising:
a sorting step of sorting out an electrode appraised to be acceptable by appraising the quality of the electrode based on obtained information on the quantity of moisture in the electrode.

12 . The method of manufacturing an electrode for a lithium-ion secondary battery according to claim 11 ,
wherein in the sorting step, the quality of the electrode is appraised by comparing the obtained information on the quantity of moisture in the electrode with reference data indicating a relationship between the quantity of moisture in an electrode and electrode characteristics prepared in advance.

13 . A moisture quantity measuring apparatus comprising:
a container that has a gas introduction pipe and a gas discharge pipe and accommodates a measurement target sample; a heating unit that heats the measurement target sample by supplying inert gas heated to a predetermined temperature in advance to the inside of the container through the gas introduction pipe and vaporizes moisture adsorbed to the measurement target sample; and a moisture quantity measuring unit that collects the moisture vaporized from the measurement target sample, through the gas discharge pipe and determines the quantity of the collected moisture.

14 . The moisture quantity measuring apparatus according to claim 13 ,
wherein the heating unit includes a first heating unit which heats the measurement target sample by supplying first inert gas heated to a predetermined temperature in advance to the inside of the container through the gas introduction pipe and vaporizes primary region water adsorbed to the measurement target sample, and a second heating unit which further heats the measurement target sample by supplying second inert gas heated to a temperature higher than the temperature of the first inert gas to the inside of the container through the gas introduction pipe and vaporizes secondary region water adsorbed to the measurement target sample.

15 . (canceled)

16 . The moisture quantity measuring apparatus according to claim 13 ,
wherein the measurement target sample has a sheet-like shape.

17 . (canceled)

18 . A method of measuring a quantity of moisture in a measurement target sample using the moisture quantity measuring apparatus according to claim 13 , the method comprising:
a step of disposing a measurement target sample inside a container; a step of causing the heating unit to heat the measurement target sample by supplying inert gas heated to a predetermined temperature in advance to the inside of the container through the gas introduction pipe and to vaporize moisture adsorbed to the measurement target sample; and a step of collecting the moisture vaporized from the measurement target sample, together with the inert gas through the gas discharge pipe and causing the moisture quantity measuring unit to determine the quantity of the collected moisture.

19 . The method of measuring a moisture quantity according to claim 18 ,
wherein the step of vaporizing moisture includes a step of heating the measurement target sample by supplying first inert gas heated to a predetermined temperature in advance to the inside of the container through the gas introduction pipe, and vaporizing primary region water adsorbed to the measurement target sample, and a step of further heating the measurement target sample by supplying second inert gas heated to a temperature higher than the temperature of the first inert gas to the inside of the container through the gas introduction pipe, and vaporizing secondary region water adsorbed to the measurement target sample after the step of vaporizing primary region water.

20 . The method of measuring a moisture quantity according to claim 19 ,
wherein the step of determining the quantity of moisture includes a step of determining the quantity of the primary region water and a step of determining the quantity of the secondary region water.

21 . The method of measuring a moisture quantity according to claim 19 ,
wherein in the step of vaporizing primary region water, the first inert gas is heated to a

Assignees

• Nec Energy Devices Ltd

Inventors

• Fukatsu Kimiyoshi
• Hayashi Tomohiko

Classifications

• G01N2001/2241

  purpose-built sampling enclosure for emissions · CPC title

• G01N31/168 Primary

  Determining water content by using Karl Fischer reagent · CPC title

• H01M10/058

  Construction or manufacture · CPC title

• H01M4/1391

  of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx · CPC title

• H01M10/052

  Li-accumulators · CPC title