# US 2013/0157145 A1 · Method for making solid electrolyte

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- Number: US 2013/0157145 A1
- Document ID: US20130157145A1
- Status: Published application
- Kind: A1
- Application number: 13/652,824
- Filed: 2012-10-16
- Published: 2013-06-20
- Earliest claimed: 2011-12-17
- Assignees: Tsinghua University; Hon Hai Precision Industry Co., Ltd.
- Inventors: LI WANG; XIANG-MING HE; JIAN-JUN LI; JIAN GAO; CHANG-YIN JIANG
- Web page: https://patentgrep.com/patent/US20130157145A1

## CPC

- C08F 2/48: by ultraviolet or visible light
- C08F 222/102: {of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate}
- C08F 299/024: {the unsaturation being in acrylic or methacrylic groups}
- C08F 220/286: {and containing polyethylene oxide in the alcohol moiety, e.g. methoxy polyethylene glycol (meth)acrylate}
- H01M 10/0565: Polymeric materials, e.g. gel-type or solid-type
- H01M 2300/0082: Organic polymers
- Y02E 60/10: Energy storage using batteries
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- 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 making a solid electrolyte includes the following steps. A first monomer, a second monomer, an initiator and a lithium salt are provided. Wherein the first monomer is R1—OCH2—CH2—OnR2, the second monomer is R3—OCH2—CH2—OmR4, each “R1”, “R2” and “R3” includes —C═C— group or —C≡C— group, “R4” is an alkyl group or a hydrogen (H), and “m” and “n” represents an integer number, molecular weights of the first and second monomers are greater than or equal to 100, and less than or equal to 800. The first and second monomers, the initiator and the lithium salt are mixed to form a mixture, and a weight ratio of the first monomer to the second monomer is less than or equal to 50%. The first and second monomers are polymerized to form an interpenetrating polymer network, and the lithium salt is transformed into a solid solution and dispersing in the interpenetrating polymer network.

## Claims

### Claim 1

A method for making a solid electrolyte, comprising:
providing a first monomer, a second monomer, an initiator, and a lithium salt; wherein the first monomer is R1—OCH2—Ch2—OnR2, the second monomer is R3—OCH2—CH2—OnR4, each “R1”, “R2” and “R3” comprises —C═C— group or —C≡C— group, “R4” is an alkyl group or a hydrogen (H), “m” and “n” respectively represents an integer number, and a molecular weight of the first monomer or a molecular weight of the second monomer is greater than or equal to 100, and less than or equal to 800;
mixing the first monomer, the second monomer, the initiator, and the lithium salt to form a mixture; wherein the first monomer is less than or equal to 50% of the second monomer by weight; and
polymerizing the first monomer with the second monomer to form an interpenetrating polymer network, and transforming the lithium salt into a solid solution and dispersing in the interpenetrating polymer network, thereby forming the solid electrolyte.

### Claim 2 (depends on 1)

The method of claim 1, wherein each “R1”, “R2” and “R3” comprises an unsaturated chain hydrocarbon group or an unsaturated chain hydrocarbon group with carbonyl.

### Claim 3 (depends on 2)

The method of claim 2, wherein each “R1”, “R2” and “R3” comprises ethenyl (—CH═CH2), ethynyl (—C≡CH), allyl (—CH═CH—CH3, or —(CH3)C═CH2), propinyl (—C≡C—CH3), or ethenyl ketonic group

### Claim 4 (depends on 1)

The method of claim 1, wherein the molecular weight of the first monomer or the molecular weight of the second monomer is greater than or equal to 200 and less than or equal to 600.

### Claim 5 (depends on 1)

The method of claim 1, wherein the lithium salt is selected from the group consisting of lithium perchlorate, lithium hexafluoro-phosphate, lithium tetrafluoro-borate, lithium bis(oxalate)-borate, lithium manganate, lithium iron phosphate, lithium nickelate, lithium cobalt oxide, and combinations thereof.

### Claim 6 (depends on 1)

The method of claim 1, wherein after the providing the first monomer, the second monomer, the initiator and the lithium salt;
providing a plasticizer; and
mixing the plasticizer with the first monomer, the second monomer, the initiator and the lithium salt to form the mixture.

### Claim 7 (depends on 6)

The method of claim 6, wherein the plasticizer is a multi-arm macromolecular material.

### Claim 8 (depends on 7)

The method of claim 7, wherein the multi-arm macromolecular material is a four-arm macromolecule material or a six-arm macromolecule material.

### Claim 9 (depends on 6)

The method of claim 6, wherein the providing the plasticizer comprises:
dropping a phloroglucionl-acetonitrile solution into phosphorus oxychloride to form a primary mixture;
stirring the primary mixture to obtain an intermediate solution;
dissolving methyl polyethylene glycol-400 into an acetonitrile to form a secondary mixture;
adding the secondary mixture into the intermediate solution; and
removing evaporated solution after about 48 hours, thereby obtaining a six-arm macromolecule material.

### Claim 10 (depends on 1)

The method of claim 1, wherein the initiator is a photo-initiator selected from the group consisting of 1-hydroxy-cyclohexyl phenyl ketone, 2-methyl-1-[4-(methylthio)-phenyl]-2-morpholino-propiopheno, and dimethylol propionic acid.

### Claim 11 (depends on 10)

The method of claim 10, wherein the polymerizing the first monomer with the second monomer to form the interpenetrating polymer network comprises a step of: putting the mixture into a protective gas, and using a UV light to irradiate the mixture for a period to polymerize the first monomer with the second monomer under the photo-initiator.

### Claim 12 (depends on 11)

The method of claim 11, wherein the protective gas is nitrogen gas, helium gas, neon gas, argon gas, krypton gas or xenon gas.

### Claim 13 (depends on 11)

The method of claim 11, wherein the period is in a range from about 30 minutes to about 2 hours.

### Claim 14 (depends on 11)

The method of claim 11, wherein the first monomer is polyethyleneglycol (200) dimethacrylate, the second monomer is methoxy polyethylene glycol (350) monoacrylate, and the photo-initiator is dimethylol propionic acid.

### Claim 15 (depends on 14)

The method of claim 14, wherein the mixing the first monomer, the second monomer, the initiator and the lithium salt to form the mixture comprises steps of mixing polyethyleneglycol (200) dimethacrylate with methoxy polyethylene glycol (350) monoacrylate with a predetermined ratio to form a middle mixture, and then adding lithium perchlorate and dimethylol propionic acid into the middle mixture.

### Claim 16 (depends on 1)

The method of claim 1, wherein the initiator is a thermo-initiator selected from the group consisting of chloride gas, bromine gas, organic peroxide, and azo initiator.

### Claim 17 (depends on 16)

The method of claim 16, wherein the step of polymerizing the first monomer with the second monomer to form the interpenetrating polymer network comprises steps of: putting the mixture into a protective gas; and heating the mixture at a temperature for a period, to polymerize the first monomer with the second monomer under the thermo-initiator, and transform the lithium salt into the solid solution.

### Claim 18 (depends on 17)

The method of claim 17, wherein the temperature ranges from about 40 centigrade degrees to about 80 centigrade degrees.

### Claim 19 (depends on 17)

The method of claim 17, wherein the period ranges from about 0.5 hours to about 24 hours.