CN109378474A - A kind of polyimide type lithium battery cathode pole piece and preparation method - Google Patents
A kind of polyimide type lithium battery cathode pole piece and preparation method Download PDFInfo
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- CN109378474A CN109378474A CN201811088524.5A CN201811088524A CN109378474A CN 109378474 A CN109378474 A CN 109378474A CN 201811088524 A CN201811088524 A CN 201811088524A CN 109378474 A CN109378474 A CN 109378474A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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Abstract
The invention discloses a kind of polyimide type lithium battery cathode pole pieces, including copper foil and negative electrode material binder, it is characterized in that, in terms of mass fraction, the negative electrode material binder includes following components: self-control polyimide resin: 18~22 parts, graphite powder: 20~60 parts, the invention also discloses the preparation methods of the self-control polyimide resin, and the preparation method of the polyimide type lithium battery cathode pole piece, lithium battery cathode pole piece is prepared through the invention, production cost can be substantially reduced, and the lithium battery cathode pole piece produced is heat-resisting, weatherability is preferable, development prospect is preferable.
Description
Technical field
The present invention relates to field of electronic device more particularly to a kind of polyimide type lithium battery cathode pole piece and preparation sides
Method.
Background technique
Lithium cell cathode material bonding agent (lithium cell cathode material bonding agent) is primarily referred to as with fire resistant polyimide
(PAI) there is good lithium cell cathode material bonding agent for one kind made of bonding agent, compared to traditional cathode of lithium battery
Material bond the features such as thermal expansivity and high heat resistance, thus is favored extensively with light, thin, compactness.With lithium electricity
It is portable that pond negative electrode material bonding agent made is widely used to mobile phone, digital camera, DV, laptop etc.
Electronic equipment and flat panel TV, business automation equipment, automotive electronics, instrument and meter, medical machinery, aerospace, military project
Equal fields.The fast development of the emerging markets such as smart electronics is benefited from, lithium cell cathode material bonding agent market will present obvious
Ascendant trend.
The lithium cell cathode material bonding agent of early stage mainly has SBR type product.Such product is by copper foil, butylbenzene
Rubber material composition.Such product is also known as lithium cell cathode material bonding agent (butadiene-styrene rubber negative electrode material).Butadiene-styrene rubber is negative
Adhesive used in the material of pole is mostly butadiene-styrene rubber and acrylate adhesive, and these two types of adhesive heat resistances are limited.With
The rapid development of electronics industry, electronic product miniaturises, lightweight and assembling densification, butadiene-styrene rubber cathode material
Material heat resistance, endurance, anti-flammability, dimensional stability, in terms of be not able to satisfy requirement, thus lithium electricity
Pond negative electrode material bonding agent gradually develops to type product.Lithium cell cathode material bonding agent has very high heat resistant requirements, tradition
The butadiene-styrene rubber or acrylate adhesive that lithium cell cathode material bonding agent uses are not able to satisfy the requirement.
Existing lithium cell cathode material bonding agent mainly using epoxy resin and nitrile rubber as flexibility adhesive, but
Be promoted lithium cell cathode material bonding agent it is flexible play the role of flexibility is rubber, but the TG point of rubber is very low, Wu Faqi
The shortcomings that heat resistance.
Summary of the invention
The purpose of the present invention is to provide a kind of polyimide type lithium battery cathode pole pieces, to solve traditional cathode of lithium battery
Pole piece heat resistance, weatherability be not strong, and lithium battery cathode pole piece conductive adhesive therewith sticks the low problem of agent glass transition temperature.
To solve the above-mentioned problems, the present invention provides a kind of polyimide type lithium battery cathode pole piece, including copper foil with
Negative electrode material binder, which is characterized in that in terms of mass fraction, the negative electrode material binder includes following components:
Self-control polyimide resin: 18~22 parts
Graphite powder: 20~60 parts.
As a preferred option, including copper foil and negative electrode material binder include following components in terms of mass fraction:
Self-control polyimide resin: 20 parts
Graphite powder: 40 parts.
As a preferred option, the self-control polyimide resin preparation method is as follows
It (1) will [4- (4- amino-benzene oxygen) phenyl] propane (BAPP) bis- without glue mother liquor, p-phenylenediamine (PPDA), 2,2-
And dimethyl acetamide (DMAC) is added in reaction kettle and mixes to dissolution；In terms of mass fraction, the no glue mother liquor
Number is 80~90 parts, and the number of the p-phenylenediamine is 10~20 parts, and 2, the 2- is bis- [4- (4- amino-benzene oxygen) phenyl]
The number of propane is 3~5 parts, and the number of the dimethyl acetamide is 250~270 parts, keeps recirculated water inside reaction kettle
Temperature reserves 1-2 kilograms of amount at 50 DEG C or so, and when dimethyl acetamide is added, for by reaction kettle inner wall remnants'
Raw material pours reaction kettle, after solution is thoroughly mixed, is stirred 60 minutes with the frequency of 25Hz, with iron bale-out bottom solution, sees
Whether have particle or aggregate undissolved, terminate to stir if without if if examining, stirs to being completely dissolved；
(2) it is slowly added to 15 parts of benzophenone tetracid dianhydride (BTDA), continues agitating solution, and in benzophenone tetracid dianhydride
5 parts of dimethyl acetamide is added after addition and rinses reaction kettle inner wall, with the frequency agitating solution of 28Hz 60 minutes after mixing；
(3) BPDA (2,3,3 ', 4 '-bibenzene tetracarboxylic dianhydride) is added into mixed solution for the first time, the amount of addition is total amount
1/4 (total amount be 133.3 parts), when addition Huan Man on one side cool down while uniformly to feed, circulating water temperature in control reaction kettle
5 parts of dimethyl acetamide is added lower than 32 DEG C, after mixing and rinses reaction kettle inner wall, is stirred to react later with the frequency of 30Hz
Kettle internal liquid 30 minutes；
Repeat the above steps (3) operation 2 times, i.e., adds the BPDA of 3/4 total amount altogether, continue to stir later, with
3.5 parts of octadecylamines are added after stirring 1 hour in the frequency of 30Hz, continue stirring 30 minutes；
(4) BPDA (33.3 parts) of remaining 1/4 total amount is added into solution, is added within (about 60 minutes) after stirring sufficiently
14 parts of dimethyl acetamide pours the Residual reactants of reaction kettle inner wall in solution, and discharge is sub- up to self-control polyamides after stirring
Polyimide resin.
As a preferred option, when BPDA is added every time, the viscosity of real-time detection mixed solution is all needed, if viscosity is
3000~7000cp then needs to slow down the addition speed of BPDA, until viscosity is 7000~15000cp, that is, stops being added
BPDA。
Prepare a kind of method of polyimide type lithium battery cathode pole piece described in claim, comprising the following steps:
(1) polyimide resin is dissolved with n,N-Dimethylformamide, polyimide solution is made；
(2) polyimide solution, graphite powder are sequentially added according to the proportion, and negative electrode material adhesive is obtained after stirring；
(3) negative electrode material adhesive made from step (2) is applied on copper foil, after drying, crosslinking, is put into baking oven
Solidify to get polyimides lithium battery cathode pole piece is arrived.
As a preferred option, in the step (2), the time of stirring is 2 hours.
As a preferred option, in the step (2), the solid content of negative electrode material adhesive is 60%.
As a preferred option, in the step (3), the negative electrode material adhesive with a thickness of 100 microns.
As a preferred option, in the step (3), the temperature of the baking oven is 180 DEG C, and curing time is 8 hours.
The technical solution has technical effect beneficial below:
(1) to make resin based on polyimides by oneself, cooperate conductive base graphite powder, be prepared for high-performance conductive gluing
Agent, the glass transition temperature of adhesive can reach 180 DEG C, with the adhesive prepare lithium cell cathode material bonding agent,
It is horizontal that heat resistance can reach lithium cell cathode material bonding agent.
(2) polyimides adhesive can be used for rubbing method and prepare lithium cell cathode material bonding agent, thus greatly reduce
Equipment and the cost of raw material, prepared lithium cell cathode material bonding agent have excellent heat resistance, flame retardant property, resistance to ion
Migration performance, weather resistance etc..
(3) PAI lithium cell cathode material bonding agent will gradually replace butadiene-styrene rubber negative electrode material, to ensure that wiring board has
More brilliant heat resistance and long-time service reliability.In terms of PAI lithium cell cathode material bonding agent manufacturing process, apply
Cloth method also will gradually replace high-temperature high-pressure legal, to reduce production cost.Thus, the exploitation of High-performance adhesive is most important, glue
Glutinous agent determines the development prospect of the following rubbing method lithium cell cathode material bonding agent.
Detailed description of the invention
Fig. 1 is the DMA curve of 3 adhesive of the embodiment of the present invention, PI composite membrane；
Fig. 2 is that the resistance to Ion transfer of the embodiment of the present invention 3 tests comb type circuit used；
Fig. 3 is 3FCCL of the embodiment of the present invention test curve of resistance to Ion transfer；
Fig. 4 is FCCL peel strength after the 3 different disposal time of the embodiment of the present invention；
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment provided below is not intended to limit the invention covered range, and described step is also not use
Sequence is executed to limit its.Those skilled in the art combine existing common knowledge to do conspicuous improvement to the present invention, also fall
Enter the present invention claims protection scope within.
Embodiment one
A kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, in terms of mass fraction, institute
The negative electrode material binder stated includes following components:
Self-control polyimide resin: 20 parts
Graphite powder: 20 parts
The polyimide type lithium battery cathode pole piece the preparation method is as follows:
(1) polyimide resin is dissolved with n,N-Dimethylformamide, polyimide solution is made；
(2) polyimide solution, graphite powder are sequentially added according to the proportion, and negative electrode material adhesive is obtained after stirring；
(3) negative electrode material adhesive made from step (2) is applied on copper foil, drying, it is partial cross-linked after, be put into
Solidify 8 hours in 180 DEG C of baking ovens to get the polyimides lithium battery cathode pole piece for arriving high Tg point.
Embodiment two
A kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, in terms of mass fraction, institute
The negative electrode material binder stated includes following components:
Self-control polyimide resin: 20 parts
Graphite powder: 30 parts
Preparation method is the same as embodiment one；
Embodiment three
A kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, in terms of mass fraction, institute
The negative electrode material binder stated includes following components:
Self-control polyimide resin: 20 parts
Graphite powder: 40 parts
Preparation method is the same as embodiment one；
Example IV
A kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, in terms of mass fraction, institute
The negative electrode material binder stated includes following components:
Self-control polyimide resin: 20 parts
Graphite powder: 50 parts
Preparation method is the same as embodiment one；
Embodiment five
A kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, in terms of mass fraction, institute
The negative electrode material binder stated includes following components:
Self-control polyimide resin: 20 parts
Graphite powder: 60 parts
Preparation method is the same as embodiment one；
Comparative example one
A kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, in terms of mass fraction, institute
The negative electrode material binder stated includes following components:
Self-control polyimide resin: 20 parts
Graphite powder: 10 parts
Preparation method is the same as embodiment one；
Comparative example two
A kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, in terms of mass fraction, institute
The negative electrode material binder stated includes following components:
Self-control polyimide resin: 20 parts
Graphite powder: 70 parts
Preparation method is the same as embodiment one；
All-round property testing is carried out to embodiment 1-5, comparative example 1,2, test method, standard are as follows:
Glass transition temperature: being tested using dynamics thermal analyzer (DMA 2980, TA company of the U.S.), using poly-
Acid imide and adhesive laminated film rise to 400 DEG C from room temperature with the heating rate of 10 DEG C/min, in dielectric dissipation factor (tan
The glass transition temperature of sample is found out at maximum value δ).
Peel strength (PS): it is tested by IPC-TM-650 2.4.9.
The test of resistance to Ion transfer: according to IPC-TM-650 2.6.14.1 test lithium cell cathode material bonding agent it is resistance to from
Sub- migration performance, line width/line-spacing of lithium cell cathode material bonding agent are 50 μm/50 μm, and test environment temperature is 85 DEG C, humidity
For 85%RH.
Flame retardant test: according to the flame retardant property of UL94 standard testing lithium cell cathode material bonding agent.
Table one: the physical property intensity of embodiment 1-5 and comparative example 1,2
As can be seen from Table 1, the specific gravity for adding conducting powder work stone ink powder (c), has a direct impact material property.Originally it is grinding
Study carefully in work, we select the formula to prepare lithium cell cathode material bonding agent, and carry out the property of related lithium battery cathode pole piece
It can test.
Adhesive heat resistance research
We test the glass transition temperature of adhesive, test curve such as Fig. 1 by dynamic thermomechanical analysis (DMA)
It is shown.The corresponding temperature of the peak value of dielectric dissipation factor (tan δ) distinguishes 180 DEG C and 333 DEG C, they are respectively PAI adhesive
The glass transition temperature of glass transition temperature and copper foil or copper sheet.The glass transition temperature of PAI adhesive is significantly larger than
Epoxy resin adhesive used in butadiene-styrene rubber negative electrode material and acrylate adhesive (< 100 DEG C).
Glass transition temperature is temperature of the high polymer by glassy transition for elastomeric state, and glass transition temperature is high poly-
One important parameter of physical change occurs for object, main related to the structure of high polymer, coherent condition, crosslink density etc..Gluing
The glass transition temperature of agent can reflect the heat resistance of adhesive to a certain extent, and lithium cell cathode material is bonded
The glass transition temperature of agent, adhesive is higher, and the heat resistance and reliability of product are higher.What this research work was developed
PAI adhesive is due to can be used for preparing lithium cell cathode material bonding agent with very high glass transition temperature.
The resistance to Ion transfer performance research of lithium cell cathode material bonding agent
The insulating reliability of lithium cell cathode material bonding agent is usually evaluated with resistance to Ion transfer performance.In this research work
In work, we test the resistance to Ion transfer performance of lithium cell cathode material bonding agent, lithium electricity using comb type circuit shown in Fig. 2
Line width/line-spacing of pond negative electrode material bonding agent is 50 μm/50 μm, and power parameter is DC 12V.Sample is placed into perseverance by access
(temperature is 85 DEG C, humidity 85%RH), the resistance of sample, acquired results such as Fig. 3 institute when testing different time in constant temperature and humidity case
Show.
From figure 3, it can be seen that lithium cell cathode material bonding agent shows excellent resistance to Ion transfer performance, show its tool
There is very high insulating reliability.The superiority and inferiority of the resistance to Ion transfer performance of lithium cell cathode material bonding agent depends primarily on insulating layer,
The especially resistance to Ion transfer performance of adhesive.In this work, the matrix resin of our adhesives used is polyimides tree
Rouge, this is entirely different with epoxide-resin glue system used in traditional lithium cell cathode material bonding agent, polyimides heat-proof aging,
Humidity resistance, reliability, electrical insulation capability etc. are all substantially better than epoxy resin, this causes PAI lithium cell cathode material viscous
The resistance to Ion transfer performance of agent is connect better than traditional butadiene-styrene rubber negative electrode material.
Lithium cell cathode material bonding agent Research on Weatherability
For the weather resistance for assessing lithium cell cathode material bonding agent, we test lithium cell cathode material bonding agent warp
" peel strength after double 85 " environmental treatments (temperature: 85 DEG C, humidity: 85%RH), test results are shown in figure 4.Before untreated,
The peel strength of lithium cell cathode material bonding agent is 1.28kgf/cm.After 240h is handled, peel strength is declined, but still
It is so maintained at higher horizontal (1.06kgf/cm), meets the requirement of lithium cell cathode material bonding agent.Weatherability test
The result shows that the adhesive of resin has good heat and moisture aging resistance based on polyimides, it is negative to can be used for PAI lithium battery
The preparation of pole material bond.
Lithium cell cathode material bonding agent Study of flame retardancy
Lithium cell cathode material bonding agent for wiring board need to have good flame retardant property.We pass through vertical combustion
Experiment tests the flame retardant property of lithium cell cathode material bonding agent.In test process, flame out time is less than 1s, can determine that
The flame retardant rating of lithium cell cathode material bonding agent reaches UL94-V-0.The outstanding flame retardant property of lithium cell cathode material bonding agent
It is closely related with PAI resin (limit oxygen index 47%), reactive phosphorus flame retardant (DOPO, SPH-100) in adhesive
The flame retardant property that then can be further improved lithium cell cathode material bonding agent is added.
2 lithium cell cathode material bonding agent comprehensive performance of table
As shown in Table 2, every comprehensive performance of the lithium cell cathode material binder prepared through the invention reach compared with
For outstanding index, therefore can also have more by the lithium battery cathode pole piece that the negative electrode material binder is prepared in conjunction with copper foil
Excellent performance, while cost is relatively low for cathode pole piece prepared by the present invention, commercial value with higher.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.To these embodiments
A variety of modifications will be readily apparent to those skilled in the art, the general principles defined herein can be with
Without departing from the spirit or scope of the present invention, it realizes in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to widest model consistent with the principles and novel features disclosed in this article
It encloses.
Claims (10)
1. a kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, which is characterized in that with quality
Number meter, the negative electrode material binder include following components:
Self-control polyimide resin: 18~22 parts；
Graphite powder: 20~60 parts.
2. a kind of polyimide type lithium battery cathode pole piece, including copper foil and negative electrode material binder, which is characterized in that with quality
Number meter includes following components:
Self-control polyimide resin: 20 parts；
Graphite powder: 40 parts.
3. a kind of polyimide type lithium battery cathode pole piece according to claim 1, which is characterized in that the self-control polyamides
Imide resin the preparation method is as follows:
(1) [4- (4- amino-benzene oxygen) phenyl] propane bis- without glue mother liquor, p-phenylenediamine, 2,2- and dimethyl acetamide are added
Enter and mixes to dissolution in reaction kettle；In terms of mass fraction, the number of the no glue mother liquor is 80~90 parts, described to benzene two
The number of amine is 10~20 parts, and the numbers of bis- [4- (4- amino-benzene oxygen) phenyl] propane of 2,2- is 3~5 parts, described two
The number of methylacetamide is 250~270 parts；
(2) it is slowly added to 15 parts of benzophenone tetracid dianhydride, continues agitating solution；
(3) 100 parts of 2,3,3 ', 4 '-bibenzene tetracarboxylic dianhydrides are added into solution by several times, and assist agitating solution, to solution
3.5 parts of octadecylamine is added after being sufficiently mixed, continues agitating solution；
(4) 33.3 parts of 2,3,3 ', 4 '-bibenzene tetracarboxylic dianhydrides are added into solution, 14 parts of diformazan is added after stirring sufficiently
Yl acetamide pours the Residual reactants of reaction kettle inner wall in solution, and discharge makes polyimide resin by oneself to obtain the final product after stirring.
4. a kind of polyimide type lithium battery cathode pole piece according to claim 3, which is characterized in that in the step (1),
Reaction temperature is 50 DEG C, and in the step (2) to the step (4), reaction temperature is 28~32 DEG C.
5. a kind of polyimide type lithium battery cathode pole piece according to claim 3, which is characterized in that in the step (3),
The number that 2,3,3 ', 4 '-bibenzene tetracarboxylic dianhydrides are added is 3 times, and the amount being added every time is equal, is 33.3 parts, and
5 parts of dimethylacetamide solution cleaning reaction kettle inner wall is all added after 2,3,3 ', 4 '-bibenzene tetracarboxylic dianhydrides of addition every time.
6. preparing a kind of described in any item polyimide type lithium battery cathode pole pieces of claim 1-5, which is characterized in that including
Following steps:
(1) polyimide resin is dissolved with n,N-Dimethylformamide, polyimide solution is made；
(2) polyimide solution, graphite powder are sequentially added according to the proportion, and negative electrode material adhesive is obtained after stirring；
(3) negative electrode material adhesive made from step (2) is applied on copper foil, after drying, crosslinking, is put into baking oven solid
Change to get polyimides lithium battery cathode pole piece is arrived.
7. a kind of preparation method of polyimide type lithium battery cathode pole piece according to claim 6, which is characterized in that described
In step (2), the time of stirring is 2 hours.
8. a kind of preparation method of polyimide type lithium battery cathode pole piece according to claim 6, which is characterized in that described
In step (2), the solid content of negative electrode material adhesive is 60%.
9. a kind of preparation method of polyimide type lithium battery cathode pole piece according to claim 6, which is characterized in that described
In step (3), the negative electrode material adhesive of coating is with a thickness of 100 microns.
10. a kind of preparation method of polyimide type lithium battery cathode pole piece according to claim 6, which is characterized in that institute
It states in step (3), the temperature of baking oven is 180 DEG C, and curing time is 8 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114672272A (en) * | 2022-03-11 | 2022-06-28 | 江苏环峰电工材料有限公司 | Preparation process and application of polyimide-based conductive adhesive |
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Application publication date: 20190222 |