CN106486651A - A kind of lithium ion battery negative material of high safety performance and preparation method thereof - Google Patents
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The invention discloses a kind of lithium ion battery negative material of high safety performance and preparation method thereof, the lithium ion battery negative material of high safety performance includes Colophonium, silica flour, graphite, lithium metaaluminate, Colophonium, LA132 binding agent, CMC binding agent and conductive agent according to the raw material of weight portion.The nano-silicon that the present invention adopts has the features such as specific surface area is big, ion the evolving path is short, wriggling is strong and plasticity is high, the bulk effect of alloy type material can be suppressed to a certain extent, and improve its chemical property using to carry out mechanical ball milling mix this modified technique to graphite surface, the first coulombic efficiency of material not only can be greatly improved, extend the cycle life of electrode, the evolving path in graphite linings for the lithium ion can also be shortened, improve the high rate capability of electrode material；Improve the conduction velocity of lithium ion battery, the dendrite reducing lithium ion battery analysis lithium generation punctures the probability of barrier film, reduces battery short circuit probability, improves the security performance of battery.
Description
Technical field
The present invention relates to lithium ion battery preparing technical field, specifically a kind of lithium ion battery of high safety performance
Negative material and preparation method thereof.
Background technology
Extensive application with various portable electric appts and electric automobile and fast development, people are to all kinds of electricity
The demand of product power supply and performance requirement also more and more higher, lithium rechargeable battery is superior with its high power characteristic etc.
Combination property in success nearly ten years and be widely used in mobile electronic terminal device field.
At present the negative material of lithium ion battery adopts graphite, and in order to improve battery capacity, or improve battery
Cryogenic property, all do various researchs in the study on the modification to graphite cathode material or attempt, such as using cladding
Graphite method, graphite expand layer etc. although these techniques can have some aspects to improve negative material performance, but total coming
Say, because its technological process is complicated, hardly possible controls, need to use all kinds of materials including catalyst, cost is very
Height is it is impossible to adapt to produce, thus actual production can not be fully converted to.
The security and stability of battery causes battery short circuit to cause battery mainly due to the thermal runaway of lithium ion battery
Catch fire, explode and cause.The following aspects is mainly passed through in the safety improving battery at present：Optimize electrolysis
Formula of liquid, using the lithium ion positive and negative pole material of ceramic diaphragm, offer safety；But these methods are electric to improving
The security performance in pond is limited.
Content of the invention
It is an object of the invention to provide a kind of lithium ion battery of high temperature resistant, good insulation preformance high safety performance
Negative material and preparation method thereof, to solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme：
A kind of lithium ion battery negative material of high safety performance, the raw material according to weight portion includes：Colophonium 2-10
Part, silica flour 5-30 part, graphite 60-80 part, lithium metaaluminate 10-20 part, Colophonium 2-10 part, LA132 glue
Knot agent 1-2 part, CMC binding agent 0.5-1 part, conductive agent 0.1-0.2 part.
As the further scheme of the present invention：The lithium ion battery negative material of described high safety performance, according to weight
The raw material of amount part includes：Silica flour 10-25 part, graphite 65-75 part, lithium metaaluminate 12-18 part, Colophonium 4-8
Part, LA132 binding agent 1.2-1.8 part, CMC binding agent 0.6-0.8 part, conductive agent 0.12-0.18 part.
As the further scheme of the present invention：The lithium ion battery negative material of described high safety performance, according to weight
The raw material of amount part includes：20 parts of silica flour, 70 parts of graphite, 15 parts of lithium metaaluminate, 6 parts of Colophonium, LA132
1.5 parts of binding agent, 0.7 part of CMC binding agent, 0.15 part of conductive agent.
As the further scheme of the present invention：The granularity of described silica flour is 50-500nm.
As the further scheme of the present invention：The granularity of described graphite is 7-22um.
The preparation method of the lithium ion battery negative material of described high safety performance, comprises the following steps that：
(1) weigh each raw material according to weight portion；
(2) silica flour and graphite are carried out mixing after mechanical ball milling 2-8h, the rotating speed of mechanical ball milling mixing is
1000-4000rpm, and it is dried 10-15h under vacuum, drying temperature is 50-180 DEG C；
(3) Colophonium is dissolved in solvent, solution temperature is 40-190 DEG C, stirring frequency is 10-40Hz,
Mixing time is 4-8h；
(4) it is added to the molten of step (3) after the silica flour that step (2) is obtained and the mixture cooling of graphite
Coated in liquid, temperature of plate is 40-190 DEG C, stirring frequency is 10-40Hz, the cladding time is 4-8h；
(5) sucking filtration removes solvent and is vacuum dried 5-18h, then under the protection of noble gases, with 1-5 DEG C
The programming rate of/min is warmed up to 420-650 DEG C, constant temperature 3-8h, then with the programming rate of 2.5-4 DEG C/min
It is warmed up to 950-1150 DEG C, constant temperature 5-8h, finally naturally cool to room temperature and obtain cathode pole piece；
(6) lithium metaaluminate, LA132 binding agent, CMC binding agent and conductive agent are mixed, and secondary
Distilled water is configured to the lithium metaaluminate slurry that concentration is 1-30%；
(7) the cathode pole piece surface-coated that above-mentioned slurry is obtained in step (5) using ultrasonic spraying process, its
Coating thickness is 1-10 μm；
(8) by the cathode pole piece after above-mentioned surface-coated under the conditions of temperature is for 50-70 DEG C, toast 0.5-2h,
It is dried to obtain finished product.
As the further scheme of the present invention：Described solvent is toluene, quinoline, carbon tetrachloride, petroleum ether, molten
One of agent gasoline, methanol, ethanol, isopropanol, acetoneand ethyl acetate or two or more.
As the present invention further scheme：Described noble gases are nitrogen, argon, helium, neon and xenon
One of gas or two or more.
Compared with prior art, the invention has the beneficial effects as follows：
The nano-silicon that the present invention adopts has that specific surface area is big, ion the evolving path is short, wriggling strong and plasticity
High the features such as, the bulk effect of alloy type material can be suppressed to a certain extent, and improve its chemical property
Using to carrying out the mechanical ball milling this modified technique to graphite surface of mixing, material not only can be greatly improved
Coulombic efficiency first, extends the cycle life of electrode additionally it is possible to shorten the evolving path in graphite linings for the lithium ion,
Improve the high rate capability of electrode material；Improve the conduction velocity of lithium ion battery, reduce lithium ion battery
The dendrite that analysis lithium produces punctures the probability of barrier film, reduces battery short circuit probability, improves the security performance of battery.
Specific embodiment
With reference to specific embodiment, the technical scheme of this patent is described in more detail.
Embodiment 1
A kind of lithium ion battery negative material of high safety performance, the raw material according to weight portion includes：Colophonium 2
Part, granularity be 5 parts of the silica flour of 50nm, granularity be 60 parts of the graphite of 7um, 10 parts of lithium metaaluminate, Colophonium
2 parts, 1 part of LA132 binding agent, 0.5 part of CMC binding agent, 0.1 part of conductive agent.
The preparation method of the lithium ion battery negative material of described high safety performance, comprises the following steps that：
(1) weigh each raw material according to weight portion；
(2) silica flour and graphite are carried out mixing after mechanical ball milling 2h, the rotating speed of mechanical ball milling mixing is 1000rpm,
And it is dried 10h under vacuum, drying temperature is 50 DEG C；
(3) Colophonium is dissolved in toluene, solution temperature is 40 DEG C, stirring frequency is 10Hz, during stirring
Between be 4h；
(4) it is added to the molten of step (3) after the silica flour that step (2) is obtained and the mixture cooling of graphite
Coated in liquid, temperature of plate is 40 DEG C, stirring frequency is 10Hz, the cladding time is 4h；
(5) sucking filtration removes toluene and is vacuum dried 5h, then under the protection of nitrogen, with the liter of 1 DEG C/min
Warm speed is warmed up to 420 DEG C, constant temperature 3h, is then warmed up to 950 DEG C with the programming rate of 2.5 DEG C/min, permanent
Warm 5h, finally naturally cools to room temperature and obtains cathode pole piece；
(6) lithium metaaluminate, LA132 binding agent, CMC binding agent and conductive agent are mixed, and secondary
Distilled water is configured to the lithium metaaluminate slurry that concentration is 2%；
(7) the cathode pole piece surface-coated that above-mentioned slurry is obtained in step (5) using ultrasonic spraying process, its
Coating thickness is 1 μm；
(8) by the cathode pole piece after above-mentioned surface-coated under the conditions of temperature is 50 DEG C, toast 0.5h, be dried
Obtain finished product.
Embodiment 2
A kind of lithium ion battery negative material of high safety performance, the raw material according to weight portion includes：Granularity is
10 parts of the silica flour of 10nm, granularity are 65 parts of the graphite of 10um, 12 parts of lithium metaaluminate, 4 parts of Colophonium, LA132
1.2 parts of binding agent, 0.6 part of CMC binding agent, 0.12 part of conductive agent.
The preparation method of the lithium ion battery negative material of described high safety performance, comprises the following steps that：
(1) weigh each raw material according to weight portion；
(2) silica flour and graphite are carried out mixing after mechanical ball milling 3h, the rotating speed of mechanical ball milling mixing is 1500rpm,
And it is dried 11h under vacuum, drying temperature is 80 DEG C；
(3) Colophonium is dissolved in quinoline, solution temperature is 100 DEG C, stirring frequency is 18Hz, during stirring
Between be 5h；
(4) it is added to the molten of step (3) after the silica flour that step (2) is obtained and the mixture cooling of graphite
Coated in liquid, temperature of plate is 100 DEG C, stirring frequency is 18Hz, the cladding time is 5h；
(5) sucking filtration removes quino vacuum drying 8h, then under the protection of argon, with the liter of 2 DEG C/min
Warm speed is warmed up to 450 DEG C, and then constant temperature 4h is warmed up to 1000 DEG C with the programming rate of 3 DEG C/min, constant temperature
5.5h, finally naturally cools to room temperature and obtains cathode pole piece；
(6) lithium metaaluminate, LA132 binding agent, CMC binding agent and conductive agent are mixed, and secondary
Distilled water is configured to the lithium metaaluminate slurry that concentration is 10%；
(7) the cathode pole piece surface-coated that above-mentioned slurry is obtained in step (5) using ultrasonic spraying process, its
Coating thickness is 3 μm；
(8) by the cathode pole piece after above-mentioned surface-coated under the conditions of temperature is 55 DEG C, toast 0.8h, be dried
Obtain finished product.
Embodiment 3
A kind of lithium ion battery negative material of high safety performance, the raw material according to weight portion includes：Granularity is
20 parts of the silica flour of 280nm, granularity are 70 parts of the graphite of 15m, 15 parts of lithium metaaluminate, 6 parts of Colophonium, LA132
1.5 parts of binding agent, 0.7 part of CMC binding agent, 0.15 part of conductive agent.
The preparation method of the lithium ion battery negative material of described high safety performance, comprises the following steps that：
(1) weigh each raw material according to weight portion；
(2) silica flour and graphite are carried out mixing after mechanical ball milling 5h, the rotating speed of mechanical ball milling mixing is 2000rpm,
And it is dried 13h under vacuum, drying temperature is 120 DEG C；
(3) Colophonium is dissolved in carbon tetrachloride, solution temperature is 100 DEG C, stirring frequency is 25Hz, stirs
Time of mixing is 6h；
(4) it is added to the molten of step (3) after the silica flour that step (2) is obtained and the mixture cooling of graphite
Coated in liquid, temperature of plate is 100 DEG C, stirring frequency is 25Hz, the cladding time is 6h；
(5) sucking filtration removes carbon tetrachloride and is vacuum dried 12h, then under the protection of helium, with 3 DEG C/min
Programming rate be warmed up to 550 DEG C, constant temperature 6h, be then warmed up to 1050 DEG C with the programming rate of 3.2 DEG C/min,
Constant temperature 7h, finally naturally cools to room temperature and obtains cathode pole piece；
(6) lithium metaaluminate, LA132 binding agent, CMC binding agent and conductive agent are mixed, and secondary
Distilled water is configured to the lithium metaaluminate slurry that concentration is 15%；
(7) the cathode pole piece surface-coated that above-mentioned slurry is obtained in step (5) using ultrasonic spraying process, its
Coating thickness is 5 μm；
(8) by the cathode pole piece after above-mentioned surface-coated under the conditions of temperature is 60 DEG C, toast 1.5h, be dried
Obtain finished product.
Embodiment 4
A kind of lithium ion battery negative material of high safety performance, the raw material according to weight portion includes：Granularity is
25 parts of the silica flour of 450nm, granularity are 75 parts of the graphite of 20um, 18 parts of lithium metaaluminate, 8 parts of Colophonium,
1.8 parts of LA132 binding agent, 0.8 part of CMC binding agent, 0.18 part of conductive agent.
The preparation method of the lithium ion battery negative material of described high safety performance, comprises the following steps that：
(1) weigh each raw material according to weight portion；
(2) silica flour and graphite are carried out mixing after mechanical ball milling 7h, the rotating speed of mechanical ball milling mixing is 3500rpm,
And it is dried 14h under vacuum, drying temperature is 150 DEG C；
(3) Colophonium is dissolved in petroleum ether, solution temperature is 150 DEG C, stirring frequency is 30Hz, stirring
Time is 7h；
(4) it is added to the molten of step (3) after the silica flour that step (2) is obtained and the mixture cooling of graphite
Coated in liquid, temperature of plate is 150 DEG C, stirring frequency is 30Hz, the cladding time is 7h；
(5) sucking filtration removes petroleum ether and is vacuum dried 15h, then under the protection of neon, with 4.5 DEG C/min
Programming rate be warmed up to 600 DEG C, constant temperature 7h, be then warmed up to 1100 DEG C with the programming rate of 4.5 DEG C/min,
Constant temperature 7h, finally naturally cools to room temperature and obtains cathode pole piece；
(6) lithium metaaluminate, LA132 binding agent, CMC binding agent and conductive agent are mixed, and secondary
Distilled water is configured to the lithium metaaluminate slurry that concentration is 25%；
(7) the cathode pole piece surface-coated that above-mentioned slurry is obtained in step (5) using ultrasonic spraying process, its
Coating thickness is 8 μm；
(8) by the cathode pole piece after above-mentioned surface-coated under the conditions of temperature is 65 DEG C, toast 1.8h, be dried
Obtain finished product.
Embodiment 5
A kind of lithium ion battery negative material of high safety performance, the raw material according to weight portion includes：Granularity is
10 parts of the Colophonium of 500nm, granularity are 30 parts of the silica flour of 22um, 80 parts of graphite, 20 parts of lithium metaaluminate,
10 parts of Colophonium, 2 parts of LA132 binding agent, 1 part of CMC binding agent, 0.2 part of conductive agent.
The preparation method of the lithium ion battery negative material of described high safety performance, comprises the following steps that：
(1) weigh each raw material according to weight portion；
(2) silica flour and graphite are carried out mixing after mechanical ball milling 8h, the rotating speed of mechanical ball milling mixing is 4000rpm,
And it is dried 15h under vacuum, drying temperature is 180 DEG C；
(3) Colophonium is dissolved in methanol, solution temperature is 190 DEG C, stirring frequency is 40Hz, during stirring
Between be 8h；
(4) it is added to the molten of step (3) after the silica flour that step (2) is obtained and the mixture cooling of graphite
Coated in liquid, temperature of plate is 190 DEG C, stirring frequency is 40Hz, the cladding time is 8h；
(5) sucking filtration removes methanol and is vacuum dried 18h, then under the protection of xenon, with the liter of 5 DEG C/min
Warm speed is warmed up to 650 DEG C, and then constant temperature 8h is warmed up to 1150 DEG C with the programming rate of 4 DEG C/min, constant temperature
8h, finally naturally cools to room temperature and obtains cathode pole piece；
(6) lithium metaaluminate, LA132 binding agent, CMC binding agent and conductive agent are mixed, and secondary
Distilled water is configured to the lithium metaaluminate slurry that concentration is 30%；
(7) the cathode pole piece surface-coated that above-mentioned slurry is obtained in step (5) using ultrasonic spraying process, its
Coating thickness is 10 μm；
(8) by the cathode pole piece after above-mentioned surface-coated under the conditions of temperature is 70 DEG C, baking 2h, dry
To finished product.
The nano-silicon that the present invention adopts has that specific surface area is big, ion the evolving path is short, wriggling strong and plasticity
High the features such as, the bulk effect of alloy type material can be suppressed to a certain extent, and improve its chemical property
Using to carrying out the mechanical ball milling this modified technique to graphite surface of mixing, material not only can be greatly improved
Coulombic efficiency first, extends the cycle life of electrode additionally it is possible to shorten the evolving path in graphite linings for the lithium ion,
Improve the high rate capability of electrode material；Improve the conduction velocity of lithium ion battery, reduce lithium ion battery
The dendrite that analysis lithium produces punctures the probability of barrier film, reduces battery short circuit probability, improves the security performance of battery.
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned enforcement
Mode, in the ken that one skilled in the relevant art possesses, can also be without departing from this patent ancestor
On the premise of purport, various changes can be made.
Claims (8)
1. a kind of lithium ion battery negative material of high safety performance is it is characterised in that include according to the raw material of weight portion：Drip
Blue or green 2-10 part, silica flour 5-30 part, graphite 60-80 part, lithium metaaluminate 10-20 part, Colophonium 2-10 part, LA132 bonding
Agent 1-2 part, CMC binding agent 0.5-1 part, conductive agent 0.1-0.2 part.
2. the lithium ion battery negative material of high safety performance according to claim 1 is it is characterised in that according to weight
The raw material of part includes：Silica flour 10-25 part, graphite 65-75 part, lithium metaaluminate 12-18 part, Colophonium 4-8 part, LA132
Binding agent 1.2-1.8 part, CMC binding agent 0.6-0.8 part, conductive agent 0.12-0.18 part.
3. the lithium ion battery negative material of high safety performance according to claim 1 is it is characterised in that according to weight
The raw material of part includes：20 parts of silica flour, 70 parts of graphite, 15 parts of lithium metaaluminate, 6 parts of Colophonium, 1.5 parts of LA132 binding agent,
0.7 part of CMC binding agent, 0.15 part of conductive agent.
4. the lithium ion battery negative material according to the arbitrary described high safety performance of claim 1-3 is it is characterised in that institute
The granularity stating silica flour is 50-500nm.
5. the lithium ion battery negative material according to the arbitrary described high safety performance of claim 1-3 is it is characterised in that institute
The granularity stating graphite is 7-22um.
6. a kind of preparation method of the described lithium ion battery negative material of high safety performance as arbitrary in claim 1-3, its
It is characterised by, comprise the following steps that：
(1) weigh each raw material according to weight portion；
(2) silica flour and graphite are carried out mixing after mechanical ball milling 2-8h, the rotating speed of mechanical ball milling mixing is 1000-4000rpm,
And it is dried 10-15h under vacuum, drying temperature is 50-180 DEG C；
(3) Colophonium is dissolved in solvent, solution temperature is 40-190 DEG C, stirring frequency is 10-40Hz, mixing time is
4-8h；
(4) it is added in the solution of step (3) after the silica flour that step (2) is obtained and the mixture cooling of graphite and carry out
Cladding, temperature of plate is 40-190 DEG C, and stirring frequency is 10-40Hz, and the cladding time is 4-8h；
(5) sucking filtration removes solvent and is vacuum dried 5-18h, then under the protection of noble gases, with the liter of 1-5 DEG C/min
Warm speed is warmed up to 420-650 DEG C, constant temperature 3-8h, is then warmed up to 950-1150 DEG C with the programming rate of 2.5-4 DEG C/min,
Constant temperature 5-8h, finally naturally cools to room temperature and obtains cathode pole piece；
(6) lithium metaaluminate, LA132 binding agent, CMC binding agent and conductive agent are mixed, joined with redistilled water
It is set to the lithium metaaluminate slurry that concentration is 1-30%；
(7) the cathode pole piece surface-coated that above-mentioned slurry is obtained in step (5) using ultrasonic spraying process, its coating thickness
For 1-10 μm；
(8) by the cathode pole piece after above-mentioned surface-coated under the conditions of temperature is for 50-70 DEG C, toast 0.5-2h, be dried to obtain
Finished product.
7. the lithium ion battery negative material of high safety performance according to claim 6 preparation method it is characterised in that
Described solvent is toluene, quinoline, carbon tetrachloride, petroleum ether, industrial naptha, methanol, ethanol, isopropanol, acetone and second
One of acetoacetic ester or two or more.
8. the lithium ion battery negative material of high safety performance according to claim 6 preparation method it is characterised in that
Described noble gases are one of nitrogen, argon, helium, neon and xenon or two or more.
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| US20130252097A1 (en) * | 2013-06-11 | 2013-09-26 | Electrochemical Materials | Method to prepare silicon particles for use in lithium secondary battery anodes |
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