CN108172792A - A kind of composite cathode material for lithium ion cell and preparation method thereof - Google Patents
A kind of composite cathode material for lithium ion cell and preparation method thereof Download PDFInfo
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- CN108172792A CN108172792A CN201711431615.XA CN201711431615A CN108172792A CN 108172792 A CN108172792 A CN 108172792A CN 201711431615 A CN201711431615 A CN 201711431615A CN 108172792 A CN108172792 A CN 108172792A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/36—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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- H01M4/00—Electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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Abstract
The invention discloses a kind of composite cathode material for lithium ion cell and preparation method thereof, include the raw material of following parts by weight：23 parts of 22 36 parts of graphene, 12 18 parts of nano silica fume, 30 40 parts of fourth amylalcohol, 58 parts of polypropylene elastomer, 5 10 parts of oxalic acid, 68 parts of sponge gourd, 35 parts of sodium carboxymethylcellulose, 48 parts of potassium permanganate, 1.5 3.4 parts of sodium bicarbonate and ethylenediamine.Raw material sources of the present invention are extensive, and preparation method is simple, and by the interaction between various raw materials, the finished product of preparation is of good performance on coulombic efficiency for the first time, discharge capacity and capacity retention ratio, have the extensive utility value of industrialization.
Description
Technical field
The present invention relates to field of batteries, specifically a kind of composite cathode material for lithium ion cell.
Background technology
In recent years, consumer electronics product increasingly tends to personalized and multifunction, and consumer uses the longevity to battery
Life, energy density and safety more are paid close attention to.Therefore, the negative material that some have extended cycle life and energy density is high is wide
It studies generally.Lithium ion battery is a kind of secondary cell (rechargeable battery), it relies primarily on lithium ion between a positive electrode and a negative electrode
Movement carrys out work.In charge and discharge process, Li+Round-trip insertion and deintercalation between two electrodes：During charging, Li+It is taken off from anode
It is embedding, cathode is embedded in by electrolyte, cathode is in rich lithium state；It is then opposite during electric discharge.
Traditional lithium ion battery negative material is using copper foil as collector, and copper foil not only cannot provide appearance to electrode slice
Amount, also accounts for electrode slice major part weight, and copper foil quality is several times of active material even higher, makes electricity for collector using copper foil
The energy density in pond reduces.In addition, copper foil is dense, inside is big for bulk effect in charge and discharge process without pore space structure
Electrode material, copper foil current collector cannot effectively alleviate bulk effect of the active material in cyclic process, cause active material
It is easy to be detached from copper foil current collector in cyclic process dusting.Due to silicon have highest theoretical specific capacity (4200mAh/g) and compared with
Low de- lithium current potential (being less than 0.5V), in recent years as one of most potential lithium ion battery negative material.
Invention content
The purpose of the present invention is to provide a kind of composite cathode material for lithium ion cell, to solve to carry in above-mentioned background technology
The problem of going out.
To achieve the above object, the present invention provides following technical solution：
A kind of composite cathode material for lithium ion cell includes the raw material of following parts by weight：22-36 parts of graphene, nano-silicon
12-18 parts of powder, 30-40 parts of fourth amylalcohol, 5-8 parts of polypropylene elastomer, 5-10 parts of oxalic acid, 6-8 parts of sponge gourd, sodium carboxymethylcellulose
2-3 parts of 3-5 parts, 4-8 parts of potassium permanganate, 1.5-3.4 parts of sodium bicarbonate and ethylenediamine.
As further embodiment of the present invention：Graphene is used in three layer graphenes, multi-layer graphene and graphene oxide
At least one.
As further embodiment of the present invention：The average molecular weight of polypropylene elastomer is 32500-36800.
The preparation method of the composite cathode material for lithium ion cell, is as follows：
Step 1, by sponge gourd slice be put into marmite and add in 6-10 times of its weight water immersion 30-60 minutes, then
It is heated to boiling, small fire is endured 1.5-3 hours slowly, is added in sodium carboxymethylcellulose and is continued after boiling 15-25 minutes, silk is obtained by filtration
Melon filtrate；
Nano silica fume is added in fourth amylalcohol and ultrasonic wave disperses 20-35 minutes, obtains nano silica fume dispersion by step 2
Liquid；
Step 3, by the mixing of graphene, polypropylene elastomer, potassium permanganate, sodium bicarbonate and ethylenediamine and dry method ball
20-40 mesh is milled to, obtains the first mixture, oxalic acid and deionized water are then added in into the first mixture and continues mixing and is stirred
It mixes, then evaporation drying, you can obtain the second mixture；
Step 4 stirs the second mixture, sponge gourd filtrate and nano silica fume dispersion liquid, obtains third mixing
Then third mixture is warming up to 320-400 degrees Celsius simultaneously by object by the speed of 2.5-4 degrees celsius/minutes in a nitrogen atmosphere
And 1-1.5 hours are kept the temperature, then 650-820 degrees Celsius is warming up to the speed of 6-8 degrees celsius/minutes and keep the temperature 5-8 hours,
It can obtain finished product.
As further embodiment of the present invention：It is needed before nitrogen atmosphere heating to third mixture in 3.2- in step 4
Hip treatment is carried out under 4.8Mpa.
Compared with prior art, the beneficial effects of the invention are as follows：Raw material sources of the present invention are extensive, and preparation method is simple, lead to
The interaction between various raw materials is crossed, the finished product of preparation has on coulombic efficiency for the first time, discharge capacity and capacity retention ratio
Superior performance has the extensive utility value of industrialization.
Specific embodiment
The technical solution of this patent is described in more detail With reference to embodiment.
Embodiment 1
A kind of composite cathode material for lithium ion cell includes the raw material of following parts by weight：22 parts of graphene, nano silica fume 12
Part, 30 parts of fourth amylalcohol, 5 parts of polypropylene elastomer, 5 parts of oxalic acid, 6 parts of sponge gourd, 3 parts of sodium carboxymethylcellulose, 4 parts of potassium permanganate,
2 parts of 1.5 parts of sodium bicarbonate and ethylenediamine.Graphene is using three layer graphenes and the mixture of multi-layer graphene.
The preparation method of the composite cathode material for lithium ion cell, is as follows：
Step 1, the water that sponge gourd slice is put into marmite and adds in 7 times of its weight are impregnated 45 minutes, are then heated to
Boiling, small fire are endured 2 hours slowly, are added in sodium carboxymethylcellulose and are continued after boiling 22 minutes, sponge gourd filtrate is obtained by filtration；
Nano silica fume is added in fourth amylalcohol and ultrasonic wave disperses 26 minutes, obtains nano silica fume dispersion liquid by step 2；
Step 3, by the mixing of graphene, polypropylene elastomer, potassium permanganate, sodium bicarbonate and ethylenediamine and dry method ball
30 mesh are milled to, obtain the first mixture, oxalic acid and deionized water are then added in into the first mixture and continue to be mixed,
Then evaporation drying, you can obtain the second mixture；
Step 4 stirs the second mixture, sponge gourd filtrate and nano silica fume dispersion liquid, obtains third mixing
Then third mixture is warming up to 360 degrees Celsius and heat preservation 1 by object by the speed of 2.5 degrees celsius/minutes in a nitrogen atmosphere
Hour, then 676 degrees Celsius are warming up to the speed of 7 degrees celsius/minutes and keep the temperature 6 hours, you can obtain finished product.
Embodiment 2
A kind of composite cathode material for lithium ion cell includes the raw material of following parts by weight：27 parts of graphene, nano silica fume 14
Part, 33 parts of fourth amylalcohol, 6 parts of polypropylene elastomer, 7.5 parts of oxalic acid, 6.6 parts of sponge gourd, 3.6 parts of sodium carboxymethylcellulose, permanganic acid
2.4 parts of 5.2 parts of potassium, 2.1 parts of sodium bicarbonate and ethylenediamine.The average molecular weight of polypropylene elastomer is 32500-36800.
The preparation method of the composite cathode material for lithium ion cell, is as follows：
Step 1, the water that sponge gourd slice is put into marmite and adds in 9 times of its weight are impregnated 50 minutes, are then heated to
Boiling, small fire are endured 2 hours slowly, are added in sodium carboxymethylcellulose and are continued after boiling 21 minutes, sponge gourd filtrate is obtained by filtration；
Nano silica fume is added in fourth amylalcohol and ultrasonic wave disperses 30 minutes, obtains nano silica fume dispersion liquid by step 2；
Step 3, by the mixing of graphene, polypropylene elastomer, potassium permanganate, sodium bicarbonate and ethylenediamine and dry method ball
20 mesh are milled to, obtain the first mixture, oxalic acid and deionized water are then added in into the first mixture and continue to be mixed,
Then evaporation drying, you can obtain the second mixture；
Step 4 stirs the second mixture, sponge gourd filtrate and nano silica fume dispersion liquid, obtains third mixing
Then third mixture is warming up to 380 degrees Celsius and heat preservation 1.5 by object by the speed of 4 degrees celsius/minutes in a nitrogen atmosphere
Hour, then 750 degrees Celsius are warming up to the speed of 8 degrees celsius/minutes and keep the temperature 8 hours, you can obtain finished product.
Embodiment 3
A kind of composite cathode material for lithium ion cell includes the raw material of following parts by weight：32 parts of graphene, nano silica fume 16
Part, 37 parts of fourth amylalcohol, 7 parts of polypropylene elastomer, 8 parts of oxalic acid, 7.5 parts of sponge gourd, 4.4 parts of sodium carboxymethylcellulose, potassium permanganate 7
2.6 parts of part, 2.8 parts of sodium bicarbonate and ethylenediamine.Graphene uses multi-layer graphene.
The preparation method of the composite cathode material for lithium ion cell, is as follows：
Step 1, the water that sponge gourd slice is put into marmite and adds in 8 times of its weight are impregnated 46 minutes, are then heated to
Boiling, small fire are endured 2.5 hours slowly, are added in sodium carboxymethylcellulose and are continued after boiling 23 minutes, sponge gourd filtrate is obtained by filtration；
Nano silica fume is added in fourth amylalcohol and ultrasonic wave disperses 34 minutes, obtains nano silica fume dispersion liquid by step 2；
Step 3, by the mixing of graphene, polypropylene elastomer, potassium permanganate, sodium bicarbonate and ethylenediamine and dry method ball
40 mesh are milled to, obtain the first mixture, oxalic acid and deionized water are then added in into the first mixture and continue to be mixed,
Then evaporation drying, you can obtain the second mixture；
Step 4 stirs the second mixture, sponge gourd filtrate and nano silica fume dispersion liquid, obtains third mixing
Third mixture is carried out hip treatment by object under 4.5Mpa, then that third mixture is Celsius by 3 in a nitrogen atmosphere
Degree/min speed be warming up to 375 degrees Celsius and keep the temperature 1 hour, be then warming up to 780 with the speed of 8 degrees celsius/minutes and take the photograph
Family name's degree and keep the temperature 7 hours, you can obtain finished product.
Embodiment 4
A kind of composite cathode material for lithium ion cell includes the raw material of following parts by weight：36 parts of graphene, nano silica fume 18
Part, 40 parts of fourth amylalcohol, 8 parts of polypropylene elastomer, 10 parts of oxalic acid, 8 parts of sponge gourd, 5 parts of sodium carboxymethylcellulose, 8 parts of potassium permanganate,
3 parts of 3.4 parts of sodium bicarbonate and ethylenediamine.Graphene uses the mixture of three layer graphenes, multi-layer graphene and graphene oxide.
The average molecular weight of polypropylene elastomer is 32500-36800.
The preparation method of the composite cathode material for lithium ion cell, is as follows：
Step 1, the water that sponge gourd slice is put into marmite and adds in 10 times of its weight are impregnated 50 minutes, are then heated
To boiling, small fire is endured 3 hours slowly, is added in sodium carboxymethylcellulose and is continued tanning after twenty minutes, sponge gourd filtrate is obtained by filtration；
Nano silica fume is added in fourth amylalcohol and ultrasonic wave disperses 32 minutes, obtains nano silica fume dispersion liquid by step 2；
Step 3, by the mixing of graphene, polypropylene elastomer, potassium permanganate, sodium bicarbonate and ethylenediamine and dry method ball
40 mesh are milled to, obtain the first mixture, oxalic acid and deionized water are then added in into the first mixture and continue to be mixed,
Then evaporation drying, you can obtain the second mixture；
Step 4 stirs the second mixture, sponge gourd filtrate and nano silica fume dispersion liquid, obtains third mixing
Third mixture is carried out hip treatment by object under 4.2Mpa, then that third mixture is Celsius by 3 in a nitrogen atmosphere
Degree/min speed be warming up to 350 degrees Celsius and keep the temperature 1.5 hours, be then warming up to 810 with the speed of 8 degrees celsius/minutes
Degree Celsius and keep the temperature 6 hours, you can obtain finished product.
Comparative example 1
Except sponge gourd is not contained, remaining raw material and preparation method are same as Example 2.
The product of product and comparative example 1 to embodiment 1-4 is tested for the property, and test result is shown in Table 1.
Table 1
The product of embodiment 1-4 is more excellent on chemical property than the product of embodiment 1 as can be seen from Table 1, this hair
The product of bright preparation is of good performance on coulombic efficiency for the first time and capacity retention ratio.
It is obvious to a person skilled in the art that the present invention is not limited to the details of above-mentioned exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requirement rather than above description limit, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in each embodiment can also be properly combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (5)
1. a kind of composite cathode material for lithium ion cell, which is characterized in that include the raw material of following parts by weight：Graphene 22-36
Part, 12-18 parts of nano silica fume, 30-40 parts of fourth amylalcohol, 5-8 parts of polypropylene elastomer, 5-10 parts of oxalic acid, 6-8 parts of sponge gourd, carboxylic first
2-3 parts of 3-5 parts of base sodium cellulosate, 4-8 parts of potassium permanganate, 1.5-3.4 parts of sodium bicarbonate and ethylenediamine.
2. composite cathode material for lithium ion cell according to claim 1, which is characterized in that the graphene uses three layers
At least one of graphene, multi-layer graphene and graphene oxide.
3. composite cathode material for lithium ion cell according to claim 1, which is characterized in that the polypropylene elastomer
Average molecular weight is 32500-36800.
4. a kind of preparation method of composite cathode material for lithium ion cell as described in any one of claims 1-3, which is characterized in that
It is as follows：
Step 1, the water that sponge gourd slice is put into marmite and adds in 6-10 times of its weight are impregnated 30-60 minutes, are then heated
To boiling, small fire is endured 1.5-3 hours slowly, is added in sodium carboxymethylcellulose and is continued after boiling 15-25 minutes, sponge gourd filter is obtained by filtration
Liquid；
Nano silica fume is added in fourth amylalcohol and ultrasonic wave disperses 20-35 minutes, obtains nano silica fume dispersion liquid by step 2；
Step 3, by graphene, polypropylene elastomer, potassium permanganate, sodium bicarbonate and ethylenediamine mix and dry ball milling extremely
20-40 mesh obtains the first mixture, and oxalic acid and deionized water are then added in into the first mixture and continues to be mixed,
Then evaporation drying, you can obtain the second mixture；
Second mixture, sponge gourd filtrate and nano silica fume dispersion liquid are stirred, obtain third mixture by step 4,
Then third mixture is warming up to 320-400 degrees Celsius by the speed of 2.5-4 degrees celsius/minutes in a nitrogen atmosphere and protected
It is 1-1.5 hours warm, then 650-820 degrees Celsius is warming up to the speed of 6-8 degrees celsius/minutes and keep the temperature 5-8 hours, you can
Obtain finished product.
5. the preparation method of composite cathode material for lithium ion cell according to claim 4, which is characterized in that the step
It needs to carry out hip treatment under 3.2-4.8Mpa to third mixture before nitrogen atmosphere heating in four.
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| CN106058257A (en) * | 2016-08-17 | 2016-10-26 | 江苏中兴派能电池有限公司 | Preparation method of graphene-coated silicon-carbon composite anode material and lithium ion battery |
| CN106410200A (en) * | 2016-10-20 | 2017-02-15 | 浙江极力动力新能源有限公司 | Preparation method of lithium battery negative pole material |
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2017
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|---|---|---|---|---|
| CN102130326A (en) * | 2011-02-12 | 2011-07-20 | 中南大学 | High-capacity functionalized carbon layered electrode and preparation method thereof |
| CN103855365A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院大连化学物理研究所 | Nitrogen-doped porous carbon material for lithium-air battery positive electrode |
| CN103855366A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院大连化学物理研究所 | Nitrogen-doped porous carbon material for lithium-air battery positive electrode |
| CN103259012A (en) * | 2013-05-15 | 2013-08-21 | 江西师范大学 | Preparation method of three-dimensional conductive super-iron battery K2FeO4/C composite negative pole material |
| CN104993160A (en) * | 2015-08-04 | 2015-10-21 | 重庆大学 | Preparing method for non-precious metal ion complexation Schiff base graphene catalyst |
| CN106058257A (en) * | 2016-08-17 | 2016-10-26 | 江苏中兴派能电池有限公司 | Preparation method of graphene-coated silicon-carbon composite anode material and lithium ion battery |
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