CN109103454A - Lithium battery graphene conductive slurry and preparation method thereof - Google Patents
Lithium battery graphene conductive slurry and preparation method thereof Download PDFInfo
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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
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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
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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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Abstract
The invention discloses a kind of lithium battery graphene conductive slurry and preparation method thereof, the electrocondution slurry is made of the raw material of following weight fraction ratio: 40-60 parts of graphene, 3-5 parts of lucium, 4-8 parts of molybdenum oxide, 2-5 parts of cobalt oxide, 100-200 parts of solvent, 5-10 parts of Myrj 45,2-5 parts of polyoxyethylene glycerine borate aliphatic ester, 1-6 parts of dodecyl phenol polyethenoxy ether and 4-8 parts of decamethylcyclopentaandoxane.It the advantages that the advantages that conductive energy of cell conductive paste provided by the invention is excellent, resistance is small, long service life, charging and discharging do not generate heat in the process, good dispersion, preparation process is simple, is easy to realize industrial production.
Description
Technical field
The present invention relates to battery technology field, specifically a kind of lithium battery graphene conductive slurry and preparation method thereof.
Background technique
Lithium battery is as a kind of novel high-energy secondary power supply, big, discharging voltage balance, voltage high and low temperature with specific energy
Performance is good, pollution-free, security performance is superior and storage and long working life, the advantages that utilization rate is high.But the lithium of the prior art
Battery mainly uses electrically conductive graphite, acetylene black and carbon nanotube as electrocondution slurry, and acetylene black is by amorphous carbon spherical in shape
The chain object of particle composition is current the most widely used electrocondution slurry, cheap, but in order to reach enhancing electrode activity
The purpose to contact with each other between substance, required additive amount is larger, to cause the decline of electrode capacity；Carbon nanotube is in line
The one-dimensional carbonaceous material of type, compared with acetylene black, carbon nanotube has more preferably electric conductivity and additive amount is few, but carbon is received at present
Mitron it is expensive, and the shortcomings that there are difficulties in dispersion when using as electrocondution slurry.
Graphene is due to big theoretical specific surface area, mechanical property outstanding and heating conduction, and at room temperature
The advantages that high conductivity, and it is low in cost, machinability is good, thus in nano electron device, sensor, hydrogen storage material, lithium
The various fields such as battery, supercapacitor have potential application prospect.But due to graphene slurry or powder in storage and
There are the problem that unstable, easy to reunite and compatibility differs in use process, cannot abundant grapheme material high-ratio surface, height
Conductive and high thermal conductivity performance advantage, this problem limit graphene in the application of field of lithium.
Summary of the invention
The present invention leads to the conductive capability of electrocondution slurry for the bad dispersibility of graphene in current battery conduction slurries
Difference, the cycle life for preparing battery is short, stablizes the problems such as difference, provides a kind of lithium battery graphene conductive slurry and its preparation side
Method.Electrocondution slurry provided by the invention has excellent dispersibility, electric conductivity and stability, and graphene is pushed to lead in battery
Domain can be widely applied.
In order to achieve the goal above, The technical solution adopted by the invention is as follows:
A kind of lithium battery graphene conductive slurry, is made of the raw material of following weight fraction ratio: 40-60 parts of graphene, rare earth
3-5 parts of mixture, 4-8 parts of molybdenum oxide, 2-5 parts of cobalt oxide, 100-200 parts of solvent, 5-10 parts of Myrj 45, polyoxy
2-5 parts of ethylene glycerine borate aliphatic ester, 1-6 parts of dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane 4-8
Part.
Further, the lucium is lanthanum, yttrium and samarium composition.Preferably, lanthanum in the lucium, yttrium and
The mass ratio of samarium is 1-3:0.2-1:0.5-2.
Further, the solvent is one of polyethylene glycol, ethyl alcohol, ethyl acetate, dimethyl sulfoxide or multiple combinations.
The present invention also provides the lithium battery preparation methods of graphene conductive slurry, comprising the following steps:
S1: according to parts by weight than meter, by 40-60 parts of graphene, 5-10 parts of Myrj 45, polyoxyethylene glycerine
4-8 parts of 2-5 parts of borate aliphatic ester, 1-6 parts of dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and solvent 50-
100 parts of addition ultrasonic dispersing machines, ultrasonic disperse 30-60min obtain graphene mixed liquor；
S2: in graphene mixed liquor be added 10-30 parts of lithium electrode material, 1-3 parts of lucium, 3-5 parts of lucium,
4-8 parts of molybdenum oxide, 2-5 parts of cobalt oxide and remaining solvent continue ultrasonic wave and disperse 20-40min, obtain electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered to the electrocondution slurry for carrying out using after electrostatic spinning to get lithium battery in syringe.
Further, the supersonic frequency of the ultrasonic disperse is 40-60KHz.
Further, the electrostatic spinning is flow velocity is 0.1-0.5mL/h, voltage is 15-25KV and needle diameter is 0
.1mm-1.0mm it is carried out under conditions of.
Further, raw material is first ground to 150-250 mesh before weighing each component raw material by the method.
Further, the lithium electrode material includes in lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate or lithia
It is a kind of.
Compared with prior art, advantages of the present invention and benefit effect are as follows:
1, the present invention is metal oxide supported on graphene by molybdenum oxide and cobalt oxide, and the synergistic effect due to three is being kept
While lithium battery height ratio capacity, high conductivity, moreover it is possible to improve the cyclical stability of electrode system, be added in the reaction system poly-
Ethylene oxide stearate, polyoxyethylene glycerine borate aliphatic ester, dodecyl phenol polyethenoxy ether and decamethyl ring five
Siloxanes can be increased substantially the compatibility and dispersibility of battery system, be solved graphite due to the synergistic effect of each component
The agglomeration traits of alkene.
2, Myrj 45 is added in the present invention in battery system, and structure has hydrophilic lipophilic group, parent
Water base group has significant solubilization to battery system, and lipophilic group is capable of forming the Hydration Shell for surrounding particle, solves graphite
The agglomeration traits of alkene battery system.
3, the polyoxyethylene glycerine borate aliphatic ester that the present invention quotes is the boron that B-O key is formed using boric acid as parent
The compound of esters of gallic acid all has good compatibility with inorganic and organic substance, has excellent dispersion performance.
4, the dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane that the present invention uses not only have excellent profit
Wet ability and defoaming capacity also have good dispersion effect, with Myrj 45, polyoxyethylene glycerine borate
Aliphatic ester generates good synergy, and each component is enabled to be uniformly dispersed in battery system.
5, the present invention is additionally added the lucium of lanthanum, yttrium and samarium composition, and the creep-resistant property that battery can be improved makes electricity
Tank discharge performance is more stable, moreover it is possible to improve the capacitance of battery.
6, the conductive energy of cell conductive paste provided by the invention is excellent, resistance is small, long service life, charging and discharging
Do not generate heat in the process, good dispersion the advantages that, preparation process is simple, industrialized production easy to accomplish, has preferable economic effect
Benefit and social benefit.
Specific embodiment
Invention is further described in detail With reference to embodiment.It is emphasized that following the description is only
It is merely exemplary, the range and its application being not intended to be limiting of the invention.
Embodiment 1
A kind of lithium battery graphene conductive slurry, is made of the raw material of following weight fraction ratio: 50 parts of graphene, rare earth mixing
3 parts of object, 6 parts of molybdenum oxide, 4 parts of cobalt oxide, 150 parts of polyethylene glycol, 4 parts of Myrj 45, polyoxyethylene glycerine boron
3 parts of acid esters aliphatic ester, 3 parts of dodecyl phenol polyethenoxy ether and 6 parts of decamethylcyclopentaandoxane.The lucium by
Lanthanum, yttrium and the samarium composition that mass ratio is 1.5:0.5:1.
Raw material is first ground to 200 mesh, preparation process packet before weighing each component raw material by the preparation of this example electrocondution slurry
Include following steps:
S1: according to parts by weight than meter, by graphene, Myrj 45, polyoxyethylene glycerine borate fatty acid
Ester, dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and 100 parts of addition ultrasonic dispersing machines of polyethylene glycol, in frequency
Rate is 50KHz ultrasonic disperse 50min, obtains graphene mixed liquor；
S2: 20 parts of lithium carbonate, lucium, lucium, molybdenum oxide, cobalt oxide are added in graphene mixed liquor and remains
Remaining polyethylene glycol continues ultrasonic wave and disperses 30min, obtains electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered in syringe flow velocity is 0.5mL/h, voltage is 20KV and needle diameter is 0
.5mm the electrocondution slurry used after electrostatic spinning to get lithium battery is carried out under conditions of.
Embodiment 2
A kind of lithium battery graphene conductive slurry, is made of the raw material of following weight fraction ratio: 45 parts of graphene, rare earth mixing
4 parts of object, 5 parts of molybdenum oxide, 3 parts of cobalt oxide, 100 parts of dimethyl sulfoxide, 5 parts of Myrj 45, polyoxyethylene glycerine boron
3 parts of acid esters aliphatic ester, 5 parts of dodecyl phenol polyethenoxy ether and 4 parts of decamethylcyclopentaandoxane.The lucium by
Lanthanum, yttrium and the samarium composition that mass ratio is 2.5:1:0.5.
Raw material is first ground to 150 mesh, preparation process packet before weighing each component raw material by the preparation of this example electrocondution slurry
Include following steps:
S1: according to parts by weight than meter, by graphene, Myrj 45, polyoxyethylene glycerine borate fatty acid
Ester, dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and 80 parts of addition ultrasonic dispersing machines of dimethyl sulfoxide, in frequency
Rate is 40KHz ultrasonic disperse 60min, obtains graphene mixed liquor；
S2: in graphene mixed liquor be added 25 parts of lithium hydroxide, lucium, lucium, molybdenum oxide, cobalt oxide and
Remaining polyethylene glycol continues ultrasonic wave and disperses 25min, obtains electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered in syringe flow velocity is 0.2mL/h, voltage is 25KV and needle diameter is 0
.2mm the electrocondution slurry used after electrostatic spinning to get lithium battery is carried out under conditions of.
Embodiment 3
A kind of lithium battery graphene conductive slurry, is made of the raw material of following weight fraction ratio: 55 parts of graphene, rare earth mixing
5 parts of object, 7 parts of molybdenum oxide, 2 parts of cobalt oxide, 180 parts of ethyl alcohol, 8 parts of Myrj 45, polyoxyethylene glycerine borate
2.5 parts of aliphatic ester, 4 parts of dodecyl phenol polyethenoxy ether and 7 parts of decamethylcyclopentaandoxane.The lucium is by matter
Amount is formed than the lanthanum, yttrium and samarium for being 3:1:1.
Raw material is first ground to 250 mesh, preparation process packet before weighing each component raw material by the preparation of this example electrocondution slurry
Include following steps:
S1: according to parts by weight than meter, by graphene, Myrj 45, polyoxyethylene glycerine borate fatty acid
Ester, dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and 150 parts of addition ultrasonic dispersing machines of ethyl alcohol are in frequency
60KHz ultrasonic disperse 40min, obtains graphene mixed liquor；
S2: 30 parts of lithium acetate, lucium, lucium, molybdenum oxide, cobalt oxide are added in graphene mixed liquor and remains
Remaining ethyl alcohol continues ultrasonic wave and disperses 20min, obtains electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered in syringe flow velocity is 0.5mL/h, voltage is 15KV and needle diameter is 0
.1mm the electrocondution slurry used after electrostatic spinning to get lithium battery is carried out under conditions of.
Embodiment 4
A kind of lithium battery graphene conductive slurry, is made of the raw material of following weight fraction ratio: 40 parts of graphene, rare earth mixing
3.5 parts of object, 4 parts of molybdenum oxide, 5 parts of cobalt oxide, 200 parts of ethyl acetate, 10 parts of Myrj 45, polyoxyethylene glycerine
2 parts of borate aliphatic ester, 3 parts of dodecyl phenol polyethenoxy ether and 5 parts of decamethylcyclopentaandoxane.The lucium
It is made of lanthanum, yttrium and samarium that mass ratio is 1:0.5:2.
Raw material is first ground to 150 mesh, preparation process packet before weighing each component raw material by the preparation of this example electrocondution slurry
Include following steps:
S1: according to parts by weight than meter, by graphene, Myrj 45, polyoxyethylene glycerine borate fatty acid
Ester, dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and 150 parts of addition ultrasonic dispersing machines of ethyl acetate, in frequency
Rate is 50KHz ultrasonic disperse 30min, obtains graphene mixed liquor；
S2: 15 parts of lithium nitrate, lucium, lucium, molybdenum oxide, cobalt oxide are added in graphene mixed liquor and remains
Remaining ethyl acetate continues ultrasonic wave and disperses 30min, obtains electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered in syringe flow velocity is 0.1mL/h, voltage is 20KV and needle diameter is 0
.5mm the electrocondution slurry used after electrostatic spinning to get lithium battery is carried out under conditions of.
Embodiment 5
A kind of lithium battery graphene conductive slurry, is made of the raw material of following weight fraction ratio: 60 parts of graphene, rare earth mixing
4 parts of object, 8 parts of molybdenum oxide, 3 parts of cobalt oxide, polyethylene glycol 200 part, 8 parts of Myrj 45, polyoxyethylene glycerine boron
5 parts of acid esters aliphatic ester, 6 parts of dodecyl phenol polyethenoxy ether and 6 parts of decamethylcyclopentaandoxane.The lucium by
Lanthanum, yttrium and the samarium composition that mass ratio is 2.5:0.8:0.7.
Raw material is first ground to 200 mesh, preparation process packet before weighing each component raw material by the preparation of this example electrocondution slurry
Include following steps:
S1: according to parts by weight than meter, by graphene, Myrj 45, polyoxyethylene glycerine borate fatty acid
Ester, dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and 150 parts of addition ultrasonic dispersing machines of polyethylene glycol, in frequency
Rate is 60KHz ultrasonic disperse 50min, obtains graphene mixed liquor；
S2: 20 parts of lithia, lucium, lucium, molybdenum oxide, cobalt oxide are added in graphene mixed liquor and remains
Remaining polyethylene glycol continues ultrasonic wave and disperses 40min, obtains electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered in syringe flow velocity is 0.5mL/h, voltage is 15KV and needle diameter is
The electrocondution slurry used after electrostatic spinning to get lithium battery is carried out under conditions of 0.1mm.
Embodiment 6
A kind of lithium battery graphene conductive slurry, is made of the raw material of following weight fraction ratio: 50 parts of graphene, rare earth mixing
5 parts of object, 6 parts of molybdenum oxide, 4 parts of cobalt oxide, 150 parts of ethyl acetate, 6 parts of Myrj 45, polyoxyethylene glycerine boron
4 parts of acid esters aliphatic ester, 5 parts of dodecyl phenol polyethenoxy ether and 8 parts of decamethylcyclopentaandoxane.The lucium by
Lanthanum, yttrium and the samarium composition that mass ratio is 1:1:1.
Raw material is first ground to 250 mesh, preparation process packet before weighing each component raw material by the preparation of this example electrocondution slurry
Include following steps:
S1: according to parts by weight than meter, by graphene, Myrj 45, polyoxyethylene glycerine borate fatty acid
Ester, dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and 100 parts of addition ultrasonic dispersing machines of ethyl acetate, in frequency
Rate is 40KHz ultrasonic disperse 60min, obtains graphene mixed liquor；
S2: add 20 parts of lithium carbonate, lucium, lucium, molybdenum oxide, cobalt oxide and residue in graphene mixed liquor
Polyethylene glycol, continue ultrasonic wave disperse 30min, obtain electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered in syringe flow velocity is 0.5mL/h, voltage is 25KV and needle diameter is
The electrocondution slurry used after electrostatic spinning to get lithium battery is carried out under conditions of 0.2mm.
Comparative example 1
This comparative example and embodiment 6 the difference is that: this example is added without Myrj 45, remaining component and preparation
Method is same as Example 6.
Comparative example 2
This comparative example and embodiment 6 the difference is that: this example is added without polyoxyethylene glycerine borate aliphatic ester,
Remaining component and preparation method are same as Example 6.
Comparative example 3
This comparative example and embodiment 6 the difference is that: this example is added without dodecyl phenol polyethenoxy ether, remaining component and
Preparation method is same as Example 6.
Comparative example 4
This comparative example and embodiment 6 the difference is that: this example is added without decamethylcyclopentaandoxane, remaining component and preparation
Method is same as Example 6.
Comparative example 5
This comparative example and embodiment 6 the difference is that: this example is added without Myrj 45, polyoxyethylene glycerine
Borate aliphatic ester, dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane, remaining component and preparation method and reality
It is identical to apply example 6.
Comparative example 6
This comparative example and embodiment 6 the difference is that: this example is added without molybdenum oxide, remaining component and preparation method and implementation
Example 6 is identical.
Comparative example 7
This comparative example and embodiment 6 the difference is that: this example is added without cobalt oxide, remaining component and preparation method and implementation
Example 6 is identical.
Comparative example 8
This comparative example and embodiment 6 the difference is that: this example is added without molybdenum oxide and cobalt oxide, remaining component and preparation side
Method is same as Example 6.
Flexible packing lithium ion battery is conventionally made in electrocondution slurry made from embodiment 1-6 and comparative example, is pressed
The performance of the measuring method test battery of more solito, test result are as shown in table 1:
Table 1: the electric property of graphene conductive slurry of the present invention
Learnt from above-mentioned test result, graphene conductive slurry prepared by the present invention due to each component synergistic effect so that electric
Pond capacitance with higher and stable circulation performance.
The above content is combine it is specific/further detailed description of the invention for preferred embodiment, cannot
Assert that specific implementation of the invention is only limited to these instructions.General technical staff of the technical field of the invention is come
It says, without departing from the inventive concept of the premise, some replacements or modifications can also be made to the embodiment that these have been described,
And these substitutions or variant are regarded as belonging to the scope of protection of the present invention.
Claims (9)
1. a kind of lithium battery graphene conductive slurry, it is characterised in that: the electrocondution slurry by following weight fraction ratio original
Material composition: 40-60 parts of graphene, 4-8 parts of molybdenum oxide, 2-5 parts of cobalt oxide, 100-200 parts of solvent, gathers 3-5 parts of lucium
5-10 parts of ethylene oxide stearate, 2-5 parts of polyoxyethylene glycerine borate aliphatic ester, dodecyl phenol polyethenoxy ether 1-
6 parts and decamethylcyclopentaandoxane 4-8 parts.
2. lithium battery graphene conductive slurry according to claim 1, it is characterised in that: the lucium be lanthanum,
Yttrium and samarium composition.
3. lithium battery graphene conductive slurry according to claim 2, it is characterised in that: lanthanum in the lucium,
The mass ratio of yttrium and samarium is 1-3:0.2-1:0.5-2.
4. lithium battery graphene conductive slurry according to claim 1, it is characterised in that: the solvent be polyethylene glycol,
One of ethyl alcohol, ethyl acetate, dimethyl sulfoxide or multiple combinations.
5. the preparation method of lithium battery graphene conductive slurry according to claim 1, it is characterised in that: including following step
It is rapid:
S1: according to parts by weight than meter, by 40-60 parts of graphene, 5-10 parts of Myrj 45, polyoxyethylene glycerine
4-8 parts of 2-5 parts of borate aliphatic ester, 1-6 parts of dodecyl phenol polyethenoxy ether and decamethylcyclopentaandoxane and solvent 50-
100 parts of addition ultrasonic dispersing machines, ultrasonic disperse 30-60min obtain graphene mixed liquor；
S2: in graphene mixed liquor be added 10-30 parts of lithium electrode material, 1-3 parts of lucium, 3-5 parts of lucium,
4-8 parts of molybdenum oxide, 2-5 parts of cobalt oxide and remaining solvent continue ultrasonic wave and disperse 20-40min, obtain electrocondution slurry；
S3: above-mentioned electrocondution slurry is delivered to the electrocondution slurry for carrying out using after electrostatic spinning to get lithium battery in syringe.
6. the preparation method of lithium battery graphene conductive slurry according to claim 5, it is characterised in that: the ultrasound point
Scattered supersonic frequency is 40-60KHz.
7. the preparation method of lithium battery graphene conductive slurry according to claim 5, it is characterised in that: the Static Spinning
Silk is carried out under conditions of flow velocity is 0.1-0.5mL/h, voltage is 15-25KV and needle diameter is 0 .1mm-1.0mm.
8. the preparation method of lithium battery graphene conductive slurry according to claim 5, it is characterised in that: the method exists
Raw material is first ground to 150-250 mesh before weighing each component raw material.
9. the preparation method of lithium battery graphene conductive slurry according to claim 5, it is characterised in that: the lithium electrode
Material includes one of lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate or lithia.
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| CN115172067A (en) * | 2022-06-30 | 2022-10-11 | 安徽碳华新材料科技有限公司 | Alkene-carbon composite material with high heat conductivity and preparation method thereof |
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Application publication date: 20181228 |