CN107317033A - A kind of graphene/carbon nano-tube composite conducting slurry and preparation method thereof - Google Patents
A kind of graphene/carbon nano-tube composite conducting slurry and preparation method thereof Download PDFInfo
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- CN107317033A CN107317033A CN201610271121.9A CN201610271121A CN107317033A CN 107317033 A CN107317033 A CN 107317033A CN 201610271121 A CN201610271121 A CN 201610271121A CN 107317033 A CN107317033 A CN 107317033A
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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
Abstract
The invention discloses a kind of graphene/carbon nano-tube composite conducting slurry and preparation method thereof, the composite conducting slurry is according to the composition of mass fraction component：1.5 3.0% graphene, 3.0 8.0% CNT, the solvent of 0.3 0.8% dispersant and remaining proportion, wherein dispersant are nonionic surface active agent.First CNT carried out pre-dispersed in the present invention, then carries out the composite diffusion of graphene, can be effectively prevented from it is issuable during graphene dispersion reunite, form the uniform and stable composite conducting slurry of dispersed ultrafine；The graphene of the point at CNT two ends and one-dimensional wire itself and two-dimensional sheet constitutes three-dimensional network conductive structure, significantly improve the electric conductivity of positive and negative pole material, rapid charge characteristic, the high rate performance of battery are improved, the cycle performance and security performance of battery is improved.The electrocondution slurry preparation method of the present invention is simple, is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to lithium ion battery technical field of material, and in particular to a kind of graphene/carbon nano-tube
Composite conducting slurry and preparation method thereof.
Background technology
Dilute graphite is a kind of two-dimensional material being made up of single layer of carbon atom, and graphene is spontaneous as a kind of new carbon
The great interest of domestic and international researcher is caused since existing, by science《Science》It is chosen as the 2009 annual world ten big sciences
One of break through.Graphene is " mono-layer graphite piece ", is the basic structural unit for constituting graphite.It is used as a peacekeeping two-dimensional nano material
The representative of material, CNT was not only had any different but also was related with graphene, and the two has complementarity in structure and performance.From knot
From the point of view of on structure, CNT is the one-dimensional crystal structure of carbon；It is truly and graphene is only made up of single carbon atom layer
Two dimensional crystal structure, is material most thin on our times.CNT drawout just forms graphene for visually, and
Graphene is rolled up just forming CNT.From performance, graphene has can compare favourably or more excellent with CNT
Different characteristic, graphene has electron mobility, thermal conductivity, superelevation charge carrier mobility, the fabulous electronics biography of superelevation
Conductance, high resiliency, high intensity and rigidity etc..Due to these excellent properties, graphene can individually make in many application fields
With or by hydridization or composition metal and semiconductor.It has been widely studied the electrode addition material as lithium ion battery
Material.
CNT and the dilute representative as new c-based nanomaterial of graphite, with excellent electronic conduction characteristic and spy
Different one-dimensional or two-dimension flexible structure, is mutually combined with Different electrodes material, can effectively improve specific capacity, the high power of active material
Rate discharge performance and cycle performance.However, the high rate performance for the electrode material that such carbon nanomaterial is individually modified still is carried
It is high limited, because one-dimensional CNT is difficult to form effective contiguous network structure, limit electrode contact.On the other hand,
Graphite is dilute to be difficult to wind around on the surface of positive electrode, and the electrochemistry for being unfavorable for improving positive electrode in a way is lived
Property.Therefore needing further optimization improves.
The content of the invention
The purpose of the present invention aims to provide a kind of graphene/carbon nano-tube composite conducting slurry and preparation method thereof, graphite
Alkene/CNT is compound it is possible to prevente effectively from graphene is used alone or the problem of CNT is present is used alone, collaboration changes
The electric conductivity of kind electrode.
To achieve these goals, the present invention uses following technical scheme：
A kind of graphene/carbon nano-tube composite conducting slurry, the composite conducting slurry is according to the composition of mass fraction component：
1.5-3.0% graphene, 3.0-8.0% CNT, the solvent of 0.3-0.8% dispersant and remaining proportion, wherein scattered
Agent is nonionic surface active agent, and solvent is 1-METHYLPYRROLIDONE.
A kind of graphene/carbon nano-tube composite conducting slurry preparation method, the preparation method comprises the following steps：
（1）Dispersant is dissolved in 1-METHYLPYRROLIDONE solvent in stirring dispersion machine and turned with rotation 1000-1500/
Min, 20-35 turns/min of revolution speed is stirred under vacuum；
（2）Mass fraction component 3.0-8.0% CNT is added ,/min is turned with rotation 1500-2000 in mixer, it is public
Pre-dispersed carbon nano tube paste is made in the speed progress vacuum high-speed stirred for turning 35-45 turns/min；
（3）Above-mentioned carbon nano tube paste is all transferred in the sand mill with zirconium pearl and is ground dispersed ultrafine, rotating speed 1500-
2500 turns/min, zirconium oxide abrasive pearl size is unlatching cooling circulating water cooling in 0.8-1.0mm, process of lapping, obtains ultra-fine
Scattered carbon nanotube conducting agent slurry；
（4）Mass fraction component 1.5-3.0% graphene is added toward above-mentioned carbon nanotube conducting agent slurry, with rotating speed 1500-
Cooling circulating water cooling is opened in 2500 turns/min grinding distributions, process of lapping, the graphene/carbon nano-tube of dispersed ultrafine is obtained
Composite conducting slurry.
As preferred, dispersant is polyvinyl alcohol in a kind of graphene/carbon nano-tube composite conducting slurry.
The beneficial effects of the invention are as follows：（1）In the graphene/carbon nano-tube composite conducting slurry preparation method of the present invention
First CNT is carried out pre-dispersed, then carry out the composite diffusion of graphene, scattered CNT can effectively be kept away in advance
Exempt from issuable reunion packing phenomenon during graphene dispersion, form the uniform and stable composite conducting slurry of dispersed ultrafine.
（2）The point and one-dimensional wire and two itself at CNT two ends in the graphene/carbon nano-tube composite conducting slurry of the present invention
Tie up sheet graphene constitute three-dimensional network conductive structure, anode and cathode slurry prepare during can effectively with both positive and negative polarity
Active material formation honeycomb-like network conductive structure, significantly improves the electric conductivity of positive and negative pole material, so as to improve electricity
Rapid charge characteristic, the high rate performance in pond, can also improve the cycle performance and security performance of battery.The graphene of the present invention/
CNT composite conducting slurry preparation method is simple, is suitable for large-scale industrial production.
Embodiment
To make those skilled in the art more fully understand the present invention program, the present invention is made with reference to embodiment
It is described in further detail.
Embodiment 1：
The composite conducting slurry of embodiment 1 is according to the composition of mass fraction component：3.0% graphene, 8.0% carbon nanometer
The 1-METHYLPYRROLIDONE solvent of pipe, 0.8% polyvinyl alcohol and remaining proportion.The preparation method of the composite conducting slurry includes
Following steps：
（1）Dispersant is dissolved in 1-METHYLPYRROLIDONE solvent and with 1500 turns/min of rotation in stirring dispersion machine, it is public
The speed for turning 35 turns/min is stirred under vacuum；
（2）The CNT of mass fraction component 8.0% is added, with 2000 turns/min of rotation in mixer, revolve round the sun 45 turns/min
Speed carry out vacuum high-speed stirred pre-dispersed carbon nano tube paste is made；
（3）Above-mentioned carbon nano tube paste is all transferred in the sand mill with zirconium pearl and is ground dispersed ultrafine, rotating speed 2500
Turn/min, zirconium oxide abrasive pearl size is unlatching cooling circulating water cooling in 0.8mm, process of lapping, obtains the carbon of dispersed ultrafine
Nanotube conductive agent slurry；
（4）The graphene of mass fraction component 3.0% is added toward above-mentioned carbon nanotube conducting agent slurry, with 2500 turns/min of rotating speed
Cooling circulating water cooling is opened in grinding distribution, process of lapping, the graphene/carbon nano-tube composite guide plasma-based of dispersed ultrafine is obtained
Material.
Embodiment 2：
The composite conducting slurry of embodiment 2 is according to the composition of mass fraction component：1.5% graphene, 3.0% carbon nanometer
The 1-METHYLPYRROLIDONE solvent of pipe, 0.3% polyvinyl alcohol and remaining proportion.The preparation method of the composite conducting slurry includes
Following steps：
（1）Dispersant is dissolved in 1-METHYLPYRROLIDONE solvent and with 1000 turns/min of rotation in stirring dispersion machine, it is public
The speed for turning 20 turns/min is stirred under vacuum；
（2）The CNT of mass fraction component 3.0% is added, with 1500 turns/min of rotation in mixer, revolve round the sun 35 turns/min
Speed carry out vacuum high-speed stirred pre-dispersed carbon nano tube paste is made；
（3）Above-mentioned carbon nano tube paste is all transferred in the sand mill with zirconium pearl and is ground dispersed ultrafine, rotating speed 1500
Turn/min, zirconium oxide abrasive pearl size is unlatching cooling circulating water cooling in 1.0mm, process of lapping, obtains the carbon of dispersed ultrafine
Nanotube conductive agent slurry；
（4）The graphene of mass fraction component 1.5% is added toward above-mentioned carbon nanotube conducting agent slurry, with 1500 turns/min of rotating speed
Cooling circulating water cooling is opened in grinding distribution, process of lapping, the graphene/carbon nano-tube composite guide plasma-based of dispersed ultrafine is obtained
Material.
Embodiment 3：
The composite conducting slurry of embodiment 3 is according to the composition of mass fraction component：2.0% graphene, 5.0% carbon nanometer
The 1-METHYLPYRROLIDONE solvent of pipe, 0.5% polyvinyl alcohol and remaining proportion.The preparation method of the composite conducting slurry includes
Following steps：
（1）Dispersant is dissolved in 1-METHYLPYRROLIDONE solvent and with 1200 turns/min of rotation in stirring dispersion machine, it is public
The speed for turning 30 turns/min is stirred under vacuum；
（2）The CNT of mass fraction component 5.0% is added, with 1800 turns/min of rotation in mixer, revolve round the sun 40 turns/min
Speed carry out vacuum high-speed stirred pre-dispersed carbon nano tube paste is made；
（3）Above-mentioned carbon nano tube paste is all transferred in the sand mill with zirconium pearl and is ground dispersed ultrafine, rotating speed 2000
Turn/min, zirconium oxide abrasive pearl size is unlatching cooling circulating water cooling in 0.9mm, process of lapping, obtains the carbon of dispersed ultrafine
Nanotube conductive agent slurry；
（4）The graphene of mass fraction component 2.0% is added toward above-mentioned carbon nanotube conducting agent slurry, with 2000 turns/min of rotating speed
Cooling circulating water cooling is opened in grinding distribution, process of lapping, the graphene/carbon nano-tube composite guide plasma-based of dispersed ultrafine is obtained
Material.
The present invention graphene/carbon nano-tube composite conducting slurry preparation method in first CNT is carried out it is pre-dispersed,
The composite diffusion of graphene is carried out again, and scattered CNT may production during being effectively prevented from graphene dispersion in advance
Raw reunion packing phenomenon, forms the uniform and stable composite conducting slurry of dispersed ultrafine；The graphene/carbon nano-tube of the present invention is answered
The graphene composition three-dimensional network for closing the point at CNT two ends and one-dimensional wire itself and two-dimensional sheet in electrocondution slurry is led
Electric structure, effectively can be tied during prepared by anode and cathode slurry with both positive and negative polarity active material formation honeycomb-like network conduction
Structure, significantly improves the electric conductivity of positive and negative pole material, so that the rapid charge characteristic of battery, high rate performance are improved,
The cycle performance and security performance of battery can be improved.The graphene/carbon nano-tube composite conducting slurry preparation method of the present invention
Simply, it is suitable for large-scale industrial production.
It should be appreciated that the foregoing is only the preferred embodiments of the present invention, the technology of the limitation present invention is e insufficient to
Scheme, for those of ordinary skills, within the spirit and principles in the present invention, can be increased according to the above description
Subtract, replace, convert or improve, and the technical scheme after all these increases and decreases, replacement, conversion or improvement, it should all belong to the present invention
The scope of technical characteristic, is included within protection scope of the present invention.
Claims (3)
1. a kind of graphene/carbon nano-tube composite conducting slurry, it is characterised in that described composite conducting slurry is according to quality point
The composition of array point is：1.5-3.0% graphene, 3.0-8.0% CNT, 0.3-0.8% dispersant and remaining proportion
Solvent, wherein dispersant be nonionic surface active agent, solvent is 1-METHYLPYRROLIDONE.
2. a kind of graphene/carbon nano-tube composite conducting slurry preparation method, it is characterised in that the preparation method includes following step
Suddenly：
（1）Dispersant is dissolved in 1-METHYLPYRROLIDONE solvent in stirring dispersion machine and turned with rotation 1000-1500/
Min, 20-35 turns/min of revolution speed is stirred under vacuum；
（2）Whole CNTs are added according to proportioning described in claim 1, turned in mixer with rotation 1500-2000/
Min, 35-45 turns/min of revolution speed carry out vacuum high-speed stirred and pre-dispersed carbon nano tube paste are made；
（3）Above-mentioned carbon nano tube paste is all transferred in the sand mill with zirconium pearl and is ground dispersed ultrafine, rotating speed 1500-
2500 turns/min, zirconium oxide abrasive pearl size is unlatching cooling circulating water cooling in 0.8-1.0mm, process of lapping, obtains ultra-fine
Scattered carbon nanotube conducting agent slurry；
（4）The graphene matched described in claim 1 is added toward above-mentioned carbon nanotube conducting agent slurry, with rotating speed 1500-2500
Turn to open cooling circulating water cooling in/min grinding distributions, process of lapping, the graphene/carbon nano-tube for obtaining dispersed ultrafine is combined
Electrocondution slurry.
3. a kind of graphene/carbon nano-tube composite conducting slurry according to claim 1, it is characterised in that dispersant is poly-
Vinyl alcohol.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108062999A (en) * | 2017-12-25 | 2018-05-22 | 新奥（内蒙古）石墨烯材料有限公司 | The method for preparing electrocondution slurry |
| CN108470914A (en) * | 2018-06-05 | 2018-08-31 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of graphene complex lithium electricity electrocondution slurry |
| CN108550856A (en) * | 2018-05-23 | 2018-09-18 | 山东希诚新材料科技有限公司 | Carbon nano tube/graphene composite conducting slurry and preparation method thereof |
| CN108822607A (en) * | 2018-04-11 | 2018-11-16 | 杭州牛墨科技有限公司 | A kind of manufactured preparation method for absorbing static electricity heating slurry of graphene carbon nanotube |
| CN109360977A (en) * | 2018-12-05 | 2019-02-19 | 江西赛特新能源科技有限公司 | A kind of preparation method of resistance to ultralow temperature cylindrical lithium ion battery |
| CN109575456A (en) * | 2018-10-26 | 2019-04-05 | 福建师范大学 | A kind of preparation method of multi-component hybridization anisotropy thermal diffusion film |
| CN109637697A (en) * | 2018-12-24 | 2019-04-16 | 广东省稀有金属研究所 | A kind of graphene conductive slurry and preparation method thereof |
| CN109841420A (en) * | 2018-12-26 | 2019-06-04 | 谢春艳 | Novel super capacitor carbon nano-onions conductive agent slurry and its supercapacitor |
| CN110111924A (en) * | 2019-05-24 | 2019-08-09 | 浙江王点科技有限公司 | A kind of graphene quantum dot and single-walled carbon nanotube composite conducting slurry and preparation method |
| CN110228805A (en) * | 2019-07-24 | 2019-09-13 | 西南交通大学 | Redox graphene/carbon nano tube compound material and preparation method thereof |
| CN110247051A (en) * | 2019-05-29 | 2019-09-17 | 常熟理工学院 | A kind of carbon nanotube mill base and preparation method thereof and the application in lithium battery |
| CN111370160A (en) * | 2020-03-27 | 2020-07-03 | 苏州聚龙能源科技有限公司 | Graphene-based conductive paste |
| CN112447969A (en) * | 2019-09-04 | 2021-03-05 | 深圳市拓邦锂电池有限公司 | Water-based positive electrode slurry of lithium iron phosphate battery and preparation method thereof |
| CN112898812A (en) * | 2021-02-05 | 2021-06-04 | 东莞市中科智恒新材料有限公司 | Far infrared quartz tube applied to electronic cigarette heater and preparation method thereof |
| CN113035407A (en) * | 2021-02-27 | 2021-06-25 | 河南克莱威纳米碳材料有限公司 | High-conductivity and high-stability carbon nanotube compound conductive slurry for lithium ion battery and preparation method thereof |
| CN114388791A (en) * | 2020-10-22 | 2022-04-22 | 山东海科创新研究院有限公司 | Composite slurry for lithium ion battery, preparation method and application thereof |
| CN114976001A (en) * | 2022-04-27 | 2022-08-30 | 广东一纳科技有限公司 | Composite conductive powder, preparation method thereof and lithium battery |
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| CN108062999A (en) * | 2017-12-25 | 2018-05-22 | 新奥（内蒙古）石墨烯材料有限公司 | The method for preparing electrocondution slurry |
| CN108822607A (en) * | 2018-04-11 | 2018-11-16 | 杭州牛墨科技有限公司 | A kind of manufactured preparation method for absorbing static electricity heating slurry of graphene carbon nanotube |
| CN108550856A (en) * | 2018-05-23 | 2018-09-18 | 山东希诚新材料科技有限公司 | Carbon nano tube/graphene composite conducting slurry and preparation method thereof |
| CN108470914A (en) * | 2018-06-05 | 2018-08-31 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of graphene complex lithium electricity electrocondution slurry |
| CN109575456A (en) * | 2018-10-26 | 2019-04-05 | 福建师范大学 | A kind of preparation method of multi-component hybridization anisotropy thermal diffusion film |
| CN109575456B (en) * | 2018-10-26 | 2022-04-26 | 福建师范大学 | Preparation method of multi-element hybrid anisotropic thermal diffusion film |
| CN109360977A (en) * | 2018-12-05 | 2019-02-19 | 江西赛特新能源科技有限公司 | A kind of preparation method of resistance to ultralow temperature cylindrical lithium ion battery |
| CN109637697A (en) * | 2018-12-24 | 2019-04-16 | 广东省稀有金属研究所 | A kind of graphene conductive slurry and preparation method thereof |
| CN109841420A (en) * | 2018-12-26 | 2019-06-04 | 谢春艳 | Novel super capacitor carbon nano-onions conductive agent slurry and its supercapacitor |
| CN110111924A (en) * | 2019-05-24 | 2019-08-09 | 浙江王点科技有限公司 | A kind of graphene quantum dot and single-walled carbon nanotube composite conducting slurry and preparation method |
| CN110247051A (en) * | 2019-05-29 | 2019-09-17 | 常熟理工学院 | A kind of carbon nanotube mill base and preparation method thereof and the application in lithium battery |
| CN110228805B (en) * | 2019-07-24 | 2021-04-16 | 西南交通大学 | Reduced graphene oxide/carbon nanotube composite material and preparation method thereof |
| CN110228805A (en) * | 2019-07-24 | 2019-09-13 | 西南交通大学 | Redox graphene/carbon nano tube compound material and preparation method thereof |
| CN112447969A (en) * | 2019-09-04 | 2021-03-05 | 深圳市拓邦锂电池有限公司 | Water-based positive electrode slurry of lithium iron phosphate battery and preparation method thereof |
| CN111370160A (en) * | 2020-03-27 | 2020-07-03 | 苏州聚龙能源科技有限公司 | Graphene-based conductive paste |
| CN111370160B (en) * | 2020-03-27 | 2021-09-28 | 苏州聚龙能源科技有限公司 | Graphene-based conductive paste |
| CN114388791A (en) * | 2020-10-22 | 2022-04-22 | 山东海科创新研究院有限公司 | Composite slurry for lithium ion battery, preparation method and application thereof |
| CN114388791B (en) * | 2020-10-22 | 2023-07-14 | 山东海科创新研究院有限公司 | Composite slurry for lithium ion battery, preparation method and application thereof |
| CN112898812A (en) * | 2021-02-05 | 2021-06-04 | 东莞市中科智恒新材料有限公司 | Far infrared quartz tube applied to electronic cigarette heater and preparation method thereof |
| CN113035407A (en) * | 2021-02-27 | 2021-06-25 | 河南克莱威纳米碳材料有限公司 | High-conductivity and high-stability carbon nanotube compound conductive slurry for lithium ion battery and preparation method thereof |
| CN114976001A (en) * | 2022-04-27 | 2022-08-30 | 广东一纳科技有限公司 | Composite conductive powder, preparation method thereof and lithium battery |
| CN114976001B (en) * | 2022-04-27 | 2024-03-19 | 广东一纳科技有限公司 | Composite conductive powder, preparation method thereof and lithium battery |
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|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 518105 4th Floor, Building A2, Liyuan Bay Industrial Park, 168 Honghu Road, Yanchuan, Songgang, Baoan District, Shenzhen City, Guangdong Province Applicant after: Shenzhen Greende Energy Group Co., Ltd. Address before: 518105 4th Floor, Building A2, Liyuan Bay Industrial Park, 168 Honghu Road, Yanchuan, Songgang, Baoan District, Shenzhen City, Guangdong Province Applicant before: Shenzhen Green's moral limited energy company |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171103 |