CN105845915B - A kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material - Google Patents
A kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material Download PDFInfo
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- H01M4/00—Electrodes
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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
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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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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- H01M4/58—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
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Abstract
A kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material, it is using plant parenchymal tissue as biomass carbon raw material, it handles to obtain the presoma of pre- carbonization by acid soak, presoma is mixed and is fully ground with alkali afterwards, heat treatment obtains three-dimensional porous carbon skeleton in tube furnace, this three-dimensional porous carbon skeleton is immersed in the solution containing cobalt salt again, then it filters and is dried, it is finally putting into heat treatment in tube furnace and obtains the compound of three-dimensional porous carbon skeleton load C oO, the compound, which is applied to lithium ion battery, has good cycle performance and high rate performance；Plant parenchymal tissue is that the porous carbon skeleton of biomass carbon raw material preparation has the load of stable structural support CoO；The porous carbon skeleton of the available different pore size distribution of additional amount by controlling urea；Porous carbon skeleton can not only stablize the structure of CoO, while the electric conductivity for also improving CoO accelerates the transmission rate of electronics, and electrochemical reaction is accelerated, and be conducive to the promotion of high rate performance.
Description
Technical field
The present invention relates to a kind of preparation method of three-dimensional porous carbon skeleton load oxide lithium ion battery negative material, tools
Body is related to a kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material.
Background technique
With the continuous development and update of electronic product of new generation and electric car, mention people to performance of lithium ion battery
Higher requirement is gone out, developing novel, cheap negative electrode material becomes one of the hot subject of Study on Li-ion batteries.Transition gold
Belong to material oxide CoO due to theoretical capacity with higher (715mAh/g) and become the hot spot studied recently, but CoO is certainly
Body poorly conductive and the volume expansion occurred in charge and discharge process limit its practical application.It solves these problems at present main
Method be the reasonable nanostructure of design or carry out compound [Yongming Sun, Xianluo Hu, Wei with other substances
Luo,and Yunhui Huang.Ultrathin CoO/Graphene Hybrid Nanosheets:A Highly Stable
Anode Material for Lithium-Ion Batteries[J].The Journal of Physical Chemistry
C,2012,116:20794-20799.].It is compound with carbons substance to be more effectively and simple method, wherein biomass carbon is
A kind of active carbonizable substance, and biological material is from a wealth of sources cheap is easier to accomplish scale production.?
It has been reported that with microalgae [Haohui Ru, Ningbo Bai, Kaixiong Xiang, et.al.Porous carbons derived
from microalgae with enhanced electrochemical performance for lithium-ion
Batteries [J] .Electrochimica Acta, 2016,194:10-16.], pomelo peel [Jun Zhang, Jiayuan
Xiang,Zimin Dong,et.al.Biomass derived activated carbon with 3D connected
architecture fo rechargeable lithium-sulfur batteries[J].Electrochimica Acta,
2014,116:146-151.], soybean residue [Feng Chen, Juan Yang, Tao Bai, et.al.Biomass waste-
derived honeycomb-like nitrogen and oxygen dual-doped porous carbon for high
performance lithium-sulfur batteries[J].Electrochimica Acta,2016,192:99-109.]
Biomass carbon negative electrode material is obtained Deng for raw material.The porous or fibr tissue that biomass itself has is to the porous carbon bone of formation
It is helpful for frame.It also to biomass carbon is favorably simultaneously matrix and the compound example of oxide, such as Jiafeng
Wu[Haohui Ru,Ningbo Bai,Kaixiong Xiang,et.al.Porous carbons derived from
microalgae with enhanced electrochemical performance for lithium-ion
Batteries [J] .Electrochimica Acta, 2016,194:10-16.] etc. be successfully prepared multiporous biological matter carbon load
Co3O4Negative electrode material, [Haiyan Wang, Dayong Ren, the Zhengju Zhu, et.al.Few-layer such as Haiyan Wang
MoS2nanosheets incorporated into hierarchical porous carbon for lithium-ion
Batteries [J] .2016,288:179-184.] it is prepared for classifying porous biomass carbon and MoS2Compound as lithium ion
Cell negative electrode material.But the aperture for loading the multiporous biological matter carbon of oxide is all bigger, this makes the specific surface of material itself
Product it is smaller, load oxide amount can also compare it is less.
Summary of the invention
The purpose of the present invention is to provide a kind of three-dimensional porous carbon skeleton with good cycle performance and high rate performance/
The preparation method of CoO negative pole of lithium ion battery with compound structure material.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of three-dimensional porous carbon skeleton/CoO composite construction
The preparation method of lithium ion battery negative material,
1) by plant parenchymal tissue raw material cleaning, drying；
2) the plant parenchymal tissue of 3~6g is taken to be put into the 60ml concentrated sulfuric acid solution that concentration is 5~10mol/L, in 80 DEG C
5~7h is reacted in baking oven, obtains suspending liquid A；
3) suspending liquid A is filtered by vacuum, and is rinsed with deionized water to pH=7, then collected and be dried to obtain forerunner
Object B；
4) predecessor B is mixed with potassium hydroxide 1:1~1:3 in mass ratio and is ground and uniformly obtain product C；
5) it is 700~900 DEG C that product C is put into setting reaction temperature in the tube furnace for be connected with argon gas, keeps the temperature 1~3h, rises
Warm rate is 3~10 DEG C of min-1, 0~0.5sccmmin of argon air-flow velocity-1, obtain product D；
6) the analytically pure four acetate hydrates cobalt of 0.02mol, 0.06~0.08mol urea is taken to be added to 100ml deionized water
In, the product D of 1~2g is put into solution after mixing evenly, 80 DEG C of dryings 12 after 12~18h of magnetic agitation at 60~80 DEG C
~18h obtains compound precursor object E；
7) compound precursor object E is put into the tube furnace for being passed through argon atmosphere, setting reaction temperature is 350~550 DEG C, is protected
0.5~2h of temperature, heating rate are 3~10 DEG C of min-1, 0~0.5sccmmin of argon air-flow velocity-1, obtain three-dimensional porous carbon
Skeleton/CoO negative pole of lithium ion battery with compound structure material.
The plant parenchymal tissue material is peanut skin, garlic skin or onion skin.
The present invention is handled using the thin wall types such as peanut skin, garlic skin, onion skin plant tissue as biomass carbon raw material by acid soak
Obtain the presoma of pre- carbonization, after presoma is mixed in a certain ratio and is fully ground with alkali, be heat-treated in tube furnace
It is immersed in the solution containing cobalt salt to three-dimensional porous carbon skeleton, then by this three-dimensional porous carbon skeleton, then filters and done
It is dry, be finally putting into heat treatment in tube furnace and obtain the compound of three-dimensional porous carbon skeleton load C oO, the compound be applied to lithium from
Sub- battery has good cycle performance and high rate performance.
1) present invention is prepared porous using the various plants such as peanut skin, garlic skin, onion skin parenchymal tissue as biomass carbon raw material
Carbon skeleton has the load of stable structural support CoO；
2) pass through the porous carbon skeleton of the available different pore size distribution of the additional amount of control urea；
3) porous carbon skeleton can not only stablize the load of CoO, while the electric conductivity for also improving CoO makes electronics
Transmission rate is accelerated, and electrochemical reaction is accelerated, and is conducive to the promotion of high rate performance.
Detailed description of the invention
Fig. 1 is three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material prepared by the embodiment of the present invention 1
XRD diagram.
Three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material prepared by Fig. 2 embodiment of the present invention 1 exists
The cycle performance figure of 50 circle of circulation under the current density of 100mA/g.
Specific embodiment
Embodiment 1: a kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by peanut skin cleaning, drying；
2) it takes the peanut skin of 3g to be put into the 60ml concentrated sulfuric acid solution that concentration is 5mol/L, reacts 5h in 80 DEG C of baking ovens,
Obtain suspending liquid A；
3) suspending liquid A is filtered by vacuum, and is rinsed with deionized water to pH=7, then collected and be dried to obtain forerunner
Object B；
4) predecessor B is mixed with potassium hydroxide 1:1 in mass ratio and is ground and uniformly obtain product C；
5) it is 800 DEG C that product C is put into setting reaction temperature in the tube furnace for be connected with argon gas, keeps the temperature 2h, heating rate 3
℃·min-1, argon air-flow velocity 0.2sccmmin-1, obtain product D；
6) it takes the analytically pure four acetate hydrates cobalt of 0.02mol, 0.06mol urea to be added in 100ml deionized water, stirs
The product D of 1g is put into solution after uniformly, 80 DEG C of dry 12h obtain compound precursor object E after magnetic agitation 12h at 60 DEG C；
7) compound precursor object E being put into the tube furnace for being passed through argon atmosphere, setting reaction temperature is 350 DEG C, 2h is kept the temperature,
Heating rate is 3 DEG C of min-1, argon air-flow velocity 0.4sccmmin-1, obtain three-dimensional porous carbon skeleton/CoO composite construction lithium
Ion battery cathode material.
By Fig. 1 it can be seen that the CoO in obtained three-dimensional porous carbon skeleton/CoO compound is pure phase, does not see and take office
It is undefined structure that the characteristic peak of what carbon, which is possible as obtained porous carbon,.
Three-dimensional porous carbon skeleton/CoO compound has good cycle performance as seen from Figure 2, with cycle-index
Increase capacity also gradually increasing and tending towards stability.
Embodiment 2: a kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by garlic skin cleaning, drying；
2) it takes the garlic skin of 4g to be put into the 60ml concentrated sulfuric acid solution that concentration is 7mol/L, reacts 7h in 80 DEG C of baking ovens, obtain
To suspending liquid A；
3) suspending liquid A is filtered by vacuum, and is rinsed with deionized water to pH=7, then collected and be dried to obtain forerunner
Object B；
4) predecessor B is mixed with potassium hydroxide 1:2 in mass ratio and is ground and uniformly obtain product C；
5) it is 700 DEG C that product C is put into setting reaction temperature in the tube furnace for be connected with argon gas, keeps the temperature 3h, heating rate 5
℃·min-1, argon air-flow velocity 0.5sccmmin-1, obtain product D；
6) it takes the analytically pure four acetate hydrates cobalt of 0.02mol, 0.08mol urea to be added in 100ml deionized water, stirs
The product D of 1.5g is put into solution after uniformly, 80 DEG C of dry 14h obtain compound precursor object after magnetic agitation 14h at 70 DEG C
E；
7) compound precursor object E is put into the tube furnace for being passed through argon atmosphere, setting reaction temperature is 500 DEG C, heat preservation
1.5h, heating rate are 5 DEG C of min-1, argon air-flow velocity 0.3sccmmin-1, it is compound to obtain three-dimensional porous carbon skeleton/CoO
Structure lithium ion battery negative electrode material.
Embodiment 3: a kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by onion skin cleaning, drying；
2) it takes the onion skin of 6g to be put into the 60ml concentrated sulfuric acid solution that concentration is 10mol/L, reacts 6h in 80 DEG C of baking ovens, obtain
To suspending liquid A；
3) suspending liquid A is filtered by vacuum, and is rinsed with deionized water to pH=7, then collected and be dried to obtain forerunner
Object B；
4) predecessor B is mixed with potassium hydroxide 1:3 in mass ratio and is ground and uniformly obtain product C；
5) it is 900 DEG C that product C is put into setting reaction temperature in the tube furnace for be connected with argon gas, keeps the temperature 1h, heating rate 8
℃·min-1, argon air-flow velocity 0.4sccmmin-1, obtain product D；
6) it takes the analytically pure four acetate hydrates cobalt of 0.02mol, 0.07mol urea to be added in 100ml deionized water, stirs
The product D of 2g is put into solution after uniformly, 80 DEG C of dry 16h obtain compound precursor object E after magnetic agitation 16h at 80 DEG C；
7) compound precursor object E being put into the tube furnace for being passed through argon atmosphere, setting reaction temperature is 500 DEG C, 1h is kept the temperature,
Heating rate is 8 DEG C of min-1, argon air-flow velocity 0.5sccmmin-1, obtain three-dimensional porous carbon skeleton/CoO composite construction lithium
Ion battery cathode material.
Embodiment 4: a kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by peanut skin cleaning, drying；
2) it takes the peanut skin of 5g to be put into the 60ml concentrated sulfuric acid solution that concentration is 9mol/L, reacts 7h in 80 DEG C of baking ovens,
Obtain suspending liquid A；
3) suspending liquid A is filtered by vacuum, and is rinsed with deionized water to pH=7, then collected and be dried to obtain forerunner
Object B；
4) predecessor B is mixed with potassium hydroxide 1:1.5 in mass ratio and is ground and uniformly obtain product C；
5) product C is put into setting reaction temperature in tube furnace is 850 DEG C, keeps the temperature 1.5h, and heating rate is 10 DEG C
min-1Obtain product D；
6) it takes the analytically pure four acetate hydrates cobalt of 0.02mol, 0.08mol urea to be added in 100ml deionized water, stirs
The product D of 1.8g is put into solution after uniformly, 80 DEG C of dry 18h obtain compound precursor object after magnetic agitation 18h at 65 DEG C
E；
7) compound precursor object E is put into tube furnace, setting reaction temperature is 550 DEG C, keeps the temperature 0.5h, heating rate 10
℃·min-1, obtain three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material.
Claims (1)
1. a kind of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material preparation method, it is characterised in that:
1) by plant parenchymal tissue raw material cleaning, drying, the plant parenchymal tissue raw material is peanut skin, garlic skin or onion skin；
2) the plant parenchymal tissue of 3~6g is taken to be put into the 60ml concentrated sulfuric acid solution that concentration is 5~10mol/L, in 80 DEG C of baking ovens
5~7h of middle reaction, obtains suspending liquid A；
3) suspending liquid A is filtered by vacuum, and is rinsed with deionized water to pH=7, then collected and be dried to obtain predecessor B；
4) predecessor B is mixed with potassium hydroxide 1:1~1:3 in mass ratio and is ground and uniformly obtain product C；
5) it is 700~900 DEG C that product C is put into setting reaction temperature in the tube furnace for be connected with argon gas, keeps the temperature 1~3h, heating speed
Rate is 3~10 DEG C of min-1, 0~0.5cm of argon air-flow velocity3·min-1, obtain product D；
6) it takes the analytically pure four acetate hydrates cobalt of 0.02mol, 0.06~0.08mol urea to be added in 100ml deionized water, stirs
The product D of 1~2g is put into solution after mixing uniformly, 80 DEG C of dry 12~18h after 12~18h of magnetic agitation at 60~80 DEG C
Obtain compound precursor object E；
7) compound precursor object E is put into the tube furnace for being passed through argon atmosphere, setting reaction temperature is 350~550 DEG C, heat preservation
0.5~2h, heating rate are 3~10 DEG C of min-1, 0~0.5cm of argon air-flow velocity3·min-1, obtain three-dimensional porous carbon skeleton/
CoO negative pole of lithium ion battery with compound structure material.
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| CN107039193B (en) * | 2017-04-14 | 2018-10-19 | 山东大学 | A kind of garlic skin matrix activated carbon electrode material and preparation method for ultracapacitor |
| CN107591250B (en) * | 2017-09-12 | 2019-06-28 | 桂林电子科技大学 | A kind of porous carbon composite and its preparation method and application of CoO- N doping |
| CN107611435A (en) * | 2017-09-13 | 2018-01-19 | 陕西科技大学 | A kind of method that three-dimensional porous sodium-ion battery carbon material used as anode is prepared based on peanut coat |
| CN108649201B (en) * | 2018-05-08 | 2021-01-01 | 宁波大学 | LaTi21O38·CoO·CuLaO2Preparation method of composite nanowire |
| CN108557797B (en) * | 2018-05-25 | 2021-07-20 | 上海应用技术大学 | Cobalt-doped porous carbon material and preparation method thereof |
| CN110429247A (en) * | 2019-07-05 | 2019-11-08 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery three-dimensional ZnO/C composite negative pole material and preparation method thereof |
| CN110415986B (en) * | 2019-07-12 | 2021-05-18 | 江苏理工学院 | Ni-doped CoO/C composite material and preparation method thereof |
| CN110931798B (en) * | 2019-12-12 | 2020-10-09 | 哈尔滨理工大学 | Preparation method of 3DPC/Co/CoO lithium battery negative electrode material |
| CN113387396B (en) * | 2021-06-11 | 2023-09-19 | 郑州大学 | Biomass carbon electrode composite material and preparation method and application thereof |
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