CN105845915A - Method for preparing anode material of three-dimensional porous carbon skeleton/CoO composite structured lithium ion battery - Google Patents
Method for preparing anode material of three-dimensional porous carbon skeleton/CoO composite structured lithium ion battery Download PDFInfo
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- CN105845915A CN105845915A CN201610375905.6A CN201610375905A CN105845915A CN 105845915 A CN105845915 A CN 105845915A CN 201610375905 A CN201610375905 A CN 201610375905A CN 105845915 A CN105845915 A CN 105845915A
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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
- H01M4/362—Composites
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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
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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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
- H01M4/58—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
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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 relates to a method for preparing an anode material of a three-dimensional porous carbon skeleton/CoO composite structured lithium ion battery. Parenchymatous tissue of plants is used as the biomass carbon material; the biomass carbon material is immersed through acid, such that a pre-carbonized precursor is obtained; then, the precursor and alkali are mixed and sufficiently grinded, and then thermally treated in a tube furnace, such that a three-dimensional porous carbon skeleton is obtained; the three-dimensional porous carbon skeleton is immersed in solution including cobalt salt; then, suction filtration and drying are carried out; and finally, the mixture is thermally treated in the tube furnace, such that a CoO loaded three-dimensional porous carbon skeleton composite is obtained. The composite is applied to the lithium ion battery, such that the lithium ion battery has good cycle performance and rate performance; the porous carbon skeleton, prepared by using the parenchymatous tissue of plants as the biomass carbon material, has a steady structure for supporting load of CoO; the porous carbon skeleton having different pore diameters can be obtained by controlling the addition amount of urea; due to the porous carbon skeleton, the CoO structure can be stabilized; simultaneously, the electrical conductivity of CoO is also improved; therefore, the electron transmission rate is increased; the electrochemical reaction is accelerated; and the rate performance is improved easily.
Description
Technical field
The present invention relates to the preparation method of a kind of three-dimensional porous carbon skeleton load oxide lithium ion battery negative material, tool
Body relates to the preparation method of a kind of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material.
Background technology
Along with a new generation's electronic product and the development of electric automobile and renewal, make people that performance of lithium ion battery to be carried
Go out higher requirement, develop one of novel, cheap negative material hot subject becoming Study on Li-ion batteries.
Transition metal material oxide CoO becomes research recently owing to having higher theoretical capacity (715mAh/g)
Focus, but CoO self-conductive difference and the volumetric expansion occurred in charge and discharge process limit its actual application.
Solve the main method of these problems at present to be nanostructured reasonable in design or be combined with other materials
[Yongming Sun,Xianluo Hu,Wei 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.].Compound with carbons material is more effectively with simple
Method, wherein, biomass carbon is a kind of active carbonizable substance, and biological material wide material sources are cheap
It is easier to accomplish scale production.Had 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.], Semen Glycines slag [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.] etc. obtain biomass for raw material
Carbon negative pole material.Porous or fibrous tissue that biomass self have are to have very much side for forming the carbon skeleton of porous
Help.Be the most favorably simultaneously matrix and the compound example of oxide in order to biomass carbon, 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 C o3O4Negative material, Haiyan Wang etc. [Haiyan Wang,
Dayong Ren,Zhengju Zhu,et.al.Few-layer MoS2nanosheets incorporated into hierarchical
Porous carbon for lithium-ion batteries [J] .2016,288:179-184.] it is prepared for classifying porous biomass carbon
And MoS2Complex as lithium ion battery negative material.But the aperture of the multiporous biological matter carbon of load oxide is all
Bigger, this makes the specific surface area of material itself smaller, and the amount of load oxide also can compare less.
Summary of the invention
It is an object of the invention 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.
For reaching above-mentioned purpose, the technical solution used in the present invention is: a kind of three-dimensional porous carbon skeleton/CoO composite junction
The preparation method of structure lithium ion battery negative material,
1) by plant parenchyma raw material cleaning, drying；
2) the plant parenchyma taking 3～6g is put in the 60ml concentrated sulfuric acid solution that concentration is 5～10mol/L, in
80 DEG C of baking ovens react 5～7h, obtains suspending liquid A；
3) suspending liquid A is carried out vacuum filtration, and with deionized water rinsing to pH=7, then collect before being dried to obtain
Drive thing B；
4) predecessor B is mixed with potassium hydroxide 1:1～1:3 in mass ratio and grinds uniformly obtain product C；
5) product C is put into that be connected with the tube furnace of argon to arrange reaction temperature be 700～900 DEG C, is incubated 1～3h,
Heating rate is 3～10 DEG C of min-1, argon air-flow velocity 0～0.5sccm min-1, obtain product D；
6) take the analytically pure four acetate hydrate cobalts of 0.02mol, 0.06～0.08mol carbamide and join 100ml deionization
In water, after stirring, the product D of 1～2g is put in solution, magnetic agitation 12～18h at 60～80 DEG C
Latter 80 DEG C dry 12～18h obtain compound precursor thing E；
7) putting in the tube furnace being passed through argon gas atmosphere by compound precursor thing E, arranging reaction temperature is 350～550 DEG C,
Insulation 0.5～2h, heating rate is 3～10 DEG C of min-1, argon air-flow velocity 0～0.5sccm min-1, obtain
Three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material.
Described plant parenchyma material is peanut skin, garlic skin or Herba Alii fistulosi skin.
The present invention is with thin wall type plant tissues such as peanut skin, garlic skin, Herba Alii fistulosi skins for biomass carbon raw material, at acid soak
Reason obtains the presoma of pre-carbonization, after presoma mixed by a certain percentage with alkali and be fully ground, hot in tube furnace
Process obtains three-dimensional porous carbon skeleton, then is immersed in the solution containing cobalt salt by this three-dimensional porous carbon skeleton, then takes out
Filter and be dried, in being finally putting into tube furnace, be thermally treated resulting in the complex of three-dimensional porous carbon skeleton load C oO,
This complex is applied to lithium ion battery and has good cycle performance and high rate performance.
1) present invention prepares many with various plants parenchymas such as peanut skin, garlic skin, Herba Alii fistulosi skins for biomass carbon raw material
Hole carbon skeleton has stable structure and supports the load of CoO；
2) addition by controlling carbamide can obtain the porous carbon skeleton of different pore size distribution；
3) carbon skeleton of porous is possible not only to the load of stable CoO, and the electric conductivity simultaneously also improving CoO makes
The transfer rate of electronics is accelerated, and electrochemical reaction is accelerated, the beneficially lifting of high rate performance.
Accompanying drawing explanation
Fig. 1 is the three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material of the embodiment of the present invention 1 preparation
The XRD figure of material.
Three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure the material of Fig. 2 embodiment of the present invention 1 preparation
The cycle performance figure of 50 circles is circulated under the electric current density of 100mA/g.
Detailed description of the invention
Embodiment 1: the preparation method of a kind of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by peanut skin cleaning, drying；
2) peanut skin taking 3g is put in the 60ml concentrated sulfuric acid solution that concentration is 5mol/L, anti-in 80 DEG C of baking ovens
Answer 5h, obtain suspending liquid A；
3) suspending liquid A is carried out vacuum filtration, and with deionized water rinsing to pH=7, then collect before being dried to obtain
Drive thing B；
4) predecessor B is mixed with potassium hydroxide 1:1 in mass ratio and grinds uniformly obtain product C；
5) product C putting into be connected with the tube furnace of argon to arrange reaction temperature be 800 DEG C, be incubated 2h, heat up speed
Rate is 3 DEG C of min-1, argon air-flow velocity 0.2sccm min-1, obtain product D；
6) take the analytically pure four acetate hydrate cobalts of 0.02mol, 0.06mol carbamide joins in 100ml deionized water,
Putting in solution by the product D of 1g after stirring, at 60 DEG C, after magnetic agitation 12h, 80 DEG C of dry 12h obtain
To compound precursor thing E；
7) putting in the tube furnace being passed through argon gas atmosphere by compound precursor thing E, arranging reaction temperature is 350 DEG C, insulation
2h, heating rate is 3 DEG C of min-1, argon air-flow velocity 0.4sccm min-1, obtain three-dimensional porous carbon skeleton/CoO and be combined
Structure lithium ion battery negative material.
By Fig. 1 it can be seen that the CoO in the three-dimensional porous carbon skeleton/CoO complex obtained is pure phase, do not see
It is undefined structure that characteristic peak to any carbon is possible as obtained porous carbon.
The most three-dimensional porous carbon skeleton/CoO complex has good cycle performance, along with circulation time
The increase capacity of number is also gradually increasing and is tending towards stability.
Embodiment 2: the preparation method of a kind of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by garlic skin cleaning, drying；
2) garlic skin taking 4g is put in the 60ml concentrated sulfuric acid solution that concentration is 7mol/L, reacts in 80 DEG C of baking ovens
7h, obtains suspending liquid A；
3) suspending liquid A is carried out vacuum filtration, and with deionized water rinsing to pH=7, then collect before being dried to obtain
Drive thing B；
4) predecessor B is mixed with potassium hydroxide 1:2 in mass ratio and grinds uniformly obtain product C；
5) product C putting into be connected with the tube furnace of argon to arrange reaction temperature be 700 DEG C, be incubated 3h, heat up speed
Rate is 5 DEG C of min-1, argon air-flow velocity 0.5sccm min-1, obtain product D；
6) take the analytically pure four acetate hydrate cobalts of 0.02mol, 0.08mol carbamide joins in 100ml deionized water,
After stirring, the product D of 1.5g is put in solution, 80 DEG C of dry 14h after magnetic agitation 14h at 70 DEG C
Obtain compound precursor thing E；
7) putting in the tube furnace being passed through argon gas atmosphere by compound precursor thing E, arranging reaction temperature is 500 DEG C, insulation
1.5h, heating rate is 5 DEG C of min-1, argon air-flow velocity 0.3sccm min-1, obtain three-dimensional porous carbon skeleton/CoO multiple
Close structure lithium ion battery negative material.
Embodiment 3: the preparation method of a kind of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by Herba Alii fistulosi skin cleaning, drying；
2) the Herba Alii fistulosi skin taking 6g is put in the 60ml concentrated sulfuric acid solution that concentration is 10mol/L, reacts in 80 DEG C of baking ovens
6h, obtains suspending liquid A；
3) suspending liquid A is carried out vacuum filtration, and with deionized water rinsing to pH=7, then collect before being dried to obtain
Drive thing B；
4) predecessor B is mixed with potassium hydroxide 1:3 in mass ratio and grinds uniformly obtain product C；
5) product C putting into be connected with the tube furnace of argon to arrange reaction temperature be 900 DEG C, be incubated 1h, heat up speed
Rate is 8 DEG C of min-1, argon air-flow velocity 0.4sccm min-1, obtain product D；
6) take the analytically pure four acetate hydrate cobalts of 0.02mol, 0.07mol carbamide joins in 100ml deionized water,
Putting in solution by the product D of 2g after stirring, at 80 DEG C, after magnetic agitation 16h, 80 DEG C of dry 16h obtain
To compound precursor thing E；
7) putting in the tube furnace being passed through argon gas atmosphere by compound precursor thing E, arranging reaction temperature is 500 DEG C, insulation
1h, heating rate is 8 DEG C of min-1, argon air-flow velocity 0.5sccm min-1, obtain three-dimensional porous carbon skeleton/CoO and be combined
Structure lithium ion battery negative material.
Embodiment 4: the preparation method of a kind of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material,
1) by peanut skin cleaning, drying；
2) peanut skin taking 5g is put in the 60ml concentrated sulfuric acid solution that concentration is 9mol/L, anti-in 80 DEG C of baking ovens
Answer 7h, obtain suspending liquid A；
3) suspending liquid A is carried out vacuum filtration, and with deionized water rinsing to pH=7, then collect before being dried to obtain
Drive thing B；
4) predecessor B is mixed with potassium hydroxide 1:1.5 in mass ratio and grinds uniformly obtain product C；
5) product C puts into tube furnace arranging reaction temperature is 850 DEG C, is incubated 1.5h, and heating rate is 10 DEG C of min-1
Obtain product D；
6) take the analytically pure four acetate hydrate cobalts of 0.02mol, 0.08mol carbamide joins in 100ml deionized water,
After stirring, the product D of 1.8g is put in solution, 80 DEG C of dry 18h after magnetic agitation 18h at 65 DEG C
Obtain compound precursor thing E；
7) putting in tube furnace by compound precursor thing E, arranging reaction temperature is 550 DEG C, is incubated 0.5h, heating rate
It is 10 DEG C of min-1, obtain three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material.
Claims (2)
1. a preparation method for three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material, its feature
It is:
1) by plant parenchyma raw material cleaning, drying；
2) the plant parenchyma taking 3～6g is put in the 60ml concentrated sulfuric acid solution that concentration is 5～10mol/L, in
80 DEG C of baking ovens react 5～7h, obtains suspending liquid A；
3) suspending liquid A is carried out vacuum filtration, and with deionized water rinsing to pH=7, then collect before being dried to obtain
Drive thing B；
4) predecessor B is mixed with potassium hydroxide 1:1～1:3 in mass ratio and grinds uniformly obtain product C；
5) product C is put into that be connected with the tube furnace of argon to arrange reaction temperature be 700～900 DEG C, is incubated 1～3h,
Heating rate is 3～10 DEG C of min-1, argon air-flow velocity 0～0.5sccm min-1, obtain product D；
6) take the analytically pure four acetate hydrate cobalts of 0.02mol, 0.06～0.08mol carbamide and join 100ml deionization
In water, after stirring, the product D of 1～2g is put in solution, magnetic agitation 12～18h at 60～80 DEG C
Latter 80 DEG C dry 12～18h obtain compound precursor thing E；
7) putting in the tube furnace being passed through argon gas atmosphere by compound precursor thing E, arranging reaction temperature is 350～550 DEG C,
Insulation 0.5～2h, heating rate is 3～10 DEG C of min-1, argon air-flow velocity 0～0.5sccm min-1, obtain
Three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material.
Three-dimensional porous carbon skeleton the most according to claim 1/CoO negative pole of lithium ion battery with compound structure material
Preparation method, it is characterised in that: described plant parenchyma material is peanut skin, garlic skin or Herba Alii fistulosi skin.
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Cited By (9)
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| CN107039193A (en) * | 2017-04-14 | 2017-08-11 | 山东大学 | A kind of garlic skin matrix activated carbon electrode material and preparation method for ultracapacitor |
| CN107591250A (en) * | 2017-09-12 | 2018-01-16 | 桂林电子科技大学 | A kind of porous carbon composite of CoO N dopings and its preparation method and application |
| 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 |
| CN108557797A (en) * | 2018-05-25 | 2018-09-21 | 上海应用技术大学 | A kind of cobalt doped porous carbon materials and preparation method thereof |
| CN108649201A (en) * | 2018-05-08 | 2018-10-12 | 宁波大学 | A kind of LaTi21O38·CoO·CuLaO2The preparation method of compound nano wire |
| CN110415986A (en) * | 2019-07-12 | 2019-11-05 | 江苏理工学院 | A kind of Ni doping CoO/C composite material and preparation method |
| 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 |
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| CN113387396A (en) * | 2021-06-11 | 2021-09-14 | 郑州大学 | Biomass carbon electrode composite material and preparation method and application thereof |
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| WO2018188422A1 (en) * | 2017-04-14 | 2018-10-18 | 山东大学 | Garlic skin-based activated carbon electrode material for use with supercapacitor and preparation method |
| CN107039193A (en) * | 2017-04-14 | 2017-08-11 | 山东大学 | A kind of garlic skin matrix activated carbon electrode material and preparation method for ultracapacitor |
| CN107591250A (en) * | 2017-09-12 | 2018-01-16 | 桂林电子科技大学 | A kind of porous carbon composite of CoO N dopings and its preparation method and application |
| 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 |
| CN108649201A (en) * | 2018-05-08 | 2018-10-12 | 宁波大学 | A kind of LaTi21O38·CoO·CuLaO2The preparation method of compound nano wire |
| 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 |
| CN108557797A (en) * | 2018-05-25 | 2018-09-21 | 上海应用技术大学 | A kind of cobalt doped porous carbon materials 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 |
| CN110415986A (en) * | 2019-07-12 | 2019-11-05 | 江苏理工学院 | A kind of Ni doping CoO/C composite material and preparation method |
| CN110415986B (en) * | 2019-07-12 | 2021-05-18 | 江苏理工学院 | Ni-doped CoO/C composite material and preparation method thereof |
| CN110931798A (en) * | 2019-12-12 | 2020-03-27 | 哈尔滨理工大学 | Preparation method of 3DPC/Co/CoO lithium battery negative electrode material |
| CN113387396A (en) * | 2021-06-11 | 2021-09-14 | 郑州大学 | Biomass carbon electrode composite material and preparation method and application thereof |
| 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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