CN108123126A - A kind of preparation method of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material - Google Patents
A kind of preparation method of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material Download PDFInfo
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- CN108123126A CN108123126A CN201711381990.8A CN201711381990A CN108123126A CN 108123126 A CN108123126 A CN 108123126A CN 201711381990 A CN201711381990 A CN 201711381990A CN 108123126 A CN108123126 A CN 108123126A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to battery material preparation fields, disclose a kind of preparation method of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material, graphene oxide solution is prepared using the Hummer methods improved, then the solution to certain density graphene oxide and containing nitrogen source carries out hydro-thermal reaction under certain condition can obtain the three-dimensional nitrogen-doped graphene sponge of definite shape, this three-dimensional nitrogen-doped graphene sponge is immersed in the precursor solution of stannic oxide reaction, hydro-thermal reaction is carried out again, calcination processing under last certain temperature in an inert atmosphere, both load, which can be obtained, the three-dimensional nitrogen-doped graphene composite material of stannic oxide.Composite material prepared by the present invention has fabulous forthright again and outstanding cycle performance, and with quite high specific capacity, improve the efficiency of transmission of electronics and lithium ion, more electronics and ion transmission channel are built, improve the chemical properties such as specific capacity and the cycle performance of stannic oxide negative material.
Description
Technical field
The invention belongs to battery material preparing technical field more particularly to a kind of high-capacity lithium ion cell stannic oxide/
The preparation method of nitrogen-doped graphene composite negative pole material.
Background technology
Lithium ion battery is because with high-energy density, low cost, it is memoryless the features such as, be widely used in each neck
Domain.Influence lithium ion battery energy density and the principal element of cycle performance are the performances of its electrode material, at present primary commercial
The positive electrode of change has LiFePO4, cobalt acid lithium, LiMn2O4, tertiary cathode material etc., according to the energy density of battery, uses ring
Border, performance requirement etc. are had nothing in common with each other.But the negative material of primary commercial is graphite material at present, graphite cathode material
Energy density only has 372mAh/g, and again in the case of current density, cycle performance is bad.Seriously constrain now to high-energy
The requirement of density and high current density, therefore it is extremely urgent to develop a kind of new negative material.In past ten years, metal
Oxide is (such as：Mn3O4, SnO2, Fe2O3, Co3O4Deng), because with higher theoretical specific capacity (500-1200mAh/g), and
And rich reserves, it is cheap, cause the research and development interest of numerous researchers.
In metal oxide negative material, SnO2Because with high theoretical energy density (782mAh/g) with relatively low
Lithium alloy forms potential (~0.5V vs.Li+/ Li), in charge and discharge process there is higher security performance, be widely studied.
But SnO2As negative material, there is also some shortcomingss：If volume expansion in poorly conductive, charge and discharge process is big, easily
Dusting etc. is caused, affects SnO2The performance of high-energy density and high rate performance.Ameliorative way common at present is carbon coating, this
It is a kind of most easy commercial process technology.Common carbon material has：Agraphitic carbon, carbon fiber, carbon nanotubes, graphene
Deng.Wherein, graphene is that conductive best material, resistivity only have 10 at room temperature-6Ω/m, and large specific surface area, are conducive to electricity
The transmission of son and the deintercalation of lithium ion, the doping of nitrogen source can cause graphene to possess more plentiful polyelectron, be conducive to electricity
The transmission of son, so as to improve SnO2The chemical property of negative material.
There are Chinese invention patent CN.107316999A propositions《A kind of three-dimensional self assembly lithium ion compound based on graphene
Electrode material and preparation method thereof》, three-dimensional grapheme gel is first prepared using graphene oxide solution, is then further carried out
Calcination processing cleans up after finally its tin-salt solution is mixed.This preparation method, complex process, and by three
After tieing up Graphene gel elder generation calcination processing, Graphene gel has lost substantial amounts of oxygen-containing functional group, back loading stannic oxide,
Load factor can be caused low, occurred with reference to the problem of force difference.Also there are Chinese invention patent CN.102244250B propositions《Graphene is grand
See body/tin oxide composite lithium ion battery cathode material and its technique》, inventor proposes a kind of with three-dimensional porous graphene
It for template, is impregnated again in certain density tin-salt solution, is then dried after handling calcination processing in inert gas,
Both growth, which can be obtained, the three-dimensional graphene composite material of nano bar-shape stannic oxide, and this patent of invention utilizes three-dimensional graphite
The adsorptivity of alkene, load capacity is limited, and in order to obtain hyperbaric tin source adsorbance, soaking time is long, and tin source concentration is high, prepares
Cycle is long, and waste rate is high.
In conclusion problem existing in the prior art is：Existing preparation method complex process, Graphene gel have lost
Substantial amounts of oxygen-containing functional group, back loading stannic oxide, load factor can be caused low, occurred with reference to the problem of force difference；Load capacity has
Limit, soaking time is long, and tin source concentration is high, long preparation period, and waste rate is high.
The content of the invention
In view of the problems of the existing technology, the present invention provides a kind of high-capacity lithium ion cell stannic oxide/nitratings
The preparation method of graphene composite negative pole.
The present invention is achieved in that a kind of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material
The preparation method of material comprises the following steps：
Step 1 prepares graphene oxide solution by the Hummer methods improved；
Nitrogen source and the graphene oxide solution mixing of step 2, certain volume and concentration, carry out first under certain condition
Secondary hydro-thermal reaction prepares three-dimensional nitrogen-doped graphene sponge；
The taking-up after deionized water immersion 1-24h of nitrogen-doped graphene sponge is put into reaction vessel, then by step 3
The precursor solution of the good a certain proportion of stannic oxide reaction of configuration is instilled, it is anti-that continuation carries out second of hydro-thermal under certain condition
It should；
Step 4, by the three-dimensional nitrogen-doped graphene deionized water for the being compounded with stannic oxide immersion or clear after reaction
It washes after multipass and carries out cool drying using liquid nitrogen；
Step 5, by the stannic oxide after freeze-drying/nitrogen-doped graphene composite material, certain temperature in an inert atmosphere
Lower calcining.
Further, the graphene oxide solution can be the aqueous solution or organic solution of graphene oxide.
Further, the organic solvent can be one or more mixed solutions in methanol, ethyl alcohol, ethylene glycol.
Further, the graphene oxide concentration for preparing three-dimensional grapheme sponge is 0.1-5mg/ml.
Further, the condition of the first time hydro-thermal reaction is 100-220 DEG C, reaction time 1-24h.
Further, the condition of second of hydro-thermal reaction is 120-220 DEG C, reaction time 1-48h.
Further, the precursor solution of the stannic oxide reaction is certain tin source and the aqueous solution of complexing agent.
Further, the tin source can be the one or more in stannous sulfate, stannic chloride, sodium stannate, stannous oxalate
Mixing.
Further, the complexing agent for two Heshui of sodium citrate, citric acid, ethylenediamine, ethylenediamine tetra-acetic acid one kind or
The a variety of mixing of person.
Further, the weight ratio of the tin source and graphene oxide is 0.1-10: 1.
Further, in the precursor solution of the stannic oxide reaction, tin source：Complexing agent：The weight ratio of deionized water
For 1-10: 0.1-3: 1.
Further, the time of the freeze-drying is 1-72h.
Further, the inert gas used during the calcination processing can be：One kind in nitrogen, helium, radon gas, argon gas
Or inert gas gaseous mixture containing 0.1-5% hydrogen.
Further, the temperature of the calcination processing is 300-900 DEG C, time 0.1-12h.
Further, the stannic oxide be nano-scale particle, grain size 1-200nm, the graphene oxide sheet footpath ruler
Very little is 0.1-100um.
Further, the nitrogen source is ammonium hydroxide, the one or more in ethylenediamine, urea mix.
Further, the mass ratio of carbon source and nitrogen source is C: N=1: 0.01-0.5 in the nitrogen-doped graphene.
Advantages of the present invention and good effect are：The present invention provides a kind of high-capacity lithium ion cell stannic oxides/mix
The preparation method of nitrogen graphene composite negative pole, using a process for preparing stannic oxide/nitrogen-doped graphene composite negative pole
Material possesses more three-dimensional conductive network structures, and with more plentiful electronics, the particle of stannic oxide is small, is nanometer
Grade, Size Distribution 1-200nm have higher specific surface area, so as to promote the electric conductivity of stannic oxide negative material, and two
Granules of stannic oxide is small to be conducive to contact in electrolyte charge and discharge, promotes reactivity.Meanwhile the three-dimensional network conductive structure of graphene
And the doping of nitrogen source, be conducive to provide more conductive channels and polyelectron for stannic oxide, so as to promote stannic oxide material
The electric conductivity of material and electron-transport efficiency.Finally so that stannic oxide has the more preferably electrochemistries such as forthright again and cyclicity
Energy.High-capacity lithium ion cell stannic oxide/nitrogen-doped graphene the composite negative pole material prepared by the present invention, stannic oxide
Nano particle is uniformly distributed in graphene sheet layer again, and can reach 2283mAh/g in 100mA/g first discharge specific capacities,
The height ratio capacity of 1239mAh/g can be still maintained under 1A/g current densities after 240 circle of Xun Huan, shows outstanding cycling
Stability and forthright again.
Description of the drawings
Fig. 1 is high-capacity lithium ion cell stannic oxide provided in an embodiment of the present invention/nitrogen-doped graphene composite negative pole material
The flow chart of the preparation method of material；
Fig. 2 is the SEM figures of stannic oxide provided in an embodiment of the present invention/nitrogen-doped graphene composite negative pole material；
Fig. 3 is the TEM figures of stannic oxide provided in an embodiment of the present invention/nitrogen-doped graphene composite negative pole material；
Fig. 4 is stannic oxide provided in an embodiment of the present invention/nitrogen-doped graphene composite negative pole material in 1A/g current densities
Under cycle performance figure.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is further described below in conjunction with the accompanying drawings.
Such as Fig. 1 institutes not, a kind of preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material
Method includes following steps：
S101：Graphene oxide solution is prepared by the Hummer methods improved；
S102：By certain volume and the nitrogen source and graphene oxide solution of concentration, the mass ratio of nitrogen source and carbon source is C: N
=1: 0.01-0.5 mixing under certain condition, 100 DEG C -220 DEG C, under reaction time 1-48h, carries out first time hydro-thermal reaction,
Prepare three-dimensional nitrogen-doped graphene sponge；
S103：Taking-up is put into reaction vessel after nitrogen-doped graphene sponge is impregnated 1-24h with deionized water, is then dripped
Enter the precursor solution of the good a certain proportion of stannic oxide reaction of configuration, the precursor solution is water-soluble for tin source and complexing agent
Liquid, using being tin source：Complexing agent: deionized water quality ratio is 1-10: 0.1-3: 1, the tin source used can be stannous sulfate, chlorine
Change tin, sodium stannate, one or more kinds of mixing in stannous oxalate, the complexing agent used is two Heshui of sodium citrate, citric acid,
The one or more of ethylenediamine, ethylenediamine tetra-acetic acid, mixing continue 120-220 DEG C under certain condition, reaction time 1-
72h carries out second of hydro-thermal reaction；
S104：The three-dimensional nitrogen-doped graphene deionized water for being compounded with stannic oxide after reaction is impregnated or cleaned
After multipass cool drying is carried out using liquid nitrogen；
S105：By the stannic oxide after freeze-drying/nitrogen-doped graphene composite material, in inert atmosphere (such as nitrogen, helium
A kind of or containing 0.1-5% hydrogen inert gas gaseous mixture in gas, radon gas, argon gas) in 300-900 DEG C of certain temperature
Lower calcining.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1：
A kind of preparation method step of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material is such as
Under：
A, graphene oxide solution is prepared by the Hummer methods improved；
B, the graphene oxide ethanol solution of 1mg/ml is configured, the 30ml solution is taken, adds in the urea of 1mg, 120 DEG C of temperature
Under, first time hydro-thermal reaction 12h prepares three-dimensional nitrogen-doped graphene sponge；
C, then, taking-up is put into reaction vessel after the nitrogen-doped graphene sponge being impregnated 12h with deionized water, then
The deionized water for the 20mg stannous sulfate+5mg citric acids+20mg for having configured config. number is instilled, continues under certain condition 180
DEG C, reaction time 12h carries out second of hydro-thermal reaction；
D, the three-dimensional nitrogen-doped graphene deionized water for being compounded with stannic oxide after reaction is impregnated or cleaning is more
After cool drying is carried out using liquid nitrogen for 24 hours；
E, it is last, the stannic oxide after freeze-drying/nitrogen-doped graphene composite material is forged at 400 DEG C in nitrogen
Burn 1h, you can obtain high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material.
Embodiment 2：
A kind of preparation method step of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material is such as
Under：
A, graphene oxide solution is prepared by the Hummer methods improved；
B, the graphene oxide ethanol solution of 1mg/ml is configured, takes the 30ml solution, adds in the ethylenediamine solution of 5ml, 150
At a temperature of DEG C, first time hydro-thermal reaction 12h prepares three-dimensional nitrogen-doped graphene sponge；
C, then, taking-up is put into reaction vessel after the nitrogen-doped graphene sponge being impregnated 12h with deionized water, then
The deionized water for the 30mg stannic chloride+20mg sodium citrates+30mg for having configured config. number is instilled, continues under certain condition 180
DEG C, the reaction time for 24 hours, carries out second of hydro-thermal reaction；
D, the three-dimensional nitrogen-doped graphene deionized water for being compounded with stannic oxide after reaction is impregnated or cleaning is more
After cool drying is carried out using liquid nitrogen for 24 hours；
E, it is last, the stannic oxide after freeze-drying/nitrogen-doped graphene composite material is forged at 600 DEG C in nitrogen
Burn 30min, you can obtain high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material, feature exist
In the preparation method of the high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material comprises the following steps：
Step 1 prepares graphene oxide solution by the Hummer methods improved；
Nitrogen source and the graphene oxide solution mixing of step 2, certain volume and concentration, carry out first time water under certain condition
Thermal response prepares three-dimensional nitrogen-doped graphene sponge；
The taking-up after deionized water immersion 1-24h of nitrogen-doped graphene sponge is put into reaction vessel, then instills by step 3
The precursor solution of the good a certain proportion of stannic oxide reaction of configuration, continuation carry out second of hydro-thermal reaction under certain condition；
The three-dimensional nitrogen-doped graphene deionized water for being compounded with stannic oxide after reaction is impregnated or cleaning is more by step 4
After cool drying is carried out using liquid nitrogen；
Step 5 by the stannic oxide after freeze-drying/nitrogen-doped graphene composite material, is forged under certain temperature in an inert atmosphere
It burns.
2. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as described in claim 1
Method, which is characterized in that the graphene oxide solution can be the aqueous solution or organic solution of graphene oxide；
The organic solvent can be one or more mixed solutions in methanol, ethyl alcohol, ethylene glycol；
The graphene oxide concentration for preparing three-dimensional grapheme sponge is 0.1-5mg/ml；
The condition of the first time hydro-thermal reaction is 100-220 DEG C, reaction time 1-24h.
3. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as described in claim 1
Method, which is characterized in that the condition of second of hydro-thermal reaction is 120-220 DEG C, reaction time 1-48h.
4. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as described in claim 1
Method, which is characterized in that the precursor solution of the stannic oxide reaction is certain tin source and the aqueous solution of complexing agent.
5. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as claimed in claim 4
Method, which is characterized in that the tin source can be that the one or more in stannous sulfate, stannic chloride, sodium stannate, stannous oxalate are mixed
It closes；
The complexing agent is two Heshui of sodium citrate, one or more kinds of mixing of citric acid, ethylenediamine, ethylenediamine tetra-acetic acid；
The weight ratio of the tin source and graphene oxide is 0.1-10: 1.
6. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as described in claim 1
Method, which is characterized in that in the precursor solution of stannic oxide reaction, tin source: complexing agent: the weight ratio of deionized water is
1-10∶0.1-3∶1；
The time of the freeze-drying is 1-72h；
The inert gas used during the calcination processing can be：One kind in nitrogen, helium, radon gas, argon gas contains
The inert gas gaseous mixture of 0.1-5% hydrogen；
The temperature of the calcination processing is 300-900 DEG C, time 0.1-12h.
7. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as described in claim 1
Method, which is characterized in that the stannic oxide be nano-scale particle, grain size 1-200nm, the graphene oxide sheet footpath size
For 0.1-100um.
8. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as described in claim 1
Method, which is characterized in that the nitrogen source is ammonium hydroxide, one or more kinds of mixing in ethylenediamine, urea.
9. the preparation side of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material as described in claim 1
Method, which is characterized in that the mass ratio of carbon source and nitrogen source is C: N=1: 0.01-0.5 in the nitrogen-doped graphene.
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| CN108717974A (en) * | 2018-06-07 | 2018-10-30 | 深圳市梅莎新能源科技有限公司 | A kind of preparation method of lithium ion battery material |
| CN109167019A (en) * | 2018-09-03 | 2019-01-08 | 大同新成新材料股份有限公司 | A kind of cell negative electrode material and preparation method thereof and preparation facilities |
| CN109360973A (en) * | 2018-11-27 | 2019-02-19 | 扬州大学 | A kind of preparation method and lithium ion battery negative material of cobalt sulfide/three-dimensional N doping macropore graphene |
| CN109546099A (en) * | 2018-10-16 | 2019-03-29 | 中航锂电（洛阳）有限公司 | A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery |
| CN109817932A (en) * | 2019-01-29 | 2019-05-28 | 西安航空学院 | One-step method prepares N- and adulterates porous carbon coating SnO2-Co3O4The method and its application of composite material |
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| CN112436127A (en) * | 2020-12-02 | 2021-03-02 | 天津工业大学 | Preparation method of novel nano-structure tin-carbon composite negative electrode material |
| CN112844254A (en) * | 2020-12-16 | 2021-05-28 | 江汉大学 | SnO (stannic oxide)2-EDTA amide compound colloidal dispersion liquid and preparation method thereof |
| CN113548689A (en) * | 2021-07-15 | 2021-10-26 | 陕西科技大学 | Nitrogen-doped carbon/tin dioxide flexible composite film and preparation method and application thereof |
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| CN108717974A (en) * | 2018-06-07 | 2018-10-30 | 深圳市梅莎新能源科技有限公司 | A kind of preparation method of lithium ion battery material |
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| CN109817932A (en) * | 2019-01-29 | 2019-05-28 | 西安航空学院 | One-step method prepares N- and adulterates porous carbon coating SnO2-Co3O4The method and its application of composite material |
| CN112117446A (en) * | 2020-09-18 | 2020-12-22 | 昆明理工大学 | Preparation method of stannic acid tin and graphene co-doped stannic oxide negative electrode material |
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| CN112844254B (en) * | 2020-12-16 | 2022-07-12 | 江汉大学 | SnO (stannic oxide)2-EDTA amide compound colloidal dispersion liquid and preparation method thereof |
| CN113548689A (en) * | 2021-07-15 | 2021-10-26 | 陕西科技大学 | Nitrogen-doped carbon/tin dioxide flexible composite film and preparation method and application thereof |
| CN115440507A (en) * | 2022-08-23 | 2022-12-06 | 西安建筑科技大学 | Tin-based oxide/nitrogen-doped graphene composite material and preparation method and application thereof |
| CN115440507B (en) * | 2022-08-23 | 2023-07-25 | 西安建筑科技大学 | Tin-based oxide/nitrogen-doped graphene composite material and preparation method and application thereof |
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