CN105609772B - Microwave method prepares N, the method for S codope graphene lithium sulfur battery anode materials - Google Patents
Microwave method prepares N, the method for S codope graphene lithium sulfur battery anode materials Download PDFInfo
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- CN105609772B CN105609772B CN201610079713.0A CN201610079713A CN105609772B CN 105609772 B CN105609772 B CN 105609772B CN 201610079713 A CN201610079713 A CN 201610079713A CN 105609772 B CN105609772 B CN 105609772B
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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 microwave method to prepare N, the method for S codope graphene lithium sulfur battery anode materials, and step includes：1) graphite oxide is prepared using Hummers methods；2) by graphite oxide and thiocarbamide according to mass ratio 1：1~6 carries out ball milling mixing；3) mixture of gained is placed in progress microwave heating in microwave reactor in a nitrogen atmosphere, obtains N, S codope graphenes；4) by gained N, S codope graphene dispersions carry out chemical deposition in sodium thiosulfate solution, with hydrochloric acid and cover sulphur, and after then being filtered, washing, product is being dried；5) products therefrom is heat-treated, obtains N, S codopes graphene/sulphur positive electrode.The method of the present invention, rapidly and efficiently, technique is simple, easy to operate, and feasibility is high, and the N of preparation, S codope graphene lithium sulfur battery anode materials show excellent chemical property.
Description
Technical field
The invention belongs to nanocomposite technical field, is related to a kind of microwave method and prepares N, S codope graphene lithium sulphur
The method of cell positive material.
Background technology
New energy is substituting the fossil energy of increasingly depleted with regenerative resource, into solution world today's energy crisis
And one of effective means of environmental problem.Secondary cell is the important component of energy storage device in new energy field, it is led
There are lead-acid battery, Ni-Cr battery, Ni-MH battery, lithium secondary battery etc..Wherein lithium secondary battery is since it is higher than energy, charging
It is efficient, temperature characterisitic is good, self discharge is low, fuel factor is small and the advantages that memory-less effect, becomes the research of new energy for charging
Hot spot.
But conventional lithium ion battery (LIB) limits it in hybrid power since energy density is difficult to break through 300Wh/kg
The extensive use in the field such as the vehicles (PHEV) and the pure electric vehicle vehicles (PEV).Therefore large-scale high-energy-density, low cost
Renewable energy system start progressively to enter into the visual field of people.Using elemental sulfur as cathode, lithium metal is electric for the lithium sulphur of anode
Pond, theoretical energy density are up to 2500Wh/kg (volume energy density is up to 2800Wh/L).With traditional lithium ion battery phase
Than lithium-sulfur cell can realize its 3~5 times of energy density, thus receive much concern.Due to elemental sulfur density is light, rich reserves,
It is cheap, environmental-friendly, so not only energy density is high but also cost is low, material source is sufficient for lithium-sulfur cell.But due to
The insulating properties of active material elemental sulfur so that elemental sulfur must be mutually compound with electronic conductor, is prepared into conductive agent/sulphur composite junction
Structure, to increase conductibility of the cathode to electronics and ion.
Graphene is that one kind forms bi-dimensional cellular shape new carbon by carbon atom.Compared with other carbon materials, graphene
Specific surface area and more excellent electric conductivity with higher.Therefore, can be compound with sulphur by graphene, effectively improve lithium
The chemical property of sulphur battery electrode material.But since graphene is the two-dimensional structure of sheet, for the bound bad of sulphur,
Although therefore battery initial capacity is high but decay is very fast.Graphene is adulterated, i.e., chemistry is carried out to graphene, works as graphene film
C atoms on layer by with its electronegativity similar in after hetero atom (such as N or S atom) substitution, its physicochemical properties obtains effectively
Regulation and control.
At present, preparing the method for doped graphene mainly includes vapour deposition process, hydro-thermal method, high temperature pyrolytic cracking (HTP), circumfluence method
Deng.However, these method reaction time are long, temperature is high, energy consumption is big, production cost is high, it is unfavorable for actual scale and uses.
The content of the invention
The object of the present invention is to provide a kind of microwave method to prepare N, the side of S codope graphene lithium sulfur battery anode materials
Method, solves the problems, such as that the preparation method reaction time of the prior art is long, temperature is high, energy consumption is big, production cost is high.
The technical solution adopted in the present invention is that a kind of microwave method prepares N, S codope graphene lithium-sulphur cell positive electrode materials
The method of material, implements according to following steps：
1) graphite oxide is prepared using Hummers methods；
2) by the graphite oxide obtained by step 1) and thiocarbamide according to mass ratio 1：1~6 carries out ball milling mixing, and Ball-milling Time is
0.5~1 it is small when；
3) mixture obtained by step 2) is placed in small beaker, then small beaker is put into the large beaker for filling activated carbon
In, progress microwave heating in microwave reactor is placed in a nitrogen atmosphere, obtains N, S codope graphenes；
4) by N obtained by step 3), for S codope graphene dispersions in sodium thiosulfate solution, sodium thiosulfate is water-soluble
The concentration of liquid is 15~45g/L, makes N, and concentration of the S codope graphenes in hypo solution is 8.3~25g/L；With
Hydrochloric acid carries out chemical deposition and covers sulphur, concentration of hydrochloric acid 1M；Then after being filtered, washing, by product in 45~60 DEG C of drying
20~30 it is small when；
5) step 4) products therefrom is heat-treated, obtains N, S codopes graphene/sulphur positive electrode.
The invention has the advantages that the technique for mainly preparing doped graphene material to tradition from mode of heating carries out
Improve.Microwave heating is different from traditional heating, and when microwave heats, carbon material absorbs microwave, and microwave energy is by being converted into heat
Can, in this process, heat produces from material internal rather than absorbs heat source from outside, itself integrally heats up at the same time, thermal energy profit
High, the material bulk temperature gradient very little with rate.Rapidly and efficiently, technique is simple for the method for the present invention, easy to operate, and feasibility is high, institute
The N of preparation, S codope graphene lithium sulfur battery anode material show excellent chemical property.
Brief description of the drawings
The N that Fig. 1 is prepared for the embodiment of the present invention 1, the X-ray diffraction of S codope graphene lithium sulfur battery anode materials
(XRD) collection of illustrative plates, wherein abscissa are the angle of diffraction (2 θ), and unit is degree, and ordinate is diffracted intensity, unit cps；
Fig. 2 is N prepared by the embodiment of the present invention 1, and S codope graphene lithium sulfur battery anode materials are in room temperature 0.1C multiplying powers
Under charging and discharging curve, wherein abscissa is specific discharge capacity, unit mAh/g, and ordinate is voltage, unit V.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
After the oxidized intercalation processing of native graphite, interlamellar spacing increase, after being heated with microwave, the functional group of interlayer and thiocarbamide point
Solution sloughs offer avtive spot into gas, oxygen-containing functional group, and thiocarbamide catabolite contacts these avtive spots and forms chemical bond,
Hetero atom is embedded into graphene lattice, and graphite oxide is reduced to graphene.The method of the present invention, implements according to following steps：
1) graphite oxide is prepared using Hummers methods；(Hummers methods are existing disclosed methods, no longer thin herein
State)；
2) by the graphite oxide obtained by step 1) and thiocarbamide according to mass ratio 1：1~6 carries out ball milling mixing, and Ball-milling Time is
0.5~1 it is small when；
3) mixture obtained by step 2) is placed in small beaker, then small beaker is put into the large beaker for filling activated carbon
In, it is placed in microwave reactor progress microwave heating in a nitrogen atmosphere, microwave power is 400~800W, the reaction time 0.5
~10 minutes, obtain N, S codope graphenes；
4) by N obtained by step 3), for S codope graphene dispersions in sodium thiosulfate solution, sodium thiosulfate is water-soluble
The concentration of liquid is 15~45g/L, makes N, and concentration of the S codope graphenes in hypo solution is 8.3~25g/L；With
Hydrochloric acid carries out chemical deposition and covers sulphur, concentration of hydrochloric acid 1M；Then after being filtered, washing, by product in 45~60 DEG C of drying
20~30 it is small when；
5) step 4) products therefrom is heat-treated, heat treatment temperature is 155~160 DEG C, obtains N, S codope graphite
Alkene/sulphur positive electrode.
Embodiment 1
Graphite oxide is prepared using Hummers methods, by graphite oxide and thiocarbamide with 1：When 3 mass are smaller than mixing and ball milling 0.5
It is placed in microwave reactor, microwave power 800W is heated under nitrogen atmosphere, and reaction obtains N, S codope graphite in 1 minute
Alkene.By 0.5g N, S codopes graphene dispersion in sodium thiosulfate solution (ultimate density 15g/L), with 1M hydrochloric acid into
Row chemical deposition covers sulphur, is then filtered, and washs to neutrality, by product when 60 DEG C of drying 30 are small, at 158 DEG C of heat
Reason, obtains N, S codopes graphene/sulphur positive electrode.
Embodiment 2
Graphite oxide is prepared using Hummers methods, by graphite oxide and thiocarbamide with 1：When 4 mass are smaller than mixing and ball milling 0.75
It is placed in microwave reactor, microwave power 500W is heated under nitrogen atmosphere, and reaction obtains N, S codope graphite in 6 minutes
Alkene.By the N of 0.67g, S codopes graphene dispersion is in sodium thiosulfate solution (ultimate density 20g/L), with 1M hydrochloric acid
Carry out chemical deposition and cover sulphur, then filtered, washed to neutrality, by product when 50 DEG C of drying 24 are small, at 155 DEG C of heat
Reason, obtains N, S codopes graphene/sulphur positive electrode.
Embodiment 3
Graphite oxide is prepared using Hummers methods, by graphite oxide and thiocarbamide with 1：After when 5 mass are smaller than mixing and ball milling 1
It is placed in microwave reactor, microwave power 700W is heated under nitrogen atmosphere, and reaction obtains N, S codope graphenes in 4 minutes.
By the N of 1.5g, S codopes graphene dispersion is carried out in sodium thiosulfate solution (ultimate density 25g/L) with 1M hydrochloric acid
Chemical deposition covers sulphur, is then filtered, and washs to neutrality, by product when 45 DEG C of drying 30 are small, is heat-treated at 160 DEG C,
Obtain N, S codopes graphene/sulphur positive electrode.
Embodiment 4
Graphite oxide is prepared using Hummers methods, by graphite oxide and thiocarbamide with 1：After when 6 mass are smaller than mixing and ball milling 1
It is placed in microwave reactor, microwave power 800W is heated under nitrogen atmosphere, and reaction obtains N, S codope graphenes in 3 minutes.
By the N of 0.6g, S codopes graphene dispersion is carried out in sodium thiosulfate solution (ultimate density 18g/L) with 1M hydrochloric acid
Chemical deposition covers sulphur, is then filtered, and washs to neutrality, by product when 60 DEG C of drying 20 are small, is heat-treated at 160 DEG C,
Obtain N, S codopes graphene/sulphur positive electrode.
Embodiment 5
Graphite oxide is prepared using Hummers methods, by graphite oxide and thiocarbamide with 1：When 1 mass is smaller than mixing and ball milling 0.5
It is placed in microwave reactor, microwave power 400W is heated under nitrogen atmosphere, and reaction obtains N, S codope graphite in 10 minutes
Alkene.By the N of 0.5g, S codopes graphene dispersion is in sodium thiosulfate solution (ultimate density 15g/L), with 1M hydrochloric acid
Carry out chemical deposition and cover sulphur, then filtered, washed to neutrality, by product when 50 DEG C of drying 24 are small, at 158 DEG C of heat
Reason obtains N, S codopes graphene/sulphur positive electrode.
Summary embodiment, further carries out battery assembling using the sample prepared by embodiment 1~5：
1) preparation of cathode
Respectively by 0.35 gram of N as made from embodiment 1~5, S codopes graphene/sulphur composite material powder and 0.1 gram
KS-6,0.05 gram of binding agent Kynoar (PVDF) mix grinding, add 2 milliliters of 1-methyl-2-pyrrolidinones, and stirring forms equal
Even anode sizing agent.
The anode sizing agent is coated uniformly on 20 microns of aluminium foil, after then solvent is removed in drying at 60 DEG C, punching, system
It is 1.22cm to obtain area2Cathode disk, working electrode is made by vacuum drying, wherein containing about 2mg active material sulphur.
2) anode uses commercially available lithium ion battery lithium piece.
3) battery assembles
Experimental cell test material performance is assembled using button cell CR2025, assemble sequence is negative electrode casing-lithium piece-electrolysis
Liquid-membrane-electrolyte-positive plate-gasket-shrapnel-anode cover, then the battery assembled is packaged, whole process exists
Completed in argon gas glove box.
It is as follows that test analysis is carried out to the above-mentioned several performances of assembled battery：
3.1) cycle performance test：(2025 formula) button cell obtained above is individually positioned in test system, it is quiet
Put 12 it is small when after, constant current discharge is first carried out to 1.5V with 0.1C, then shelve 2 minutes, constant current charge is then carried out with 0.1C
To 3V.The discharge capacity first of battery is recorded, the first discharge specific capacity of 1 resulting materials of embodiment is 1314mAh/g, Ran Houchong
Above-mentioned steps 50 times again, record the discharge capacity of battery, and discharge capacity maintains 430mAh/g after 50 circulations, and capacity is kept
Rate is 32.7%, compared with homogeneous electrode material, effectively increases the capacity retention ratio of battery, other embodiment data such as following table
Shown in 1.
Table 1, cycle performance test performance data comparison
Fig. 1 is the XRD spectrum (X ray diffracting spectrum) of product obtained by embodiment 1：The oxygen prepared by Hummers methods
Graphite carries out having a sharp diffraction maximum in 2 θ=10 ° or so, is the characteristic peak of graphite oxide.From N, S codope graphite
In the XRD spectrum of alkene/sulphur composite material as can be seen that after microwave irradiation, the characteristic peak of graphite oxide disappears, in 2 θ=25 °
There is wide bag in left and right, illustrates that graphite oxide is reduced, and disordered structure is presented；Compared with the XRD spectrum of sulphur simple substance, sulphur is to tie
The form of crystalline state is present in composite material.
Ns of the Fig. 2 synthesized by embodiment 1, the charge-discharge test curve of S codopes graphene/sulphur positive electrode.In room temperature
Under 0.1C multiplying powers, the specific discharge capacity after charge and discharge cycles 50 times is 430mAh/g.As it can be seen that the N that the present invention synthesizes, S codopes
When graphene/sulphur composite material is used as lithium sulfur battery anode material, there is excellent cycle performance.
From the testing result of above-described embodiment, under different reaction conditions, the N of gained, S codope stone graphenes
Positive electrode is respectively provided with good chemical property, the N for understanding to be prepared using the method for the present invention from 1 data of table, S codopes
Lithium-sulfur cell made of graphene has higher initial discharge specific capacity, and repeatedly after circulation, remaining reversible capacity is higher, explanation
The avtive spot for graphene produce after Heteroatom doping using microwave method can effectively adsorb more in charge and discharge process
Sulfide, reduces the loss of active material, so as to improve the cycle performance of battery；This method preparation process is simple, and cost is low,
Really the applied defect of sulphur positive electrode can effectively be solved.
Claims (1)
1. a kind of microwave method prepares N, the method for S codope graphene lithium sulfur battery anode materials, it is characterised in that according to following
Step is implemented：
1) graphite oxide is prepared using Hummers methods；
2) by the graphite oxide obtained by step 1) and thiocarbamide according to mass ratio 1：1~6 carries out ball milling mixing, Ball-milling Time 0.5
~1 it is small when；
3) mixture obtained by step 2) is placed in small beaker, is then put into small beaker in the large beaker for filling activated carbon,
It is placed in microwave reactor progress microwave heating in a nitrogen atmosphere, microwave power be 400~800W, the reaction time is 0.5~
10 minutes, obtain N, S codope graphenes；
4) by N obtained by step 3), S codope graphene dispersions in sodium thiosulfate solution, sodium thiosulfate solution
Concentration is 15~45g/L, makes N, and concentration of the S codope graphenes in hypo solution is 8.3~25g/L；Use hydrochloric acid
Carry out chemical deposition and cover sulphur, concentration of hydrochloric acid 1M；Then after being filtered, washing, product dried at 45~60 DEG C to 20~
30 it is small when；
5) step 4) products therefrom being heat-treated, heat treatment temperature is 155~160 DEG C, obtains N, S codopes graphene/
Sulphur positive electrode.
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| CN106115667A (en) * | 2016-06-20 | 2016-11-16 | 南京工程学院 | The low temperature preparation method of S, N codope Graphene and application |
| CN106654236B (en) * | 2017-02-17 | 2019-05-10 | 中南大学 | A kind of three-dimensional porous graphene/sulfur composite positive electrode material of sulfur doping and its preparation method and application |
| EP3788666A4 (en) * | 2018-04-30 | 2022-01-19 | Lyten, Inc. | Lithium ion battery and battery materials |
| CN111099578B (en) * | 2018-10-27 | 2022-09-09 | 中国石油化工股份有限公司 | Nitrogen-doped three-dimensional graphene material |
| CN110010868A (en) * | 2019-04-03 | 2019-07-12 | 山东星火科学技术研究院 | A kind of preparation method of the graphene composite sponge of Li-S cell positive material |
| CN114655949B (en) * | 2020-12-23 | 2023-09-29 | 中国石油化工股份有限公司 | Preparation method of sulfur-oxygen co-doped graphene |
| CN114400313A (en) * | 2021-12-06 | 2022-04-26 | 西安理工大学 | Evaluation method and device for preparing graphene-sulfur composite cathode material by microwave method |
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| CN103187570B (en) * | 2011-12-28 | 2015-09-30 | 清华大学 | The preparation method of sulphur-graphene composite material |
| CN104192830A (en) * | 2014-05-20 | 2014-12-10 | 江苏欧力特能源科技有限公司 | Preparing method of nitrogen-sulfur co-doped graphene by hydrothermal method |
| CN105244476A (en) * | 2014-06-11 | 2016-01-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nitrogen-doped graphene-coated nanometer sulfur cathode composite material, and preparation method and applications thereof |
| US10137150B2 (en) * | 2014-06-17 | 2018-11-27 | Elena Molokanova | Graphene and graphene-related materials for manipulation of cell membrane potential |
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