CN105609772A - Method for preparing N, S-codoped graphene cathode material for lithium-sulfur battery by microwave method - Google Patents
Method for preparing N, S-codoped graphene cathode material for lithium-sulfur battery by microwave method Download PDFInfo
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- CN105609772A CN105609772A CN201610079713.0A CN201610079713A CN105609772A CN 105609772 A CN105609772 A CN 105609772A CN 201610079713 A CN201610079713 A CN 201610079713A CN 105609772 A CN105609772 A CN 105609772A
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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 method for preparing an N, S-codoped graphene cathode material for a lithium-sulfur battery by a microwave method. The method comprises the following steps: (1) preparing graphite oxide by a Hummers method; (2) carrying out ball-mill mixing on the graphite oxide and thiourea at the mass ratio of 1 to (1-6); (3) carrying out microwave heating on the obtained mixture in a microwave reactor in a nitrogen atmosphere to obtain N, S-codoped graphene; (4) dispersing the obtained N, S-codoped graphene into a sodium thiosulfate water solution, carrying out chemical deposition sulphur coating with hydrochloric acid, carrying out suction filtration and washing and then drying the product; and (5) carrying out thermal treatment on the obtained product to obtain the N, S-codoped graphene/sulfur cathode material. The method disclosed by the invention is fast, efficient, simple in process, convenient to operate and high in feasibility; and the prepared N, S-codoped graphene cathode material for the lithium-sulfur battery demonstrates excellent electrochemical properties.
Description
Technical field
The invention belongs to nano composite material technical field, relate to a kind of microwave method and prepare N, S codope stoneThe method of China ink alkene lithium sulfur battery anode material.
Background technology
New forms of energy and regenerative resource are replacing day by day exhausted fossil energy, have become to solve the world todayOne of effective means of energy crisis and environmental problem. Secondary cell is energy storage device in new energy fieldImportant component part, it mainly contains lead-acid battery, Ni-Cr battery, Ni-MH battery, lithium secondary battery etc.Wherein lithium secondary battery because its specific energy is high, charge efficiency is high, temperature characterisitic is good, self discharge is low,The advantages such as the little and memory-less effect of Chargeable heat effect, become the study hotspot of new forms of energy.
But traditional lithium ion battery (LIB), because energy density is difficult to break through 300Wh/kg, has limitedIt is extensive the fields such as hybrid vehicles (PHEV) and pure electric vehicle (PEV)Application. Therefore large-scale high-energy-density, renewable energy system starts progressively to enter into people's cheaplyThe visual field. Using elemental sulfur as positive pole, the lithium-sulfur cell that lithium metal is negative pole, theoretical energy density is up to 2500Wh/kg (volume energy density can reach 2800Wh/L). Compared with traditional lithium ion battery, lithium sulphur electricityIts energy density of 3～5 times can be realized in pond, thereby receives much concern. Because elemental sulfur density is light, reservesAbundant, cheap, environmental friendliness, so lithium-sulfur cell is can not only metric density high and cost is low, materialMaterial source is sufficient. But due to the insulating properties of active material elemental sulfur, elemental sulfur must be led with electronicsBody is mutually compound, is prepared into conductive agent/sulphur composite construction, increases the anodal conductibility to electronics and ion.
Graphene is that one forms bi-dimensional cellular shape new carbon by carbon atom. With other material with carbon element phasesRatio, Graphene has higher specific area and more excellent electric conductivity. Therefore, can be by graphiteAlkene and sulphur are compound, effectively improve the chemical property of lithium-sulfur cell electrode material. But because Graphene isThe two-dimensional structure of sheet, bound not good for sulphur, declines although therefore battery initial capacity is highSubtract very fast. To Graphene doping, Graphene is carried out to chemistry, when the C atom quilt on graphene sheet layerAfter the hetero atom (as N or S atom) close with its electronegativity replaces, its physicochemical properties are hadThe regulation and control of effect.
At present, the method for preparing doped graphene mainly comprises vapour deposition process, hydro-thermal method, high temperature pyrolysisMethod, circumfluence method etc. But these method reaction time are long, temperature is high, energy consumption is large, production cost is high,Be unfavorable for actual scale utilization.
Summary of the invention
The object of this invention is to provide a kind of microwave method and prepare N, S codope Graphene lithium-sulphur cell positive electrodeThe method of material, preparation method's reaction time of having solved prior art is long, temperature is high, energy consumption is large, rawProduce the high problem of cost.
The technical solution adopted in the present invention is that a kind of microwave method is prepared N, S codope Graphene lithium sulphur electricityThe method of pond positive electrode, implement according to following steps:
1) utilize Hummers method to prepare graphite oxide;
2) by step 1) graphite oxide of gained carries out ball milling with thiocarbamide according to mass ratio 1:1～6 and mixes,Ball-milling Time is 0.5～1 hour;
3) by step 2) mixture of gained is placed in small beaker, and then small beaker is put into and filled activityIn the large beaker of carbon, be placed in microwave reactor and carry out heating using microwave under nitrogen atmosphere, obtain N, S is commonDoped graphene;
4) by step 3) gained N, S codope Graphene is dispersed in sodium thiosulfate solution, sulfo-The concentration of aqueous sodium persulfate solution is 15～45g/L, makes N, and S codope Graphene is in hypo solutionConcentration be 8.3～25g/L; Carry out chemical deposition with hydrochloric acid and cover sulphur, concentration of hydrochloric acid is 1M; Then enterAfter row suction filtration, washing, product is dried 20～30 hours at 45～60 DEG C;
5) by step 4) products therefrom heat-treats, and obtains N, the anodal material of S codope Graphene/sulphurMaterial.
The invention has the beneficial effects as follows, main from mode of heating, tradition is prepared to doped graphene materialTechnique is improved. Heating using microwave is different from traditional heating, and when heating using microwave, material with carbon element absorbs microwave,Microwave energy is by being converted into heat energy, and in this process, heat is from material internal generation instead of from outsideAbsorb thermal source, self entirety heats up simultaneously, and heat utilization rate is high, and material monolithic thermograde is very little. ThisRapidly and efficiently, technique is simple for inventive method, and easy to operate, feasibility is high, prepared N, S codopeGraphene lithium sulfur battery anode material shows excellent chemical property.
Brief description of the drawings
Fig. 1 is N prepared by the embodiment of the present invention 1, S codope Graphene lithium sulfur battery anode materialX-ray diffraction (XRD) collection of illustrative plates, wherein abscissa is the angle of diffraction (2 θ), unit is degree, ordinateFor diffracted intensity, unit is cps;
Fig. 2 is N prepared by the embodiment of the present invention 1, and S codope Graphene lithium sulfur battery anode material is in chamberCharging and discharging curve under temperature 0.1C multiplying power, wherein abscissa is specific discharge capacity, unit is mAh/g,Ordinate is voltage, and unit is V.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Native graphite is after oxidation intercalation processing, and interlamellar spacing increases, with after heating using microwave, and the sense of interlayerGroup and thiocarbamide resolve into gas, and sloughing of oxygen-containing functional group provides avtive spot, the contact of thiocarbamide cataboliteThese avtive spots form chemical bond, and hetero atom is embedded in Graphene lattice, and graphite oxide is reduced to stoneChina ink alkene. Method of the present invention, implement according to following steps:
1) utilize Hummers method to prepare graphite oxide; (Hummers method is existing disclosed sideMethod, no longer carefully states at this);
2) by step 1) graphite oxide of gained carries out ball milling with thiocarbamide according to mass ratio 1:1～6 and mixes,Ball-milling Time is 0.5～1 hour;
3) by step 2) mixture of gained is placed in small beaker, and then small beaker is put into and filled activityIn the large beaker of carbon, be placed in microwave reactor and carry out heating using microwave under nitrogen atmosphere, microwave power is400～800W, the reaction time is 0.5～10 minute, obtains N, S codope Graphene;
4) by step 3) gained N, S codope Graphene is dispersed in sodium thiosulfate solution, sulfo-The concentration of aqueous sodium persulfate solution is 15～45g/L, makes N, and S codope Graphene is in hypo solutionConcentration be 8.3～25g/L; Carry out chemical deposition with hydrochloric acid and cover sulphur, concentration of hydrochloric acid is 1M; Then enterAfter row suction filtration, washing, product is dried 20～30 hours at 45～60 DEG C;
5) by step 4) products therefrom heat-treats, and heat treatment temperature is 155～160 DEG C, obtainsN, S codope Graphene/sulphur positive electrode.
Embodiment 1
Utilize Hummers legal system for graphite oxide, graphite oxide is mixed with 1:3 mass ratio with thiocarbamideBall milling is placed in microwave reactor for 0.5 hour, and under nitrogen atmosphere, microwave power 800W heats,React and within 1 minute, obtain N, S codope Graphene. By 0.5gN, S codope Graphene is dispersed in sulfo-sulphurIn acid sodium aqueous solution (ultimate density is 15g/L), carry out chemical deposition with 1M hydrochloric acid and cover sulphur, soAfter carry out suction filtration, washing, to neutral, is dried product 30 hours at 60 DEG C, 158 DEG C of heat treatments,Obtain N, S codope Graphene/sulphur positive electrode.
Embodiment 2
Utilize Hummers legal system for graphite oxide, graphite oxide is mixed with 1:4 mass ratio with thiocarbamideBall milling is placed in microwave reactor for 0.75 hour, and under nitrogen atmosphere, microwave power 500W heats,React and within 6 minutes, obtain N, S codope Graphene. By the N of 0.67g, S codope Graphene is dispersed in sulphurIn the sodium thiosulfate aqueous solution (ultimate density is 20g/L), carry out chemical deposition with 1M hydrochloric acid and cover sulphur,Then carry out suction filtration, washing, to neutral, is dried product 24 hours at 50 DEG C, 155 DEG C of heat treatments,Obtain N, S codope Graphene/sulphur positive electrode.
Embodiment 3
Utilize Hummers legal system for graphite oxide, graphite oxide is mixed with 1:5 mass ratio with thiocarbamideBall milling is placed in microwave reactor for 1 hour, and under nitrogen atmosphere, microwave power 700W heats, anti-Answer and within 4 minutes, obtain N, S codope Graphene. By the N of 1.5g, S codope Graphene is dispersed in sulfo-In aqueous sodium persulfate solution (ultimate density is 25g/L), carry out chemical deposition with 1M hydrochloric acid and cover sulphur,Then carry out suction filtration, washing, to neutral, is dried product 30 hours at 45 DEG C, 160 DEG C of heat treatments,Obtain N, S codope Graphene/sulphur positive electrode.
Embodiment 4
Utilize Hummers legal system for graphite oxide, graphite oxide is mixed with 1:6 mass ratio with thiocarbamideBall milling is placed in microwave reactor for 1 hour, and under nitrogen atmosphere, microwave power 800W heats, anti-Answer and within 3 minutes, obtain N, S codope Graphene. By the N of 0.6g, S codope Graphene is dispersed in sulfo-In aqueous sodium persulfate solution (ultimate density is 18g/L), carry out chemical deposition with 1M hydrochloric acid and cover sulphur,Then carry out suction filtration, washing, to neutral, is dried product 20 hours at 60 DEG C, 160 DEG C of heat treatments,Obtain N, S codope Graphene/sulphur positive electrode.
Embodiment 5
Utilize Hummers legal system for graphite oxide, graphite oxide is mixed with 1:1 mass ratio with thiocarbamideBall milling is placed in microwave reactor for 0.5 hour, and under nitrogen atmosphere, microwave power 400W heats,React and within 10 minutes, obtain N, S codope Graphene. By the N of 0.5g, S codope Graphene is dispersed in sulphurIn the sodium thiosulfate aqueous solution (ultimate density is 15g/L), carry out chemical deposition with 1M hydrochloric acid and cover sulphur,Then carry out suction filtration, washing, to neutral, is dried product 24 hours at 50 DEG C, 158 DEG C of heat treatmentsObtain N, S codope Graphene/sulphur positive electrode.
Comprehensive above-described embodiment, further adopts the prepared sample of embodiment 1～5 to carry out battery assembling:
1) anodal preparation
Respectively by 0.35 gram of N being made by embodiment 1～5, S codope Graphene/sulphur composite material powderWith 0.1 gram of KS-6,0.05 gram of binding agent Kynoar (PVDF) is mixed to be ground, and adds 2 milliliters1-METHYLPYRROLIDONE, stirs and forms even anode sizing agent.
This anode sizing agent is evenly coated on the aluminium foil of 20 microns to then dry desolventizing at 60 DEG CAfter, punching, making area is 1.22cm2Anodal disk, make working electrode through vacuum drying,Wherein containing having an appointment 2mg active material sulphur.
2) negative pole adopts commercially available lithium ion battery lithium sheet.
3) battery assembling
Adopt button cell CR2025 assembling experimental cell test material performance, assemble sequence is negative electrode casing-lithium sheet-electrolyte-barrier film-electrolyte-positive plate-pad-shell fragment-anode cover, then the battery assembling is enteredRow encapsulation, whole process all completes in argon gas glove box.
The several performances of above-mentioned assembled battery are carried out to test analysis as follows:
3.1) cycle performance test: above-mentioned (2025 formula) button cell making is placed on respectively to surveyOn test system, leave standstill after 12 hours, first carry out constant current discharge to 1.5V with 0.1C, then shelve 2 pointsClock, then carries out constant current charge to 3V with 0.1C. Record the discharge capacity first of battery, embodimentThe first discharge specific capacity of 1 resulting materials is 1314mAh/g, then repeats above-mentioned steps 50 times, noteThe discharge capacity of record battery, after 50 circulations, discharge capacity maintains 430mAh/g, capability retentionBe 32.7%, compare with similar electrode material, effectively improved the capability retention of battery, other enforcementsNumber of cases is according to as shown in table 1 below.
Table 1, cycle performance test performance Data Comparison
Fig. 1 is the XRD collection of illustrative plates (X ray diffracting spectrum) of embodiment 1 obtained product: pass throughThe standby graphite oxide of Hummers legal system carries out there is a sharp-pointed diffraction maximum in ° left and right, 2 θ=10, is oxygenThe characteristic peak of fossil China ink. From N, in the XRD collection of illustrative plates of S codope Graphene/sulphur composite, can find out,After microwave irradiation, the characteristic peak of graphite oxide disappears, and has occurred wide bag, explanation in a ° left and right, 2 θ=25Graphite oxide is reduced, and presents disordered structure; Compared with the XRD collection of illustrative plates of sulphur simple substance, sulphur is with crystallizationThe form of state is present in composite.
Fig. 2 is the N of embodiment 1 synthesized, the charge-discharge test of S codope Graphene/sulphur positive electrodeCurve. Under room temperature 0.1C multiplying power, the specific discharge capacity after charge and discharge cycles 50 times is 430mAh/g.The N visible, the present invention is synthetic, S codope Graphene/sulphur composite is as lithium sulfur battery anode materialTime, there is excellent cycle performance.
From the testing result of above-described embodiment, under different reaction conditions, the N of gained, S mixes altogetherAssorted stone graphene anode material all has good chemical property, from the known employing the present invention of table 1 dataThe N that method prepares, the lithium-sulfur cell that S codope Graphene is made has higher initial discharge specific volumeAmount, repeatedly, after circulation, residue reversible capacity is higher, illustrates and utilizes microwave method to carry out hetero atom to GrapheneThe avtive spot producing after doping can effectively adsorb polysulfide in charge and discharge process, reduces active matterThe loss of matter, thus the cycle performance of battery promoted; The method preparation technology is simple, and cost is low, energyEnough applied defects that really effectively solves sulphur positive electrode.
Claims (3)
1. microwave method is prepared a N, the method for S codope Graphene lithium sulfur battery anode material, its featureBe, implement according to following steps:
1) utilize Hummers method to prepare graphite oxide;
2) by step 1) graphite oxide of gained carries out ball milling with thiocarbamide according to mass ratio 1:1～6 and mixes,Ball-milling Time is 0.5～1 hour;
3) by step 2) mixture of gained is placed in small beaker, and then small beaker is put into and filled activityIn the large beaker of carbon, be placed in microwave reactor and carry out heating using microwave under nitrogen atmosphere, obtain N, S is commonDoped graphene;
4) by step 3) gained N, S codope Graphene is dispersed in sodium thiosulfate solution, sulfo-The concentration of aqueous sodium persulfate solution is 15～45g/L, makes N, and S codope Graphene is in hypo solutionConcentration be 8.3～25g/L; Carry out chemical deposition with hydrochloric acid and cover sulphur, concentration of hydrochloric acid is 1M; Then enterAfter row suction filtration, washing, product is dried 20～30 hours at 45～60 DEG C;
5) by step 4) products therefrom heat-treats, and obtains N, the anodal material of S codope Graphene/sulphurMaterial.
2. microwave method according to claim 1 is prepared N, S codope Graphene lithium-sulphur cell positive electrode materialThe method of material, is characterized in that: described step 3) in, microwave power is 400～800W, reactionTime is 0.5～10 minute.
3. microwave method according to claim 1 is prepared N, S codope Graphene lithium-sulphur cell positive electrode materialThe method of material, is characterized in that: described step 5) in, heat treatment temperature is 155～160 DEG C.
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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 |
| CN106654236A (en) * | 2017-02-17 | 2017-05-10 | 中南大学 | Sulfur-doped three-dimensional porous graphene/sulfur composite positive electrode material and preparation method and application thereof |
| 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 |
| CN111099578A (en) * | 2018-10-27 | 2020-05-05 | 中国石油化工股份有限公司 | Nitrogen-doped three-dimensional graphene material |
| JP2021523547A (en) * | 2018-04-30 | 2021-09-02 | ライテン・インコーポレイテッド | Lithium-ion batteries and battery materials |
| 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 |
| CN114655949A (en) * | 2020-12-23 | 2022-06-24 | 中国石油化工股份有限公司 | Preparation method of sulfur and oxygen co-doped graphene |
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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 |
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| CN111099578A (en) * | 2018-10-27 | 2020-05-05 | 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 |
| CN114655949A (en) * | 2020-12-23 | 2022-06-24 | 中国石油化工股份有限公司 | Preparation method of sulfur and oxygen co-doped graphene |
| 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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