CN107611374A - A kind of preparation method of new lithium sulfur battery anode material - Google Patents
A kind of preparation method of new lithium sulfur battery anode material Download PDFInfo
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Abstract
A kind of preparation method of new lithium sulfur battery anode material, belongs to lithium-sulfur cell preparing technical field.Preparation method is as follows：（1）Prepare carbon material；（2）By metal salt, carbon material, surfactant, ascorbic acid aqueous solution hybrid reaction；（3）Will（2）Obtained product calcining；（4）It is compound with sulphur simple substance, heating；（5）Will（4）Obtained compound mixes with conductive agent and binding agent, drying.It is an advantage of the invention that：The positive electrode of the present invention is made up of the compound of sulphur simple substance and molybdenum dioxide and graphene, and elemental sulfur is by melting diffusion method into molybdenum dioxide and the inside compounds of graphene.Molybdenum dioxide has good fixation to lithium-sulfur cell discharging product, can lift the stability of battery；Graphene can provide a conductive network, can also increase the loading of sulphur.
Description
Technical field
The invention belongs to lithium-sulfur cell preparing technical field, and in particular to a kind of preparation of new lithium sulfur battery anode material
Method.
Background technology
With the development of portable electronic industry, the battery of high-energy-density is the emphasis place studied at present.It is limited to pass
The restriction of system anode material for lithium-ion batteries, current lithium ion battery can not meet the needs of present, therefore seek one
The secondary cell of kind more height ratio capacity is imperative.Lithium-sulfur cell has capacity height（1675mAh/g）, cost is low, elemental sulfur is next
The advantages that source is wide, nontoxic, is paid much attention to by researcher in recent years, promises to be the secondary electricity of high-energy-density of future generation
Pond body system.
But the development of lithium-sulfur cell is faced with the challenge of many at present.Mainly there is following problem：(1) elemental sulfur
It is non-conductive, serious polarization, influence the performance of whole battery；(2) discharge potential is than relatively low, only 2.1V；(3) produced among electric discharge
The more lithium sulfides of thing are soluble in electrolyte, cause sulphur to move to negative terminal surface by electrolyte, influence battery life；(4) elemental sulfur
Discharge process volumetric expansion is serious, destroys anode structure；(5) short circuit easily occurs, deposits as negative material from elemental lithium
In potential safety hazard.Wherein, it is faced with the problem of most in terms of positive pole.
The method for generally solving the dissolving of the more lithium sulfides of positive pole is compound from a kind of carbon material and elemental sulfur, by elemental sulfur
It is wrapped in electric discharge intermediate product in the duct of carbon material.Carbon material good conductivity, the nonconducting problem of sulphur simple substance can be improved.
Meanwhile the high-specific surface area of carbon material is advantageous to being uniformly distributed for sulphur simple substance, while positive pole in discharge process can also be alleviated
Volumetric expansion problem.But recent studies suggest that, carbon material belongs to nonpolar molecule, more lithium sulfide interaction forces with polarity
It is poor, long-term cyclical stability can not be obtained.Based on such a viewpoint, researcher chooses element doping modified carbonaceous components again
Surface texture, but the avtive spot adulterated is limited, the lifting unobvious to cycle performance.Recently, metal oxide is as lithium
The research of sulphur cell positive electrode carrier material turns into the focus for suppressing shuttle effect.But metal oxide poorly conductive itself, meeting
Influence the high rate performance of battery；Metal oxide specific surface area is low, is unfavorable for the preparation of the lithium-sulfur cell of high carrying capacity.How to tie
It is to need most asking for solution at present that the advantages of closing carbon material and metal oxide, which prepares a kind of efficient lithium-sulphur cell positive electrode carrier,
Topic.
The content of the invention
The invention aims to solve the deficiency of existing lithium sulfur battery anode material, there is provided a kind of new lithium-sulfur cell
Metal oxide is bonded on the carbon material as lithium-sulphur cell positive electrode carrier by the preparation method of positive electrode, this kind of method, with
The compound of simple physical mixed is compared, and the chemical bond between metal oxide and carbon material can promote the transmission of electronics,
Lift the dynamics of cell reaction.
To achieve the above object, the technical scheme that the present invention takes is as follows：
A kind of preparation method of new lithium sulfur battery anode material, methods described comprise the following steps that：
Step 1：Carbon material is prepared, the concentration of the carbon material is 1-5mg/mL；
Step 2：Take 100-200mg metal salts to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 10-20 mL
Carbon material continue stirring 30 minutes；Take 200mg surfactants to be added in 30mL deionized waters to stir to being completely dissolved,
100mg ascorbic acid is added, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred in polytetrafluoroethylene (PTFE)
In lining, 160-200 DEG C of hydro-thermal reaction 36-72 hour；
Step 3：The product that step 3 is obtained 600 DEG C of calcining 3-6h under the conditions of argon gas, obtain metal oxide and carbon material
Compound；
Step 4：The metal oxide and carbon material compound that step 3 is obtained are with sulphur simple substance according to 1：2-5 mass ratio mixes
Close, 155 DEG C of heating 12-24 hours under the conditions of argon gas；
Step 5：The compound that step 4 is obtained is with conductive agent and binding agent according to mass ratio 8：1：1 mixing, is preparing sulphur just
Pole, it is put into 40-70 DEG C of drying in baking oven.
It is of the invention to be relative to the beneficial effect of prior art：The positive electrode of the present invention by sulphur simple substance and molybdenum dioxide with
The compound of graphene is formed, and elemental sulfur is by melting diffusion method into molybdenum dioxide and the inside compounds of graphene.Dioxy
Change molybdenum has good fixation to lithium-sulfur cell discharging product, can lift the stability of battery；Graphene can provide
One conductive network, the loading of sulphur can also be increased；Chemical bond between molybdenum dioxide and graphene be present, electricity can be provided
Sub- transmission channel, reduce the extra energy required for charge transfer between molybdenum dioxide and graphene, be advantageous to lift lithium sulphur
The high rate performance of battery.
Brief description of the drawings
Fig. 1 is MoO2With the scanning electron microscope diagram piece of graphene complex；
Fig. 2 is MoO prepared by the present invention2, graphene and sulphur composite as lithium-sulphur cell positive electrode when the punching of 0.2C first circles put
Electric cyclic curve figure；
Fig. 3 is MoO prepared by the present invention2, graphene and sulphur composite and physical mixed molybdenum dioxide and graphene mixture
（MoO2+G）High rate performance comparison diagram during as lithium-sulphur cell positive electrode.
Embodiment
Technical scheme is further described below in conjunction with the accompanying drawings, but is not limited thereto, it is every to this
Inventive technique scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
Embodiment one：What present embodiment was recorded is a kind of preparation method of new lithium sulfur battery anode material,
Methods described comprises the following steps that：
Step 1：Carbon material is prepared, the concentration of the carbon material is 1-5mg/mL；
Step 2：Take 100-200mg metal salts to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 10-20 mL
Carbon material continue stirring 30 minutes；Take 200mg surfactants to be added in 30mL deionized waters to stir to being completely dissolved,
100mg ascorbic acid is added, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred in polytetrafluoroethylene (PTFE)
In lining, 160-200 DEG C of hydro-thermal reaction 36-72 hour；
Step 3：The product that step 3 is obtained 600 DEG C of calcining 3-6h under the conditions of argon gas, obtain metal oxide and carbon material
Compound；
Step 4：The metal oxide and carbon material compound that step 3 is obtained are with sulphur simple substance according to 1：2-5 mass ratio mixes
Close, 155 DEG C of heating 12-24 hours under the conditions of argon gas；
Step 5：The compound that step 4 is obtained is with conductive agent and binding agent according to mass ratio 8：1：1 mixing, is preparing sulphur just
Pole, it is put into 40-70 DEG C of drying in baking oven.
Embodiment two：A kind of preparation side of new lithium sulfur battery anode material described in embodiment one
Method, in step 1, the carbon material is one kind in graphene oxide, CNT or porous carbon；
The specific preparation process of the graphene oxide is as follows：
Dense H is sequentially added into natural flake graphite2SO4, dense HNO3And NaNO3Stirring, adds potassium permanganate and hydrogen peroxide
Graphite oxidation is obtained into graphene oxide；
The specific preparation process of the CNT is as follows：
Take 1g CNTs to add 10mL concentrated nitric acids, 90 DEG C of heating reflux reactions 5 hours, then cleaned with deionized water into
Property, filter, dry；
The specific preparation process of the CNT is as follows：
Take 1g Ketjen blacks to add 10mL concentrated nitric acids, 90 DEG C of heating reflux reactions 5 hours, then cleaned with deionized water to neutrality,
Filtering, dry.
Embodiment three：A kind of preparation side of new lithium sulfur battery anode material described in embodiment one
Method, in step 2, the surfactant is polyvinylpyrrolidone, PEO-PPOX-PEO three
One kind in block copolymer or sodium stearyl sulfate.
Embodiment four：A kind of preparation side of new lithium sulfur battery anode material described in embodiment one
Method, in step 2, the metal salt is one kind in molybdenum salt, manganese salt, zinc salt, cobalt salt or nickel salt.
Embodiment 1：
（1）Under the conditions of sub-cooled liquid circulation, the dense H of 120 mL are sequentially added into 5 g natural flake graphites2SO4、50
The dense HNO of mL3With 2.5 g NaNO3, continuously stir 2 h；15 g potassium permanganate are gradually added, stirring 1h withdraws cooling liquid
The circulatory system, sticky graphite oxide solution is obtained after continuously stirring 48 h of reaction at room temperature.To sticky graphite oxide
80 mL deionized waters are slowly added in solution, after being down to room temperature, add deionized water that graphite oxide solution is diluted into 750 mL,
30% H is added dropwise after stirring dropwise2O2, stood after the color of graphite oxide solution is changed into glassy yellow, by resulting solution
With HCl with 1:10 ratio is diluted, and obtains the graphene oxide that concentration is 3mg/mL；
（2）Take 100mg ammonium molybdates to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 10mL 3mg/mL oxidation
Graphene continues stirring 30 minutes；Take 100mg polyvinylpyrrolidones to be added in 30mL deionized waters to stir to completely molten
Solution, adds 100mg ascorbic acid, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred to polytetrafluoroethylene (PTFE)
In liner, 180 DEG C of hydro-thermals 48 hours；
（3）Hydrothermal product is freeze-dried, is then transferred into tube furnace, in the case where argon gas protects atmosphere, 600 DEG C are heated 4 hours,
Obtain MoO2And graphene complex；
（4）By 50 mg MoO2It is uniform with graphene complex and the grinding of 200 mg bright sulfurs, it is put into tube furnace, logical argon gas is done
Protect 155 DEG C of gas to calcine 12 hours, obtain MoO2, graphene and sulphur composite.
Embodiment 2：
（1）Under the conditions of sub-cooled liquid circulation, the 120 dense H of m L are sequentially added into 5 g natural flake graphites2SO4、
The 50 dense HNO of m L3With 2.5 g NaNO3, continuously stir 2 h；15 g potassium permanganate are gradually added, stirring 1h withdraws cold
But fluid circulation system, sticky graphite oxide solution is obtained after continuously stirring 48 h of reaction at room temperature.To sticky oxygen
80 mL deionized waters are slowly added in graphite solution, after being down to room temperature, add deionized water to be diluted to graphite oxide solution
750 mL, 30% H is added dropwise after stirring dropwise2O2, stood after the color of graphite oxide solution is changed into glassy yellow.By institute
Solution is obtained with HCl with 1:10 ratio is diluted, and obtains the graphene oxide that concentration is 3mg/mL；
（2）Take 200mg ammonium molybdates to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 10mL 3mg/mL oxidation
Graphene continues stirring 30 minutes；Take 100mg polyvinylpyrrolidones to be added in 30mL deionized waters to stir to completely molten
Solution, adds 100mg ascorbic acid, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred to polytetrafluoroethylene (PTFE)
In liner, 160 DEG C of hydro-thermals 200 hours；
（3）Hydrothermal product is freeze-dried, is then transferred into tube furnace, lower 600 DEG C is enclosed in argon gas protection gas and heats 4 hours,
Obtain MoO2And graphene complex；
（4）By 50 mg MoO2It is uniform with graphene complex and the grinding of 200 mg bright sulfurs, it is put into tube furnace, logical argon gas is done
Protect 155 DEG C of gas to calcine 12 hours, obtain MoO2, graphene and sulphur composite.
Embodiment 3：
（1）Under the conditions of sub-cooled liquid circulation, the dense H of 120 mL are sequentially added into 5 g natural flake graphites2SO4、50
The dense HNO of mL3With 2.5 g NaNO3, continuously stir 2 h；15 g potassium permanganate are gradually added, stirring 1h withdraws coolant
Systemic circulatory system, sticky graphite oxide solution is obtained after continuously stirring 48 h of reaction at room temperature.To sticky oxidation stone
80 mL deionized waters are slowly added in black solution, after being down to room temperature, add deionized water that graphite oxide solution is diluted into 750
ML, 30% H is added dropwise after stirring dropwise2O2, stood after the color of graphite oxide solution is changed into glassy yellow.Gained is molten
Liquid is with HCl with 1:10 ratio is diluted, and obtains the graphene oxide that concentration is 3mg/mL；
（2）Take 100mg ammonium molybdates to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 20mL 3mg/mL oxidation
Graphene continues stirring 30 minutes；Take 100mg polyvinylpyrrolidones to be added in 30mL deionized waters to stir to completely molten
Solution, adds 100mg ascorbic acid, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred to polytetrafluoroethylene (PTFE)
In liner, 200 DEG C of hydro-thermals 36 hours；
（3）Hydrothermal product is freeze-dried, is then transferred into tube furnace, in the case where argon gas protects atmosphere, 600 DEG C are heated 4 hours,
Obtain MoO2And graphene complex；
（4）By 50 mg MoO2It is uniform with graphene complex and the grinding of 200 mg bright sulfurs, it is put into tube furnace, logical argon gas is done
Protect 155 DEG C of gas to calcine 12 hours, obtain MoO2, graphene and sulphur composite.
Embodiment 4：
（1）Under the conditions of sub-cooled liquid circulation, the 120 dense H of m L are sequentially added into 5 g natural flake graphites2SO4、
The 50 dense HNO of m L3With 2.5 g NaNO3, continuously stir 2 h；15 g potassium permanganate are gradually added, stirring 1h withdraws cold
But fluid circulation system, sticky graphite oxide solution is obtained after continuously stirring 48 h of reaction at room temperature.To sticky oxygen
80 mL deionized waters are slowly added in graphite solution, after being down to room temperature, add deionized water to be diluted to graphite oxide solution
750 mL, 30% H is added dropwise after stirring dropwise2O2, stood after the color of graphite oxide solution is changed into glassy yellow.By institute
Solution is obtained with HCl with 1:10 ratio is diluted, and obtains the graphene oxide that concentration is 3mg/mL；
（2）Take 200mg ammonium molybdates to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 20mL 3mg/mL oxidation
Graphene continues stirring 30 minutes；Take 100mg polyvinylpyrrolidones to be added in 30mL deionized waters to stir to completely molten
Solution, adds 100mg ascorbic acid, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred to polytetrafluoroethylene (PTFE)
In liner, 180 DEG C of hydro-thermals 48 hours；
（3）Hydrothermal product is freeze-dried, is then transferred into tube furnace, in the case where argon gas protects atmosphere, 600 DEG C are heated 6 hours,
Obtain MoO2And graphene complex；
（4）By 50 mg MoO2It is uniform with graphene complex and the grinding of 200 mg bright sulfurs, it is put into tube furnace, logical argon gas is done
Protect 155 DEG C of gas to calcine 12 hours, obtain MoO2, graphene and sulphur composite.
Embodiment 5：
（1）Under the conditions of sub-cooled liquid circulation, the 120 dense H of m L are sequentially added into 5 g natural flake graphites2SO4、
The 50 dense HNO of m L3With 2.5 g NaNO3, continuously stir 2 h；15 g potassium permanganate are gradually added, stirring 1h withdraws cold
But fluid circulation system, sticky graphite oxide solution is obtained after continuously stirring 48 h of reaction at room temperature.To sticky oxygen
80 mL deionized waters are slowly added in graphite solution, after being down to room temperature, add deionized water to be diluted to graphite oxide solution
750 mL, 30% H is added dropwise after stirring dropwise2O2, stood after the color of graphite oxide solution is changed into glassy yellow.By institute
Solution is obtained with HCl with 1:10 ratio is diluted, and obtains the graphene oxide that concentration is 3mg/mL；
（2）Take 200mg ammonium molybdates to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 10mL 3mg/mL oxidation
Graphene continues stirring 30 minutes；Take 200mg polyvinylpyrrolidones to be added in 30mL deionized waters to stir to completely molten
Solution, adds 100mg ascorbic acid, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred to polytetrafluoroethylene (PTFE)
In liner, 180 DEG C of hydro-thermals 48 hours.
（3）Hydrothermal product is freeze-dried, is then transferred into tube furnace, 600 DEG C of heating 3 are small in the case where argon gas protects atmosphere
When, obtain MoO2And graphene complex.
（4）By 50 mg MoO2It is uniform with graphene complex and the grinding of 100 mg bright sulfurs, it is put into tube furnace, leads to argon
Gas does 155 DEG C of protection gas and calcined 12 hours, obtains MoO2, graphene and sulphur composite.
The preparation and performance test of electrode：By electrode material, Super P and PVDF according to mass ratio 8: 1 : 1
Mixing, solvent is made with NMP, forms slurry, stirs 12 hours, coated in positive pole is used as on aluminium foil, by the use of lithium metal as negative pole, makes
With the model barrier films of Celgard 2400,1mol/L LiTFSI is dissolved in DOL/DME (volume ratios 1:1) in solvent
It is electrolyte, 1mol/L LiNO3Additive is done, button cell is assembled into glove box.Surveyed using Neware batteries
Test system carries out constant current charge-discharge test, and charging/discharging voltage scope is 1.7 V-2.8 V.As shown in figure 1, it is the present embodiment system
Standby MoO2With the scanning electron microscope diagram piece of graphene complex, it can be seen that MoO2It is evenly distributed in graphene table
Face；Fig. 2 is MoO manufactured in the present embodiment2, graphene and sulphur composite as lithium-sulphur cell positive electrode when the punching of 0.2C first circles put
Electric cyclic curve, it can be seen that discharge capacity is 1123 mAh/g first；Fig. 3 is MoO manufactured in the present embodiment2And graphene
Composite and physical mixed molybdenum dioxide and graphene mixture（MoO2+G）High rate performance during as lithium-sulphur cell positive electrode
Comparison diagram, it can be seen that the molybdenum dioxide and graphene composite material of chemical bonding are clearly demarcated to the lifting ten of lithium-sulfur cell high rate performance
It is aobvious.
Claims (4)
- A kind of 1. preparation method of new lithium sulfur battery anode material, it is characterised in that：Methods described comprises the following steps that：Step 1：Carbon material is prepared, the concentration of the carbon material is 1-5mg/mL；Step 2：Take 100-200mg metal salts to be added in 20mL 2M hydrochloric acid to stir 30 minutes, add 10-20 mL Carbon material continue stirring 30 minutes；Take 200mg surfactants to be added in 30mL deionized waters to stir to being completely dissolved, 100mg ascorbic acid is added, obtained solution is poured into above-mentioned solution and stirred 30 minutes, is transferred in polytetrafluoroethylene (PTFE) In lining, 160-200 DEG C of hydro-thermal reaction 36-72 hour；Step 3：The product that step 3 is obtained 600 DEG C of calcining 3-6h under the conditions of argon gas, obtain metal oxide and carbon material Compound；Step 4：The metal oxide and carbon material compound that step 3 is obtained are with sulphur simple substance according to 1：2-5 mass ratio mixes Close, 155 DEG C of heating 12-24 hours under the conditions of argon gas；Step 5：The compound that step 4 is obtained is with conductive agent and binding agent according to mass ratio 8：1：1 mixing, is preparing sulphur just Pole, it is put into 40-70 DEG C of drying in baking oven.
- A kind of 2. preparation method of new lithium sulfur battery anode material according to claim 1, it is characterised in that：Step 1 In, the carbon material is one kind in graphene oxide, CNT or porous carbon；The specific preparation process of the graphene oxide is as follows：Dense H is sequentially added into natural flake graphite2SO4, dense HNO3And NaNO3Stirring, adds potassium permanganate and hydrogen peroxide Graphite oxidation is obtained into graphene oxide；The specific preparation process of the CNT is as follows：Take 1g CNTs to add 10mL concentrated nitric acids, 90 DEG C of heating reflux reactions 5 hours, then cleaned with deionized water into Property, filter, dry；The specific preparation process of the CNT is as follows：Take 1g Ketjen blacks to add 10mL concentrated nitric acids, 90 DEG C of heating reflux reactions 5 hours, then cleaned with deionized water to neutrality, Filtering, dry.
- A kind of 3. preparation method of new lithium sulfur battery anode material according to claim 1, it is characterised in that：Step 2 In, the surfactant is polyvinylpyrrolidone, PEO-PPOX-PEO triblock copolymer One kind in thing or sodium stearyl sulfate.
- A kind of 4. preparation method of new lithium sulfur battery anode material according to claim 1, it is characterised in that：Step 2 In, the metal salt is one kind in molybdenum salt, manganese salt, zinc salt, cobalt salt or nickel salt.
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| CN109081376A (en) * | 2018-10-25 | 2018-12-25 | 济南大学 | A kind of derivative MoO of MOF of rGO package2The preparation and its application of micron bar |
| CN109912796A (en) * | 2019-02-25 | 2019-06-21 | 嘉兴学院 | A method of preparing positive pole material for high-performance lithium-sulfur battery, electrode and battery |
| CN110336031A (en) * | 2019-06-28 | 2019-10-15 | 陕西科技大学 | A kind of sulphur load molybdenum oxide/graphene hollow structure electrode material preparation method |
| CN111403712A (en) * | 2020-03-27 | 2020-07-10 | 清华大学深圳国际研究生院 | Lithium-sulfur battery positive electrode material, preparation method thereof and lithium-sulfur battery |
| CN111628156A (en) * | 2020-06-29 | 2020-09-04 | 蜂巢能源科技有限公司 | Molybdenum-doped porous silicon-carbon composite material, preparation method thereof and lithium ion battery |
| CN113582231A (en) * | 2021-06-08 | 2021-11-02 | 湖南师范大学 | MoO (MoO)2Preparation method of/carbon composite interlayer |
| CN114436333A (en) * | 2022-04-11 | 2022-05-06 | 中博龙辉装备集团股份有限公司 | Molybdenum dioxide nanodot-loaded carbon nanotube conductive microsphere and preparation method and application thereof |
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