CN107845780A - The solvent heat assistant preparation method of lithium-sulfur cell carbon-sulfur compound positive electrode - Google Patents
The solvent heat assistant preparation method of lithium-sulfur cell carbon-sulfur compound positive electrode Download PDFInfo
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Abstract
The present invention relates to a kind of solvent heat assistant preparation method of lithium-sulfur cell carbon-sulfur compound positive electrode, uses carbon material with elemental sulfur for raw material, and the carbon-sulfur compound for being used as lithium sulfur battery anode material is made by solvent thermal reaction process in a solvent.This method raw material is easy to get, flow is simple, easy to operate, suitable for large-scale production.Compared with sulphur method is filled in the melting of existing physics, solvent heat auxiliary law has that temperature is low, the time is short, inactive material damage, green advantage, and the lithium-sulfur cell performance that obtained carbon-sulfur compound assembles is suitable, has a good application prospect.
Description
Technical field
The present invention relates to a kind of solvent heat assistant preparation method of lithium-sulfur cell carbon-sulfur compound positive electrode.
Background technology
With fossil resource exhaustion increasingly, ecological pollution constantly aggravates, global climate constantly warms the problems such as appearance,
Secondary cell substitutes the heat that power-equipment turns into academia and industrial circle is paid close attention to jointly such as traditional fossil fuel driving motor vehicle
Point.In commercialized secondary cell, lithium ion battery is current energy density highest secondary cell, but is based on " deintercalation "
Theoretical lithium ion battery, its theoretical specific capacity are currently less than 300mA h g-1, actual energy density is less than 200Wh kg-1, far
Can not meet people to electric automobile 500km the needs of continuing a journey.Lithium-sulfur cell has high theoretical specific capacity (~1675mAh g-1)
With energy density (~2500W h kg-1), and sulphur also has aboundresources, asepsis environment-protecting, cost cheap as active material
Advantage, thus it is widely regarded as the preferable replacer of lithium ion battery.
Positive pole is to restrict lithium-sulfur cell volumetric properties and the key component of cycle life, and its existing subject matter has：1.
Active material sulphur poorly conductive, cause great activation polarization initial stage in electric discharge；2. charge and discharge process intermediate polysulfide
With stronger solubility property, cause the reduction of volumetric properties and cycle life to cathode of lithium surface by shuttle；3. electric discharge end
Phase, reactant sulphur generate the process of product lithium sulfide through discharge process, and 80% cubical expansivity causes greatly to anode structure
Destruction.
The excellent electric conductivity of carbon material effectively lowers activation polarization effect, while its abundant pore structure can also be delayed
Battery performance fails caused by solving volumetric expansion and shuttle effect, thus is widely used in lithium sulfur battery anode material.At present,
Also there is certain limitation for the common preparation method of carbon-sulfur compound positive electrode：1st, physics fusion method needs higher anti-
Temperature (155 DEG C) and longer reaction time (10~24h) are answered, while is accompanied by the loss of active material；2nd, chemical synthesis
Method would generally produce pernicious gas (such as H2S), while disproportionated reaction will also result in the waste of element sulphur.Therefore, it is necessary to develop
A kind of low energy consumption, low cost, quick, environmental protection carbon-sulfur compound preparation method, to meet that large-scale production requires.
The content of the invention：
Lithium-sulfur cell carbon-sulfur compound positive pole is prepared it is an object of the invention to provide a kind of solvent heat auxiliary law and is easy to big
Large-scale production.
The purpose of the present invention is achieved in the following ways；
Use carbon material with elemental sulfur for raw material, be made by solvent thermal reaction process be used as lithium-sulfur cell just in a solvent
The carbon-sulfur compound of pole material.Described carbon material is CNT, graphene, carbon nano-fiber, bamboo-carbon fibre, carbonized cotton fibre
One or two or more kinds in dimension or carbon dust BP2000, KB600, KB300, XC-72, Super-P, acetylene black, activated carbon.
Described solvent is methanol, ethanol, ethylene glycol, isopropanol, n-butanol, acetonitrile, ether, acetone, water, dimethyl methyl
It is more than one or both of acid amides, dimethyl sulfoxide (DMSO), tetrahydrofuran.
The specific implementation step of described solvent thermal reaction process is as follows：
(1) carbon material and elemental sulfur are compared into ground and mixed by required quality；
(2) it is the mixture after grinding is scattered in a solvent, it is transferred to heating response in reactor after stirring 0.5~12h；
(3) after being cooled to room temperature, product is filtered out, and is washed 2-10 times repeatedly with solvent, 2 are dried at 50~90 DEG C
~24h, obtain carbon-sulfur compound positive electrode.
Described carbon material and the mass ratio of elemental sulfur are 40:60~10:90；
Heating response temperature described in step (2) is 80~200 DEG C, and the described reaction time is 0.5~24h.
The present invention beneficial outcomes be：
The advantages of present invention prepares carbon-sulfur compound using the method for solvent heat auxiliary has between the carbon sulphur in solvent
Stronger affinity, carbon pores can be rapidly entered in the saturated vapor pressure sulphur simple substance of water, ensures that active material sulphur carries with conductive
Abundant contact between body carbon, the electric conductivity of positive electrode is effectively improved, reduce activation polarization effect, be advantageous to improve activity
Material utilization, improve circulating battery stability and high rate performance.
It is of the invention compared with carbon-sulfur compound preparation method in existing lithium-sulfur cell, have the following advantages that：First, with more
Low reaction temperatures and faster reaction time, energy consumption is greatly reduced, shorten the production cycle；Second, due to using close
The reaction unit closed, there is no the loss of active material in positive electrode preparation process, effectively reduce the waste of raw material；Its
Three, occur without disproportionated reaction in preparation process, do not produce pernicious gas, it is environmentally friendly；Fourth, solvent heat auxiliary law is easy to material
The further modification of material, it is expected to realize the high performance lithium sulfur battery anode material of one-step synthesis, simplifies preparation technology.
Solvent heat auxiliary law proposed by the present invention suitable for large-scale production, has a good application prospect into simple.
Brief description of the drawings
Fig. 1 is the SEM figures of carbon-sulfur compound in comparative example 1, comparative example 2 and embodiment 1；
Fig. 2 is the cyclic voltammetry curve of lithium-sulfur cell in comparative example 1, comparative example 2 and embodiment 1；
Fig. 3 is the AC impedance spectroscopy of lithium-sulfur cell in comparative example 1, comparative example 2 and embodiment 1；
Fig. 4 is the cycle performance schematic diagram of lithium-sulfur cell in comparative example 1, comparative example 2 and embodiment 1；
Fig. 5 is the cycle performance schematic diagram of the lithium-sulfur cell obtained under different carbon sulphur mixed proportions；
Fig. 6 is the cycle performance schematic diagram of the lithium-sulfur cell obtained at a temperature of differential responses；
Fig. 7 is the cycle performance schematic diagram of the lithium-sulfur cell obtained under the differential responses time；
Fig. 8 is the cycle performance schematic diagram of the lithium-sulfur cell obtained under different solvents.
Embodiment
Below by embodiment and comparative example, the invention will be further described, rather than the limitation present invention.
Comparative example 1
After 30mg commercialization KB carbon dusts uniformly mix with 70mg S, it is scattered in 1.3gN- methyl pyrrolidones (NMP), treats
After being uniformly dispersed, after adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, 0.132g 10wt% is added and gathers inclined fluorine
Ethene (PVDF) solution, solvent NMP stir 5h, and regulation scraper scratches film forming, 70 DEG C overnight to 200 μm in aluminum laminated films
After drying, a diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, using this sequin as positive pole (monolithic
It is about 1mg cm to carry sulfur content-2), lithium piece is negative pole, and clegard 2325 is barrier film, molten with double (the trifluoromethyl semi-annular jade pendant acyl) imine lithiums of 1M
Liquid (LiTFSI) and 5wt%LiNO3For electrolyte solution, solvent is DOX (DOL) and glycol dimethyl ether (DME)
Mixed liquor (volume ratio v/v=1:1), assembled battery, charge-discharge test is carried out under 0.2C multiplying powers.
Comparative example 2
After 0.3g commercialization KB carbon dusts uniformly mix with 0.7g S, it is placed in tube furnace, is warming up to 155 DEG C, heating rate
For 1 DEG C of min-1, constant temperature 20h, take 0.1g sample dispersions therein to wait to be uniformly dispersed in 1.3gN- methyl pyrrolidones (NMP)
Afterwards, after adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar
(PVDF) solution, solvent NMP stir 5h, and regulation scraper scratches film forming, 70 DEG C of dryings overnight to 200 μm in aluminum laminated films
Afterwards, a diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulphur using this sequin as positive pole
Amount is about 1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution of 1M
And 5wt%LiNO (LiTFSI)3For electrolyte solution, solvent is DOX (DOL) and glycol dimethyl ether (DME)
Mixed liquor (volume ratio v/v=1:1), assembled battery, charge-discharge test is carried out under 0.2C multiplying powers.
Embodiment 1
Take 0.3g commercialization KB carbon dusts and after 0.7g elemental sulfur ground and mixeds, be dispersed in water, reaction is transferred to after stirring 4h
In kettle.Reactor is placed in 120 DEG C of baking ovens and reacts 2h.After being cooled to room temperature, product is filtered out, and washed repeatedly with water
3 times, 12h is dried at 70 DEG C, obtains carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1:1), assembled battery, charge-discharge test is carried out under 0.2C multiplying powers.
As can be seen from Figure 1 with the presence of Massive Sulphur in comparative example 1, and the sulphur in comparative example 2 and embodiment 1 is evenly dispersed in carbon
Surface, illustrate that physics fusion method and solvent heat auxiliary law can effectively improve distribution uniformity of the sulphur in carbon material surface.With reference to
Cyclic voltammetry curve (Fig. 2) and AC impedance spectroscopy (Fig. 3), it can be found that fusion method and solvent-thermal method fill polarization of electrode after sulphur
Effect and electrochemical impedance have and significantly reduced.Contrast the battery performance (Fig. 4) of three kinds of method electrodes, wherein embodiment
1 is made the cyclical stability of electrode and comparative example 2 quite, and is substantially better than comparative example 1.Illustrate that solvent auxiliary law can be relatively low
At a temperature of, reach suitable with physics fusion method in the short period and fill sulphur effect, successfully reduce energy consumption, shorten and prepare
Cycle.
Embodiment 2
Take 0.4g commercialization KB carbon dusts and after 0.6g elemental sulfur ground and mixeds, be dispersed in water, reaction is transferred to after stirring 2h
In kettle.Reactor is placed in 120 DEG C of baking ovens and reacts 2h.After being cooled to room temperature, product is filtered out, and washed repeatedly with water
3 times, 24h is dried at 70 DEG C, obtains carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1:1), assembled battery, charge-discharge test is carried out under 0.2C multiplying powers.
Embodiment 3
Take 0.2g commercialization KB carbon dusts and after 0.8g elemental sulfur ground and mixeds, be dispersed in water, reaction is transferred to after stirring 2h
In kettle.Reactor is placed in 120 DEG C of baking ovens and reacts 2h.After being cooled to room temperature, product is filtered out, and washed repeatedly with water
3 times, 24h is dried at 70 DEG C, obtains carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1: 1), assembled battery, carries out charge-discharge test under 0.2C multiplying powers.
The cycle performance of battery of comparative example 1,2,3, embodiment 1 and embodiment 2 show phase as can be seen from Figure 5
When cyclical stability, and the battery special capacity fade speed of embodiment 3 significantly increases.This is the pore capacities institute by KB carbon materials
Caused, the sulfur content of embodiment 3 is too high, causes sulphur simple substance to cannot be introduced into carbon pores, the inhomogeneity for causing it to be distributed, is unfavorable for
It is fully contacted with carbon material, thus causes circulating battery stability to decline.
Embodiment 4
Take 0.3g commercialization KB carbon dusts and after 0.7g elemental sulfur ground and mixeds, be dispersed in water, reaction is transferred to after stirring 2h
In kettle.Reactor is placed in 80 DEG C of baking ovens and reacts 2h.After being cooled to room temperature, product is filtered out, and 3 are washed repeatedly with water
It is secondary, 24h is dried at 70 DEG C, obtains carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1: 1), assembled battery, carries out charge-discharge test under 0.2C multiplying powers.
Embodiment 5
Take 0.3g commercialization KB carbon dusts and after 0.7g elemental sulfur ground and mixeds, be dispersed in water, reaction is transferred to after stirring 2h
In kettle.Reactor is placed in 160 DEG C of baking ovens and reacts 2h.After being cooled to room temperature, product is filtered out, and washed repeatedly with water
3 times, 24h is dried at 70 DEG C, obtains carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1:1), assembled battery, charge-discharge test is carried out under 0.2C multiplying powers.
The cycle performance of battery of comparative example 1,4,5, as can be seen from Figure 6 relative to embodiment 5, embodiment 1 is 100
Specific discharge capacity after secondary circulation reduces without obvious, illustrates can to obtain under 120 DEG C of reaction temperatures and good fills sulphur effect.And
The battery special capacity fade speed of embodiment 4 significantly increases, and sulphur fails to effectively enter carbon pores under the conditions of illustrating 80 DEG C, battery
Cyclical stability is poor.
Embodiment 6
Take 0.3g commercialization KB carbon dusts and after 0.7g elemental sulfur ground and mixeds, be dispersed in water, reaction is transferred to after stirring 2h
In kettle.Reactor is placed in 120 DEG C of baking ovens and reacts 12h.After being cooled to room temperature, product is filtered out, and washed repeatedly with water
Wash 3 times, dry 24h at 70 DEG C, obtain carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1:1), assembled battery, charge-discharge test is carried out under 0.2C multiplying powers.
Embodiment 7
Take 0.3g commercialization KB carbon dusts and after 0.7g elemental sulfur ground and mixeds, be dispersed in water, reaction is transferred to after stirring 2h
In kettle.Reactor is placed in 120 DEG C of baking ovens and reacts 0.5h.After being cooled to room temperature, product is filtered out, and washed repeatedly with water
Wash 3 times, dry 24h at 70 DEG C, obtain carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1: 1), assembled battery, carries out charge-discharge test under 0.2C multiplying powers.
The cycle performance of battery of comparative example 1,6,7, as can be seen from Figure 7 relative to embodiment 6, embodiment 1 is 100
Specific discharge capacity after secondary circulation reduces without obvious, illustrates that 2h reaction time is enough to obtain and good fills sulphur effect.And implement
The battery special capacity fade speed of example 7 significantly increases, and illustrates that sulphur fails to effectively enter carbon pores, the circulation of battery in the 0.5h times
Less stable.
Embodiment 8
0.3g commercialization KB carbon dusts are taken in ethanol, to be transferred to instead after stirring 2h with after 0.7g elemental sulfur ground and mixeds, disperseing
Answer in kettle.Reactor is placed in 100 DEG C of baking ovens and reacts 6h.After being cooled to room temperature, product is filtered out, and with ethanol repeatedly
Washing 3 times, dries 24h at 70 DEG C, obtains carbon-sulfur compound；
Carbon-sulfur compound made from 0.1g is taken, is scattered in 1.3gN- methyl pyrrolidones (NMP), after being uniformly dispersed,
After adding 24.7mg commercialization Super P, ultrasonic 20min, 1h is stirred, adds 0.132g 10wt% Kynoar (PVDF)
Solution, solvent NMP stir 5h, and regulation scraper scratches film forming in aluminum laminated films, after 70 DEG C of dryings overnight, cut to 200 μm
A diameter of 14mm sequins are cut into, after weighing, after 60 DEG C of vacuum drying 24h, (monolithic carries sulfur content using this sequin as positive pole
1mg cm-2), lithium piece is negative pole, and clegard 2325 is barrier film, with double (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M
And 5wt%LiNO3For electrolyte solution, solvent is the mixed liquor of DOX (DOL) and glycol dimethyl ether (DME)
(volume ratio v/v=1:1), assembled battery, charge-discharge test is carried out under 0.2C multiplying powers.
The cycle performance of battery of comparative example 1,8, as can be seen from Figure 8 relative to embodiment 1, embodiment 8 is at 100 times
Specific discharge capacity after circulation decreases.This is due to that elemental sulfur is slightly soluble in ethanol, and its solubility can be significantly under critical condition
Degree lifting, and be cooled to the sulphur simple substance dissolved after room temperature and separate out, cause itself and conductive carrier KB contact to be deteriorated, capacity plays
And the cyclical stability of battery decreases.
Claims (7)
1. the solvent heat assistant preparation method of lithium-sulfur cell carbon-sulfur compound positive electrode, it is characterised in that：Using carbon material with
Elemental sulfur is raw material, and the carbon-sulfur compound for being used as lithium sulfur battery anode material is made by solvent thermal reaction process in a solvent.
2. preparation method according to claim 1, it is characterised in that：Described carbon material is CNT, graphene, carbon
Nanofiber, bamboo-carbon fibre, carbonization cotton fiber or carbon dust BP2000, KB600, KB300, XC-72, Super-P, acetylene black, work
One or two or more kinds in property charcoal.
3. preparation method according to claim 1, it is characterised in that：Described solvent is methanol, ethanol, ethylene glycol, different
One or both of propyl alcohol, n-butanol, acetonitrile, ether, acetone, water, dimethylformamide, dimethyl sulfoxide (DMSO), tetrahydrofuran
More than.
4. preparation method according to claim 1, it is characterised in that：The specific implementation step of described solvent thermal reaction process
It is rapid as follows：
(1) carbon material and elemental sulfur are compared into ground and mixed by required quality；
(2) it is the mixture after grinding is scattered in a solvent, it is transferred to heating response in reactor after stirring 0.5~12h；
(3) after being cooled to room temperature, filter out product, and washed 2-10 times repeatedly with solvent, at 50~90 DEG C dry 2~
24h, obtain carbon-sulfur compound positive electrode.
5. the preparation method according to claim 1 or 4, it is characterised in that：Described carbon material and the mass ratio of elemental sulfur
For 40: 60~10: 90.
6. the preparation method according to claim 1 or 4, it is characterised in that：Described thermal response temperature is 80~200 DEG C.
7. the preparation method according to claim 1 or 4, it is characterised in that：The described thermal response time is 0.5~24h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112701266A (en) * | 2020-12-30 | 2021-04-23 | 江西昌河汽车有限责任公司 | Preparation method and application of porous carbon and sulfur composite material |
| CN113764635A (en) * | 2021-08-18 | 2021-12-07 | 广东东岛新能源股份有限公司 | One-step hydrothermal preparation method and application of sulfur-carbon composite material |
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2016
- 2016-09-18 CN CN201610826115.5A patent/CN107845780A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112701266A (en) * | 2020-12-30 | 2021-04-23 | 江西昌河汽车有限责任公司 | Preparation method and application of porous carbon and sulfur composite material |
| CN112701266B (en) * | 2020-12-30 | 2022-04-01 | 江西昌河汽车有限责任公司 | Preparation method and application of porous carbon and sulfur composite material |
| CN113764635A (en) * | 2021-08-18 | 2021-12-07 | 广东东岛新能源股份有限公司 | One-step hydrothermal preparation method and application of sulfur-carbon composite material |
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Application publication date: 20180327 |