CN106058208B - Sulphur carbon positive electrode and preparation method thereof for lithium-sulfur rechargeable battery - Google Patents
Sulphur carbon positive electrode and preparation method thereof for lithium-sulfur rechargeable battery Download PDFInfo
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- 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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- H—ELECTRICITY
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H—ELECTRICITY
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- H—ELECTRICITY
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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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 sulphur carbon positive electrode and preparation method thereof that the invention discloses a kind of for lithium-sulfur rechargeable battery, the following steps are included: poloxamer is added to absolute ethanol warm dissolution by (1), then dissolution is stirred at room temperature in the above-mentioned clear solution of heat cured liquid phenolic resin addition and forms solution I.(2) solution I is added in sodium thiosulfate and vulcanized sodium and stirs a few minutes, dilute sulfuric acid is then added and is stirred to react a period of time formation colloidal sol II.(3) colloidal sol II is poured into culture dish to be placed in after baking oven constant temperature is stood and generates sulphur carbon positive electrode coarse granule in tubular type kiln roasting.(4) above-mentioned coarse granule is dispersed into sulphur carbon positive electrode fine grained by cryomilling method.Being formed uniformly by sulphur positive electrode prepared by chemical synthesis process restrained effectively the loss of sulphur volume expansion and sulphur active material in the electrolytic solution in mesoporous carbon inner wall, improves electronics conduction efficiency, improves electrical property.
Description
Technical field
The present invention relates to electrode material of secondary lithium ion battery preparation fields, are used for the secondary electricity of lithium sulphur more particularly to one kind
The sulphur carbon positive electrode in pond and preparation method thereof.
Background technique
The problem of in order to alleviate energy shortage, sulfur materials are exploited out the wherein a member that can be used as energy storage material.At present
The popular energy storage mode of sulfur materials has sodium-sulphur battery and lithium-sulfur rechargeable battery.
On the one hand sodium-sulphur battery compensates for due to energy deficiency as the newcomer in electrochemical energy family, its generation
The crisis of initiation, on the other hand, since it does not discharge any harmful substance, using or environment will not be caused after scrapping secondary
Pollution is a kind of environment-friendly type new energy truly.Sodium-sulphur battery has original advantage for energy storage, is mainly reflected in
Raw material reserves are big, energy and power density are big, efficiency for charge-discharge is high, the features such as not limited by place, is easy to maintain.It is external big
Power (especially Japanese) develops sodium-sulfur battery energy storage in addition to the high performance characteristics of sodium-sulphur battery itself, one main reasons is that from
Resource and environmental consideration, not only specific energy is low for lead-acid battery, and manufacturing process and old and useless battery can all cause serious dirt to environment
It contaminates, the Li and Co (its positive electrode LiCoO at present in lithium ion battery2) earth reserves not enrich (especially Co), this
Outer Co is toxic, and manufacturing process and old and useless battery have injury to environment and human body.In contrast, Na and S almost with it not
It exhausts.Simple substance Na and S element itself is no toxicity to human body, and Na in old and useless battery and S can almost be returned with 100%
It receives.Therefore, either from the point of view of the Development of Novel energy, energy saving, environmental protection, or from the strategy of sustainable development
Height go measure and think deeply, China develop sodium-sulfur battery energy storage system be completely it is necessary to, make this technical transform production
Power is very urgent.
Blueness of lithium-sulfur rechargeable battery due to specific capacity is high, resourceful, low in cost and environmentally friendly by researcher
It looks at, but lithium-sulfur rechargeable battery, there is also some problems, usual elemental sulfur is the insulator of electronics and ion, needs to add a large amount of
Conductive agent, so that reducing the utilization rate of active material.And in lithium-sulfur cell discharge process, more lithium sulfides of generation are soluble
In electrolyte, the final product lithium sulfide after electric discharge is easy to generate biggish crystal again, loses electro-chemical activity, causes battery
Specific capacity decline, cycle performance are deteriorated.The shortcomings that in order to overcome sulphur poorly conductive, researcher by conductive polymer polymer with
Elemental sulfur is compound, the conductive network of electron-transport is formed using electrically conductive composite, polymer is because having special structure, Ke Yiqi
To conductive, dispersion, suction-operated, the utilization efficiency of sulphur is improved.Document [Carbon46 (2008) 229] prepares mesoporous carbon first,
Then sulphur is melted with mesoporous carbon compound.Central South University patent CN103840143A is also substep preparation S/TiO2Composite material,
Mesoporous TiO is prepared first2, then heated with sulphur.But this compound mode is usually that substep carries out, and is made first
Standby conductive polymer polymer out, then be combined with each other in a manner of grinding, melting, be heat-treated or deposit etc. with sulphur.It is this compound
The sulphur composite material uniformity that mode is formed is very poor, some site sulphur are reunited seriously, some site sulphur are lax even without distribution
It is very uneven.Lithium-sulfur rechargeable battery is dispersed very poor in water another problem is that the molecule of sulphur is hydrophobic grouping, dissolves the molten of sulphur
Agent is not explosive (CS2) it is exactly the big (CCl of toxicity4, toluene, benzene), in dehydrated alcohol dispersibility still so that with solvent be situated between
The difficulty that matter prepares sulphur by chemical synthesis increases.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is the chemical synthesis gone out by one pot of Water-In-Oil to provide one kind for lithium
Sulphur carbon positive electrode of sulfur rechargeable battery and preparation method thereof, prepared by spherical sulphur be embedded in ordered mesoporous carbons anode composite material
Material restrained effectively the loss of sulphur volume expansion and sulphur active material in the electrolytic solution, improve electronics conduction efficiency, improve
Electrical property.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that: a kind of sulphur for lithium-sulfur rechargeable battery
The preparation method of carbon positive electrode, comprising the following steps:
(1) poloxamer is added to absolute ethanol warm dissolution, adds heat cured liquid phenolic resin, is stirred at room temperature
Dissolution forms solution；
(2) stoichiometrically sodium thiosulfate and vulcanized sodium are added in the solution of step (1), stirring 5 minutes, then
Be added dilute sulfuric acid the reaction was stirred for 2 to 6 hours formed colloidal sol；
(3) colloidal sol is poured into culture dish and is placed in after baking oven constant temperature is stood the inert atmosphere roasting generation sulphur carbon in tube furnace
Positive electrode coarse granule；
(4) above-mentioned coarse granule is dispersed into sulphur carbon positive electrode fine grained by cryomilling method.
Poloxamer described in the step (1): heat cured liquid phenolic resin: dehydrated alcohol is (0.8 according to weight ratio
~1.35): 1:(6~10).
Step (1) the warm solution temperature control is at 30~50 DEG C, and warm dissolution time control was at 15~60 minutes；Room
For warm whipping temp at 20~30 DEG C, it is 30~150 minutes that the time, which is stirred at room temperature,.
Dilute sulfuric acid is (1.5~3) by weight in dehydrated alcohol and step (2) in the step (1): 1, dilute sulfuric acid mole
Concentration is 0.1~5mol/L；In the step (2), according to chemical reaction equation Na2S2O3+2Na2S+3H2SO4=3Na2SO4+4S
+3H2O is with molar ratio computing, additional amount sodium thiosulfate: vulcanized sodium: sulfuric acid=(1.05~1.15): 2:3.
Step (3) colloidal sol pour into culture dish with a thickness of 0.1~5mm, constant temperature dwell temperature and time be first 20~
30 DEG C stand 12 hours, and latter 90~120 DEG C stand 24 hours.
It is argon gas or nitrogen that step (3) tube furnace, which roasts inert atmosphere or inert gas used,；Maturing temperature is 500
~750 DEG C.
Step (4) the cryomilling method uses dry ball milling or wet ball grinding 2~3 hours, wet ball grinding solvent for use
For nonpolar solvent acetone or ether.
The above-mentioned preparation method sulphur carbon positive electrode obtained for being used for lithium-sulfur rechargeable battery.
Beneficial effects of the present invention: it is formed uniformly by sulphur positive electrode prepared by chemical synthesis process in mesoporous carbon
Wall restrained effectively the loss of sulphur volume expansion and sulphur active material in the electrolytic solution, improve electronics conduction efficiency, improve
Electrical property.
Specific embodiment
Preparation method of the invention is described in detail combined with specific embodiments below.
The preparation method of sulphur carbon positive electrode for lithium-sulfur rechargeable battery of the invention, comprising the following steps:
(1) poloxamer is added to absolute ethanol warm dissolution, adds heat cured liquid phenolic resin, is stirred at room temperature
Dissolution forms solution；
(2) stoichiometrically sodium thiosulfate and vulcanized sodium are added in the solution of step (1), stirring 5 minutes, then
Be added dilute sulfuric acid the reaction was stirred for 2 to 6 hours formed colloidal sol；
(3) colloidal sol is poured into culture dish and is placed in after baking oven constant temperature is stood the inert atmosphere roasting generation sulphur carbon in tube furnace
Positive electrode coarse granule；
(4) above-mentioned coarse granule is dispersed into sulphur carbon positive electrode fine grained by cryomilling method.
Poloxamer described in the step (1): heat cured liquid phenolic resin: dehydrated alcohol is (0.8 according to weight ratio
~1.35): 1:(6~10).
Step (1) the warm solution temperature control is at 30~50 DEG C, and warm dissolution time control was at 15~60 minutes；Room
For warm whipping temp at 20~30 DEG C, it is 30~150 minutes that the time, which is stirred at room temperature,.
Dilute sulfuric acid is (1.5~3) by weight in dehydrated alcohol and step (2) in the step (1): 1, dilute sulfuric acid mole
Concentration is 0.1~5mol/L；In the step (2), according to chemical reaction equation Na2S2O3+2Na2S+3H2SO4=3Na2SO4+4S
+3H2O is with molar ratio computing, additional amount sodium thiosulfate: vulcanized sodium: sulfuric acid=(1.05~1.15): 2:3.
Step (3) colloidal sol pour into culture dish with a thickness of 0.1~5mm, constant temperature dwell temperature and time be first 20~
30 DEG C stand 12 hours, and latter 90~120 DEG C stand 24 hours.
It is argon gas or nitrogen that step (3) tube furnace, which roasts inert atmosphere or inert gas used,；Maturing temperature is 500
~750 DEG C.
Step (4) the cryomilling method uses dry ball milling or wet ball grinding 2~3 hours, wet ball grinding solvent for use
For nonpolar solvent acetone or ether.
The above-mentioned preparation method sulphur carbon positive electrode obtained for being used for lithium-sulfur rechargeable battery.
Advantages of the present invention:
1) chemical synthesis process that the present invention is gone out using one pot of Water-In-Oil, it is poly- that oily phase self assembly generates orderly conductive polymer
Phase sulfur is generated and is mutually wrapped up by oily while closing object, and sulphur is made to be successfully embed into conductive polymer inner polymer wall.
2) the method keeps the sulfur granules of synthesis tiny because the ordered space of conductive polymer polymer limits effect.
3) because chemical synthesis process carries out in the solution first, then poloxamer surfactants rise simultaneously as raw material
Alleviate oil-water interfaces surface tension effect, entire synthetic environment is uniform, and sulfur granules is allow equably to be created on macromolecule
The inner wall of conducting polymer.
4) synthetic method of Water-In-Oil keeps the sulfur granules to be formed almost spherical.
5) cryomilling ensure that sulfur granules are not oxidized and restore.
Embodiment 1
A kind of preparation method of lithium-sulfur rechargeable battery sulphur carbon positive electrode, comprising the following steps:
(1) 7.5g poloxamer is added 40 DEG C of warms dissolution 30 minutes in 45g dehydrated alcohol, then by 7.5g thermosetting property liquid
Above-mentioned 20 DEG C of clear solution room temperature stirring and dissolving 60 minutes formation solution I is added in state phenolic resin.
(2) solution I stoichiometrically is added in 1.05 mMs of sodium thiosulfate and 2 mMs of vulcanized sodium and stirs 5 points
Clock, the molar concentration for being then added 3 mMs is that 0.1mol/L dilute sulfuric acid is stirred to react 3 hours formation colloidal sol II.
(3) colloidal sol II is poured into culture dish, with a thickness of 1mm, is placed in 20 DEG C of baking oven elder generation constant temperature and stands 12 hours, latter 90 DEG C
24 hours are stood, then roasts 500 DEG C of generation sulphur carbon positive electrode coarse granules under protection of argon gas in tube furnace.
(4) above-mentioned coarse granule was dispersed into sulphur carbon positive electrode fine grained by dry method cryomilling 2 hours.
Embodiment 2
A kind of preparation method of lithium-sulfur rechargeable battery sulphur carbon positive electrode, comprising the following steps:
(1) 10g poloxamer is added 30 DEG C of warms dissolution 60 minutes in 90g dehydrated alcohol, then by 10g heat cured liquid
Above-mentioned 30 DEG C of clear solution room temperature stirring and dissolving 30 minutes formation solution I is added in phenolic resin.
(2) solution I stoichiometrically is added in 11 mMs of sodium thiosulfate and 20 mMs of vulcanized sodium and stirs 5 points
Clock, the molar concentration for being then added 30 mMs is that 1mol/L dilute sulfuric acid is stirred to react 2 hours formation colloidal sol II.
(3) colloidal sol II is poured into culture dish, with a thickness of 3mm, is placed in 30 DEG C of baking oven elder generation constant temperature and stands 12 hours, rear 120
DEG C stand 24 hours, then roast 750 DEG C of generation sulphur carbon positive electrode coarse granules under nitrogen protection in tube furnace.
(4) above-mentioned coarse granule was dispersed into sulphur carbon positive electrode fine grained by dry method cryomilling 3 hours.
Embodiment 3
A kind of preparation method of lithium-sulfur rechargeable battery sulphur carbon positive electrode, comprising the following steps:
(1) 7.2g poloxamer is added 40 DEG C of warms dissolution 30 minutes in 60g dehydrated alcohol, then by 6g heat cured liquid
Above-mentioned 20 DEG C of clear solution room temperature stirring and dissolving 60 minutes formation solution I is added in phenolic resin.
(2) solution I stoichiometrically is added in 1.15 mMs of sodium thiosulfate and 2 mMs of vulcanized sodium and stirs 5 points
Clock, the molar concentration for being then added 3 mMs is that 0.1mol/L dilute sulfuric acid is stirred to react 3 hours formation colloidal sol II.
(3) colloidal sol II is poured into culture dish, with a thickness of 1mm, is placed in 25 DEG C of baking oven elder generation constant temperature and stands 12 hours, latter 90 DEG C
24 hours are stood, then roasts 600 DEG C of generation sulphur carbon positive electrode coarse granules under protection of argon gas in tube furnace.
It (4) is solvent liquid nitrogen wet ball grinding 2 hours by acetone by above-mentioned coarse granule, latter 30 DEG C are evaporated completely solvent, obtain
The sulphur carbon positive electrode fine grained of dispersion.
Battery made of the sulphur carbon positive electrode made from the method for the present invention, charge and discharge blanking voltage are 1.5-3.0V.It will
Each embodiment is made material and is assembled into 2032 type lithium sulphur button cells and is tested, and obtaining data see the table below:
| Embodiment | 0.1C discharge capacity (mAh/g) for the first time | 50 weeks circulation conservation rates (%) |
| 1 | 865 | 88 |
| 2 | 854 | 87 |
| 3 | 878 | 84 |
As can be seen from the table, battery made of the positive electrode made from the method provided by the present invention, for the first time discharge capacity
Greater than 850mAh/g, circulating battery remains to reach 84% or more capacity retention ratio within 50 weeks, shows to be uniformly embedded into orderly due to sulphur
The structure of mesoporous carbon preferably inhibits sulphur active material in the loss of charge and discharge process.
In conclusion the contents of the present invention are not limited in the above embodiments, the knowledgeable people in same area can
Can propose other embodiments easily within technological guidance's thought of the invention, but this embodiment is included in this hair
Within the scope of bright.
Claims (8)
1. a kind of preparation method of the sulphur carbon positive electrode for lithium-sulfur rechargeable battery, which comprises the following steps:
(1) poloxamer is added to absolute ethanol warm dissolution, adds heat cured liquid phenolic resin, dissolution is stirred at room temperature
Form solution；
(2) stoichiometrically sodium thiosulfate and vulcanized sodium are added in the solution of step (1), stir 5 minutes, is then added
Dilute sulfuric acid the reaction was stirred for 2 to 6 hours formed colloidal sol；
(3) colloidal sol is poured into culture dish and is placed in after baking oven constant temperature is stood the inert atmosphere roasting generation sulphur carbon anode in tube furnace
Material coarse granule；
(4) above-mentioned coarse granule is dispersed into sulphur carbon positive electrode fine grained by cryomilling method.
2. the preparation method for the sulphur carbon positive electrode of lithium-sulfur rechargeable battery according to claim 1, which is characterized in that institute
State poloxamer described in step (1): heat cured liquid phenolic resin: dehydrated alcohol is (0.8~1.35) according to weight ratio: 1:
(6~10).
3. the preparation method for the sulphur carbon positive electrode of lithium-sulfur rechargeable battery according to claim 1, which is characterized in that institute
The solution temperature control of step (1) warm is stated at 30~50 DEG C, warm dissolution time control was at 15~60 minutes；Temperature is stirred at room temperature
At 20~30 DEG C, it is 30~150 minutes that the time, which is stirred at room temperature,.
4. the preparation method for the sulphur carbon positive electrode of lithium-sulfur rechargeable battery according to claim 1, which is characterized in that institute
State in step (1) that dilute sulfuric acid is (1.5~3) by weight in dehydrated alcohol and step (2): 1, dilute sulfuric acid molar concentration is 0.1
~5mol/L；In the step (2), according to chemical reaction equation Na2S2O3+2Na2S+3H2SO4=3Na2SO4+4S+3H2O is to rub
You are than meter, additional amount sodium thiosulfate: vulcanized sodium: sulfuric acid=(1.05~1.15): 2:3.
5. the preparation method for the sulphur carbon positive electrode of lithium-sulfur rechargeable battery according to claim 1, which is characterized in that institute
It states step (3) colloidal sol and pours into being first 20~30 DEG C with a thickness of 0.1~5mm, constant temperature dwell temperature and time and stand 12 of culture dish
Hour, latter 90~120 DEG C stand 24 hours.
6. the preparation method for the sulphur carbon positive electrode of lithium-sulfur rechargeable battery according to claim 1, which is characterized in that institute
Stating step (3) tube furnace and roasting inert atmosphere or inert gas used is argon gas or nitrogen；Maturing temperature is 500~750 DEG C.
7. the preparation method for the sulphur carbon positive electrode of lithium-sulfur rechargeable battery according to claim 1, which is characterized in that institute
Step (4) cryomilling method is stated using dry ball milling or wet ball grinding 2~3 hours, wet ball grinding solvent for use is that nonpolarity is molten
Agent acetone or ether.
8. being used for the sulphur carbon positive electrode of lithium-sulfur rechargeable battery as made from the described in any item preparation methods of claim 1-7.
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| CN107591528A (en) * | 2017-09-26 | 2018-01-16 | 珠海光宇电池有限公司 | Carbon sulphur composite for lithium-sulphur cell positive electrode and preparation method thereof |
| CN113113605B (en) * | 2021-03-22 | 2022-08-09 | 西安交通大学 | Network structure ion conductive adhesive and preparation method and application thereof |
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