CN106058208A - Sulfur-carbon positive pole material for lithium-sulfur secondary battery and preparation method of sulfur-carbon positive pole material - Google Patents
Sulfur-carbon positive pole material for lithium-sulfur secondary battery and preparation method of sulfur-carbon positive pole material Download PDFInfo
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- CN106058208A CN106058208A CN201610627227.8A CN201610627227A CN106058208A CN 106058208 A CN106058208 A CN 106058208A CN 201610627227 A CN201610627227 A CN 201610627227A CN 106058208 A CN106058208 A CN 106058208A
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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
- H01M4/362—Composites
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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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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
- H01M4/13—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
- 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
- H01M4/38—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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- 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 sulfur-carbon positive pole material for a lithium-sulfur secondary battery and a preparation method of the sulfur-carbon positive pole material. The method comprises the following steps: (1) adding poloxamer into anhydrous ethanol, carrying out warm/thermal dissolving, adding thermosetting liquid-state phenol-formaldehyde resin into the transparent solution, and carrying out room-temperature stirred dissolving so as to prepare a solution I; (2) adding sodium thiosulfate and sodium sulfide into the solution I, carrying out stirring for a few minutes, then, adding dilute sulfuric acid, and carrying out a stirred reaction for a period of time so as to prepare sol II; (3) pouring the sol II into a culture dish, putting the culture dish into a baking oven, carrying out constant-temperature standing, and then, carrying out roasting in a tube type furnace so as to produce coarse granules of the sulfur-carbon positive pole material; (4) dispersing the coarse granules into fine granules of the sulfur-carbon positive pole material by a liquid-nitrogen ball milling method. A sulfur positive pole material prepared by a chemical synthesis method is uniformly formed in inside walls of mesoporous carbon, so that the volume expansion of sulfur and the loss of sulfur active substances in an electrolyte are effectively inhibited, the efficiency of electron conduction is increased, and the electric properties are improved.
Description
Technical field
The present invention relates to electrode material of secondary lithium ion battery preparation field, particularly relate to a kind of for lithium sulfur secondary electricity
The sulfur carbon positive electrode in pond and preparation method thereof.
Background technology
In order to alleviate energy starved problem, sulfur materials is exploited out can be as wherein a member of 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 compensate for because of energy deficiency as the newcomer in electrochemical energy family, its generation
The crisis caused, on the other hand, does not discharge any harmful substance, environment will not be caused secondary after using or scrapping yet due to it
Pollute, be a kind of environment-friendly type new forms of energy truly.Sodium-sulphur battery has original advantage for energy storage, is mainly reflected in
Raw material reserves are big, energy and power density is big, efficiency for charge-discharge is high, do not limited by place, the feature such as easy to maintenance.External big
Power (especially Japan) development 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, lead-acid battery not only specific energy is low, and environment all can be caused serious dirt by its manufacture process and old and useless battery
Dye, Li and Co (its positive electrode LiCoO at present in lithium ion battery2) earth reserves the abundantest (especially Co), this
Outer Co is toxic, and its manufacture process and old and useless battery have injury to environment and human body.In contrast, Na and S almost use no
Exhaust.Simple substance Na and S element itself are not have toxicity to human body, and Na and S in old and useless battery almost can with 100% return
Receive.Therefore, either from the point of view of the Development of Novel energy, the saving energy, environmental conservation, or from the strategy of sustainable development
Highly going to weigh and thinking, China's development sodium-sulfur battery energy storage system is necessary completely, makes this technical transform for producing
Power is the most very urgent.
Lithium-sulfur rechargeable battery is because of specific capacity height, aboundresources, with low cost and environmentally friendly and by researcher green grass or young crops
Looking at, but lithium-sulfur rechargeable battery there is also some problems, usual elemental sulfur is the insulator of electronics and ion, needs to add substantial amounts of
Conductive agent, so that reducing the utilization rate of active substance.And in lithium-sulfur cell discharge process, many lithium sulfides of generation are soluble
In electrolyte, the end product lithium sulfide after electric discharge the most easily generates bigger crystal, loses electro-chemical activity, causes battery
Specific capacity declines, and cycle performance is deteriorated.In order to overcome the shortcoming of sulfur poorly conductive, research worker by conductive polymer polymer with
Elemental sulfur is combined, and utilizes electrically conductive composite to form the conductive network of electric transmission, and polymer is because having special structure, Ke Yiqi
To conduction, dispersion, adsorption, improve the utilization ratio of sulfur.Mesoporous carbon first prepared by document [Carbon46 (2008) 229],
Then by melted to sulfur and mesoporous carbon compound.Central South University's patent CN103840143A is also substep preparation S/TiO2Composite,
First mesoporous TiO is prepared2, then carry out heat treated with sulfur.But this compound mode is usually substep to be carried out, and first makes
For going out conductive polymer polymer, then it is combined with each other in modes such as grinding, melted, heat treatments or deposition with sulfur.This compound
The sulfur composite uniformity that mode is formed is very poor, and some sites sulfur is reunited serious, and some site sulfur is lax even without, distribution
The most uneven.Lithium-sulfur rechargeable battery another problem is that the molecule of sulfur is hydrophobic group, and in water, dispersibility is very poor, dissolves the molten of sulfur
Agent is not explosive (CS2) it is exactly the big (CCl of toxicity4, toluene, benzene), in dehydrated alcohol, dispersibility still may be used so that with solvent for be situated between
The difficulty that matter prepares sulfur by chemosynthesis strengthens.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide a kind of for lithium by the chemical synthesis that Water-In-Oil one pot goes out
Sulfur carbon positive electrode of sulfur rechargeable battery and preparation method thereof, its prepared spherical sulfur embeds ordered mesoporous carbons anode composite material
Material restrained effectively sulfur volumetric expansion and the loss in the electrolytic solution of sulfur active substance, improves electronics conduction efficiency, improves
Electrical property.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: a kind of sulfur for lithium-sulfur rechargeable battery
The preparation method of carbon positive electrode, comprises the following steps:
(1) poloxamer adds warm in dehydrated alcohol dissolve, then heat cured liquid phenolic resin is added above-mentioned
Bright solution is stirred at room temperature dissolving and forms solution；
(2) stoichiometrically sodium thiosulfate and sodium sulfide are added in the solution of step (1), stir 5 minutes, then
Add dilute sulfuric acid stirring reaction and form colloidal sol in 2～6 hours；
(3) colloidal sol is poured into culture dish is placed in baking oven constant temperature stand after in tube furnace inert atmosphere roasting generate sulfur carbon
Positive electrode coarse granule；
(4) above-mentioned coarse granule is dispersed into sulfur carbon positive electrode fine grained by cryomilling method.
Poloxamer described in described step (1): heat cured liquid phenolic resin: dehydrated alcohol is (0.8 according to weight ratio
～1.35): 1:(6～10).
Described step (1) warm solution temperature controls at 30～50 DEG C, and warm dissolution time controlled at 15～60 minutes；Room
Temperature whipping temp is at 20～30 DEG C, and the time of being stirred at room temperature is 30～150 minutes.
In described step (1) in dehydrated alcohol and step (2) dilute sulfuric acid by weight being (1.5～3): 1, dilute sulfuric acid mole
Concentration is 0.1～5mol/L；In described step (2), according to chemical reaction equation Na2S2O3+2Na2S+3H2SO4=3Na2SO4+4S
+3H2O is with molar ratio computing, addition sodium thiosulfate: sodium sulfide: sulphuric acid=(1.05～1.15): 2:3.
The thickness of culture dish poured into by described step (3) colloidal sol is 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.
Used by described step (3) tube furnace roasting, inert atmosphere or noble gas are argon or nitrogen；Sintering temperature is 500
～750 DEG C.
Described step (4) cryomilling method uses dry ball milling or wet ball grinding 2～3 hours, wet ball grinding solvent for use
For non-polar solven acetone or ether.
The sulfur carbon positive electrode for lithium-sulfur rechargeable battery that above-mentioned preparation method prepares.
Beneficial effects of the present invention: the sulfur positive electrode prepared by chemical synthesis process is formed uniformly in mesoporous carbon
Wall, restrained effectively sulfur volumetric expansion and the loss in the electrolytic solution of sulfur active substance, improves electronics conduction efficiency, improves
Electrical property.
Detailed description of the invention
Below in conjunction with specific embodiment, the preparation method of the present invention is described in detail.
The preparation method of the sulfur carbon positive electrode for lithium-sulfur rechargeable battery of the present invention, comprises the following steps:
(1) poloxamer adds warm in dehydrated alcohol dissolve, then heat cured liquid phenolic resin is added above-mentioned
Bright solution is stirred at room temperature dissolving and forms solution；
(2) stoichiometrically sodium thiosulfate and sodium sulfide are added in the solution of step (1), stir 5 minutes, then
Add dilute sulfuric acid stirring reaction and form colloidal sol in 2～6 hours；
(3) colloidal sol is poured into culture dish is placed in baking oven constant temperature stand after in tube furnace inert atmosphere roasting generate sulfur carbon
Positive electrode coarse granule；
(4) above-mentioned coarse granule is dispersed into sulfur carbon positive electrode fine grained by cryomilling method.
Poloxamer described in described step (1): heat cured liquid phenolic resin: dehydrated alcohol is (0.8 according to weight ratio
～1.35): 1:(6～10).
Described step (1) warm solution temperature controls at 30～50 DEG C, and warm dissolution time controlled at 15～60 minutes；Room
Temperature whipping temp is at 20～30 DEG C, and the time of being stirred at room temperature is 30～150 minutes.
In described step (1) in dehydrated alcohol and step (2) dilute sulfuric acid by weight being (1.5～3): 1, dilute sulfuric acid mole
Concentration is 0.1～5mol/L；In described step (2), according to chemical reaction equation Na2S2O3+2Na2S+3H2SO4=3Na2SO4+4S
+3H2O is with molar ratio computing, addition sodium thiosulfate: sodium sulfide: sulphuric acid=(1.05～1.15): 2:3.
The thickness of culture dish poured into by described step (3) colloidal sol is 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.
Used by described step (3) tube furnace roasting, inert atmosphere or noble gas are argon or nitrogen；Sintering temperature is 500
～750 DEG C.
Described step (4) cryomilling method uses dry ball milling or wet ball grinding 2～3 hours, wet ball grinding solvent for use
For non-polar solven acetone or ether.
The sulfur carbon positive electrode for lithium-sulfur rechargeable battery that above-mentioned preparation method prepares.
Advantages of the present invention:
1) present invention uses one pot of chemical synthesis process gone out of Water-In-Oil, and oil phase self assembly generates orderly conductive polymer and gathers
While compound, phase sulfur generates and is wrapped up by oil phase, makes sulfur be successfully embed into conductive polymer inner polymer wall.
2) the method makes the sulfur granules of synthesis tiny because of the spacing effect of the ordered space of conductive polymer polymer.
3) carrying out the most in the solution because of chemosynthesis process, then poloxamer surfactants rises as raw material simultaneously
The capillary effect of alleviation oil-water interfaces, whole synthetic environment is homogeneous, makes sulfur granules can be created on macromolecule equably
The inwall of conducting polymer.
4) to make the sulfur granules of formation be close to spherical for water in oil synthetic method.
5) cryomilling ensure that sulfur granules is not oxidized and reduces.
Embodiment 1
The preparation method of a kind of lithium-sulfur rechargeable battery sulfur carbon positive electrode, comprises the following steps:
(1) 7.5g poloxamer adds 40 DEG C of warms in 45g dehydrated alcohol dissolve 30 minutes, then by 7.5g thermosetting liquid
State phenolic resin adds 20 DEG C of stirring and dissolving of above-mentioned clear solution room temperature and forms solution I in 60 minutes.
(2) stoichiometrically 1.05 mMs of sodium thiosulfate and 2 mMs of sodium sulfide are added solution I and stir 5 points
Clock, the molar concentration being subsequently adding 3 mMs is that the stirring reaction of 0.1mol/L dilute sulfuric acid forms colloidal sol II in 3 hours.
(3) pouring in culture dish by colloidal sol II, thickness is 1mm, is placed in baking oven elder generation constant temperature 20 DEG C and stands 12 hours, latter 90 DEG C
Standing 24 hours, then in tube furnace, under argon shield, roasting 500 DEG C generates sulfur carbon positive electrode coarse granule.
(4) above-mentioned coarse granule is dispersed into sulfur carbon positive electrode fine grained for 2 hours by dry method cryomilling.
Embodiment 2
The preparation method of a kind of lithium-sulfur rechargeable battery sulfur carbon positive electrode, comprises the following steps:
(1) 10g poloxamer adds 30 DEG C of warms in 90g dehydrated alcohol dissolve 60 minutes, then by 10g heat cured liquid
Phenolic resin adds 30 DEG C of stirring and dissolving of above-mentioned clear solution room temperature and forms solution I in 30 minutes.
(2) stoichiometrically 11 mMs of sodium thiosulfate and 20 mMs of sodium sulfide are added solution I and stir 5 points
Clock, the molar concentration being subsequently adding 30 mMs is that the stirring reaction of 1mol/L dilute sulfuric acid forms colloidal sol II in 2 hours.
(3) pouring in culture dish by colloidal sol II, thickness is 3mm, is placed in baking oven elder generation constant temperature 30 DEG C and stands 12 hours, rear 120
DEG C stand 24 hours, then in tube furnace under nitrogen protection roasting 750 DEG C generate sulfur carbon positive electrode coarse granule.
(4) above-mentioned coarse granule is dispersed into sulfur carbon positive electrode fine grained for 3 hours by dry method cryomilling.
Embodiment 3
The preparation method of a kind of lithium-sulfur rechargeable battery sulfur carbon positive electrode, comprises the following steps:
(1) 7.2g poloxamer adds 40 DEG C of warms in 60g dehydrated alcohol dissolve 30 minutes, then by 6g heat cured liquid
Phenolic resin adds 20 DEG C of stirring and dissolving of above-mentioned clear solution room temperature and forms solution I in 60 minutes.
(2) stoichiometrically 1.15 mMs of sodium thiosulfate and 2 mMs of sodium sulfide are added solution I and stir 5 points
Clock, the molar concentration being subsequently adding 3 mMs is that the stirring reaction of 0.1mol/L dilute sulfuric acid forms colloidal sol II in 3 hours.
(3) pouring in culture dish by colloidal sol II, thickness is 1mm, is placed in baking oven elder generation constant temperature 25 DEG C and stands 12 hours, latter 90 DEG C
Standing 24 hours, then in tube furnace, under argon shield, roasting 600 DEG C generates sulfur carbon positive electrode coarse granule.
(4) being solvent liquid nitrogen wet ball grinding 2 hours by above-mentioned coarse granule by acetone, latter 30 DEG C are evaporated completely solvent, obtain
Scattered sulfur carbon positive electrode fine grained.
The battery that the sulfur carbon positive electrode prepared by the inventive method is made, discharge and recharge blanking voltage is 1.5-3.0V.Will
Each embodiment prepares material and is assembled into 2032 type lithium sulfur button cells and tests, and obtains data and see table:
| Embodiment | 0.1C discharge capacity first (mAh/g) | Circulation conservation rate (%) in 50 weeks |
| 1 | 865 | 88 |
| 2 | 854 | 87 |
| 3 | 878 | 84 |
As can be seen from the table, the battery that the positive electrode prepared by provider's method of the present invention is made, discharge capacity first
More than 850mAh/g, within 50 weeks, circulating battery remains to reach the capability retention of more than 84%, shows owing to sulfur is uniformly embedded in order
The structure of mesoporous carbon preferably inhibits sulfur active substance in the loss of charge and discharge process.
In sum, present disclosure is not limited in the above embodiments, and the knowledgeable people in same area can
Can propose other embodiment within technological guidance's thought of the present invention easily, but this embodiment is included in this
Within the scope of bright.
Claims (8)
1. the preparation method for the sulfur carbon positive electrode of lithium-sulfur rechargeable battery, it is characterised in that comprise the following steps:
(1) poloxamer adds warm in dehydrated alcohol dissolve, then heat cured liquid phenolic resin is added above-mentioned transparent molten
Liquid chamber temperature stirring and dissolving forms solution；
(2) stoichiometrically sodium thiosulfate and sodium sulfide are added in the solution of step (1), stir 5 minutes, be subsequently adding
Dilute sulfuric acid stirring reaction forms colloidal sol in 2～6 hours；
(3) colloidal sol is poured into culture dish is placed in baking oven constant temperature stand after in tube furnace inert atmosphere roasting generate sulfur carbon positive pole
Material coarse granule；
(4) above-mentioned coarse granule is dispersed into sulfur carbon positive electrode fine grained by cryomilling method.
It is used for the preparation method of the sulfur carbon positive electrode of lithium-sulfur rechargeable battery the most according to claim 1, it is characterised 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).
It is used for the preparation method of the sulfur carbon positive electrode of lithium-sulfur rechargeable battery the most according to claim 1, it is characterised in that institute
Stating step (1) warm solution temperature and control at 30～50 DEG C, warm dissolution time controlled at 15～60 minutes；Temperature is stirred at room temperature
At 20～30 DEG C, the time of being stirred at room temperature is 30～150 minutes.
It is used for the preparation method of the sulfur carbon positive electrode of lithium-sulfur rechargeable battery the most according to claim 1, it is characterised in that institute
Stating in step (1) in dehydrated alcohol and step (2) dilute sulfuric acid by weight for (1.5～3): 1, dilute sulfuric acid molar concentration is 0.1
～5mol/L；In described step (2), according to chemical reaction equation Na2S2O3+2Na2S+3H2SO4=3Na2SO4+4S+3H2O is to rub
You count by ratio, addition sodium thiosulfate: sodium sulfide: sulphuric acid=(1.05～1.15): 2:3.
It is used for the preparation method of the sulfur carbon positive electrode of lithium-sulfur rechargeable battery the most according to claim 1, it is characterised in that institute
Stating step (3) colloidal sol and pouring the thickness of culture dish into is 0.1～5mm, constant temperature dwell temperature and time be first 20～30 DEG C stand 12
Hour, latter 90～120 DEG C stand 24 hours.
It is used for the preparation method of the sulfur carbon positive electrode of lithium-sulfur rechargeable battery the most according to claim 1, it is characterised in that institute
Stating inert atmosphere or noble gas used by step (3) tube furnace roasting is argon or nitrogen；Sintering temperature is 500～750 DEG C.
It is used for the preparation method of the sulfur carbon positive electrode of lithium-sulfur rechargeable battery the most according to claim 1, it is characterised in that institute
Stating step (4) cryomilling method and use dry ball milling or wet ball grinding 2～3 hours, wet ball grinding solvent for use is nonpolar molten
Agent acetone or ether.
8. the sulfur carbon positive electrode for lithium-sulfur rechargeable battery that the preparation method as described in any one of claim 1-7 prepares.
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| CN113113605A (en) * | 2021-03-22 | 2021-07-13 | 西安交通大学 | Network structure ion conductive adhesive and preparation method and application thereof |
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