CN108123102A - A kind of preparation method of lithium-sulphur cell positive electrode - Google Patents
A kind of preparation method of lithium-sulphur cell positive electrode Download PDFInfo
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- CN108123102A CN108123102A CN201711415050.6A CN201711415050A CN108123102A CN 108123102 A CN108123102 A CN 108123102A CN 201711415050 A CN201711415050 A CN 201711415050A CN 108123102 A CN108123102 A CN 108123102A
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- positive electrode
- lithium
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- sulphur cell
- mass ratio
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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
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention discloses a kind of preparation method of lithium-sulphur cell positive electrode, and the positive electrode, conductive agent and binding agent press 70 ~ 80：10~15：10 ~ 15 mass ratio is uniformly mixed to form slurry；The positive electrode is 1 in mass ratio by graphene and glucose:2.5 ~ 3.5, it is prepared through ultrasonic disperse, spray pyrolysis processing and carbonization shaping；The preparation it is of low cost, simple for process and can be in continuous production lithium-sulfur cell, electrochemistry specific capacity be high, cycle performance is excellent, stable structure, environmental-friendly, electrochemical performance.The preparation method of the lithium-sulphur cell positive electrode of the present invention effectively by means of metal framework, by the proportioning of rational positive electrode, conductive agent and binding agent, can control the special process of positive electrode, and the lithium-sulphur cell positive electrode of function admirable is made.
Description
Technical field
The present invention relates to technical field of material, more particularly to a kind of preparation method of lithium-sulphur cell positive electrode.
Background technology
Constantly increase with the consumption requirements of world energy sources, the petroleum resources increasingly depleted that can be developed, and environment is dirty
Dye but getting worse, therefore using electrochemical energy storage technology by clean solar energy, wind energy storage recycling is undoubtedly the mankind and exists
21 century solves the problems, such as this most effective approach；In addition mobile electronic device, electric vehicle etc. of people's life are influenced also all
Higher requirement is proposed to following electrochemical energy storage technology.These are required for safe, cheap, high-energy density and long-life
Secondary cell is realized.In many energy storage modes, lithium ion battery is with light weight, capacity is high and the advantages that memory-less effect,
Core status is occupied in current energy storage industry.
Lithium ion battery uses graphite material to contain lithium metal oxide as cathode, LiFePO4, cobalt acid lithium, LiMn2O4 etc.
As anode, using lithium ion between positive and negative anodes " rocking chair effect " capacity is contributed, existing secondary lithium-ion electricity at present
Nonetheless pond itself theoretical specific capacity nearly 300mAh/g is also difficult to the requirement for reaching the secondary cell needed for people, simultaneously
Fuel cell is also more difficult practical in a short time, thus the lithium sulfonium battery with 1650mAh/g theoretical specific capacities becomes current
Most attraction secondary cell system.
Using elemental sulfur as anode, lithium metal just reaches lithium sulfonium battery as cathode, the theory of wherein elemental sulfur than energy
2600Wh/kg, and elemental sulfur is cheap, resourceful, it is environmentally friendly, lithium-ion electric can be substituted to a certain extent
Pond, but the actual specific capacity of lithium sulfonium battery is far smaller than theoretical specific capacity, therefore limit its large-scale utilization.Cause this
The main reason for a phenomenon be lithium-sulfur cell during charge and discharge cycles, polysulfide is soluble in electrolyte, is being cycled
During termination, final product is not completely converted into, causes the loss of active principle, simultaneously because the dissolving of polysulfide is made
Into " shuttle effect " so that the capacity of lithium sulfonium battery is greatly lowered.Therefore lithium sulfonium battery " shuttle effect can be improved by inventing
Should " positive electrode it is very urgent.
Due to a series of deficiencies of the elemental sulfur as positive electrode, scientific research personnel by the use of carbon material and elemental sulfur it is compound as
The research of positive active material is the most universal.Carbon material has good electric conductivity, and structure also can be to the migration of polysulfide
Inhibitory action is played in diffusion.
The content of the invention
It is an object of the invention to provide a kind of specific capacity is high, cycle performance is excellent, stable structure, environmental-friendly lithium sulphur
The preparation method of anode, of low cost, simple for process and can be in continuous production lithium-sulfur cell, the electrochemistry ratio of the preparation
Capacity is high, cycle performance is excellent, stable structure, environmental-friendly, electrochemical performance.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of lithium-sulphur cell positive electrode is provided, is comprised the following steps：
S1. positive electrode, conductive agent and binding agent are taken by 70~80：10~15：10~15 mass ratio uniformly mixes shape
Into slurry；
S2. slurry is made to be uniformly distributed in nickel foam, and makes the nickel foam by the pretreated nickel foam of slurry again
Load sulfur content be 80~120mg/cm2, then at 50~100 DEG C of drying, under vacuum in 50~100 DEG C of dry 12~20h；
Wherein, the positive electrode is 1 in mass ratio by graphene and glucose:2.5~3.5, through ultrasonic disperse, spraying
Pyrolysis processing and carbonization shaping are prepared；The conductive agent is any one of carbon black, acetylene black and graphene；The bonding
At least one of agent PVDF, PVA, PEO, LA132 polyacrylic acid.
Anode prepared by the preparation method of this lithium-sulphur cell positive electrode reduces " the shuttle effect " of lithium-sulfur cell, so as to
Improve the chemical property of positive electrode.
The principle of the present invention is：Mixed uniformly carbohydrate is with carbon material in deionized water solution as persursor material, warp
After ultrasonic atomizatio, during spray pyrolysis, moisture evaporation is heated, material forms the larger structure of specific surface area.
Further, the mass ratio of the positive electrode, conductive agent and binding agent is 75：14：13.
Further, the preparation of the positive electrode comprises the following steps：
Y1. ultrasonic disperse：Graphene and glucose in deionized water solution are mixed, stirred at room temperature in deionized water
Mix 3~8h；The mass ratio of the gross mass and deionized water of the graphene and glucose is 1:25；It is carried out using electromagnetic acoustic device
Ultrasonic disperse, the power of the ultrasonic disperse is 800~850W；Scattered 0.5h, obtains mixed solution；
Y2. spray pyrolysis is handled：It by mixed solution described in step Y1, is atomized by ultrasonic nebulizer, the stream of the atomization
Speed is 250cc/min, by the mixed solution after atomization, is passed through and is connected in advance in the vacuum tube furnace of inert gas, carries out constant temperature
Processing is warming up to 400 DEG C in advance, keeps the temperature 25h；Constant temperature continues 1h again after spraying, after reacting furnace is cooled to room temperature, receives
The product of deposition in collector；
Y3. it is carbonized：The product of deposition is ground in being managed described in step Y2, and the rotating speed of the grinding is 200r/min, institute
The time for stating grinding is 2.5h；It after crossing 100~300 mesh sieves, is put into the vacuum tube furnace for being passed through inert gas, is warming up to 750
DEG C, soaking time 2h treats that vacuum tube furnace is cooled to room temperature.
Further, the inert gas is one kind in nitrogen, argon gas.
The present invention utilizes electromagnetic acoustic device ultrasonic disperse after glucide and other carbon materials are mixed.It will divide
Mixed solution after dissipating is placed in professional container and is sprayed by ultrasonic nebulizer in ELECTROMAGNETIC VACUUM tube furnace, in high pure nitrogen or argon
Protection carries out carbonization treatment, obtained positive electrode under gas.Lithium-sulphur cell positive electrode of the present invention can realize continuous preparation, it is at low cost,
It is environmentally protective, it has a good application prospect.
Compared with the prior art, the present invention has the advantages that：
The preparation method of the lithium-sulphur cell positive electrode of the present invention can pass through rational anode material effectively by means of metal framework
The proportioning of material, conductive agent and binding agent controls the special process of positive electrode, and the lithium-sulphur cell positive electrode of function admirable is made.
At room temperature under the effect of 0.1C current densities, first charge-discharge specific capacity reaches 1450mAh/g, cycles coulomb for the first time
Effect reaches 98%；And with preferable cycle performance, after 500 times cycle, capacity still maintains 88.9%, has good
Commercial application prospect.
The preparation method of the lithium-sulphur cell positive electrode of the present invention is easy to operate, and cost is relatively low, energy conservation and environmental protection, has huge warp
Ji benefit.
Specific embodiment
It is further illustrated the present invention with reference to specific embodiment.Unless stated otherwise, used in the embodiment of the present invention
Raw material and method are this field routinely raw material purchased in market and conventional use of method.
The invention will be further described by the following examples.
The present invention discloses the preparation method of lithium-sulphur cell positive electrode, comprises the following steps：
S1. positive electrode, conductive agent and binding agent are taken by 70~80：10~15：10~15 mass ratio uniformly mixes shape
Into slurry；
S2. slurry is made to be uniformly distributed in nickel foam, and makes the nickel foam by the pretreated nickel foam of slurry again
Load sulfur content be 80~120mg/cm2, then at 50~100 DEG C of drying, under vacuum in 50~100 DEG C of dry 12~20h；
Wherein, the positive electrode is 1 in mass ratio by graphene and glucose:2.5~3.5, through ultrasonic disperse, spraying
Pyrolysis processing and carbonization shaping are prepared；The conductive agent is any one of carbon black, acetylene black and graphene；The bonding
At least one of agent PVDF, PVA, PEO, LA132 polyacrylic acid.
Wherein, the preparation of positive electrode comprises the following steps：
Y1. ultrasonic disperse：Graphene and glucose in deionized water solution are mixed, stirred at room temperature in deionized water
Mix 3~8h；The mass ratio of the gross mass and deionized water of graphene and glucose is 1:25；Ultrasound is carried out using electromagnetic acoustic device
Scattered, the power of ultrasonic disperse is 800~850W；Scattered 0.5h, obtains mixed solution；
Y2. spray pyrolysis is handled：It by mixed solution described in step Y1, is atomized by ultrasonic nebulizer, the flow velocity of atomization is
250cc/min by the mixed solution after atomization, is passed through and is connected in advance in the vacuum tube furnace of inert gas, carries out constant temperature processing,
It is pre- to be warming up to 400 DEG C, keep the temperature 25h；Constant temperature until continue 1h, after reacting furnace is cooled to room temperature, collecting pipe again after spraying
The product of interior deposition；
Y3. it is carbonized：The product of deposition is ground in the pipe of step Y2, and the rotating speed of grinding is 200r/min, the grinding
Time be 2.5h；It after crossing 100~300 mesh sieves, is put into the vacuum tube furnace for being passed through inert gas, is warming up to 750 DEG C, heat preservation
Time is 2h, treats that vacuum tube furnace is cooled to room temperature.
Specific embodiment is as follows.
The preparation of 1 lithium-sulphur cell positive electrode of embodiment
The preparation method of the lithium-sulphur cell positive electrode of the present embodiment, comprises the following steps：
S1. positive electrode, conductive agent and binding agent are taken by 70：15：15 mass ratio is uniformly mixed to form slurry；
S2. slurry is made to be uniformly distributed in nickel foam, and makes the nickel foam by the pretreated nickel foam of slurry again
Load sulfur content be 80mg/cm2, then at 50 DEG C of drying, under vacuum in 100 DEG C of dry 12h；
Wherein, the positive electrode is 1 in mass ratio by graphene and glucose:2.5, through ultrasonic disperse, spray pyrolysis
Processing and carbonization shaping are prepared；The conductive agent is carbon black；The binding agent is PVDF.
Wherein, the preparation of positive electrode comprises the following steps：
Y1. ultrasonic disperse：Graphene and glucose in deionized water solution are mixed, stirred at room temperature in deionized water
Mix 8h；The mass ratio of the gross mass and deionized water of the graphene and glucose is 1:25；Surpassed using electromagnetic acoustic device
Sound disperses, and the power of ultrasonic disperse is 850W；Scattered 0.5h, obtains mixed solution；
Y2. spray pyrolysis is handled：It by the mixed solution of step Y1, is atomized by ultrasonic nebulizer, the flow velocity of the atomization
It for 250cc/min, by the mixed solution after atomization, is passed through and is connected in advance in the vacuum tube furnace of inert gas, carry out at constant temperature
Reason is warming up to 400 DEG C in advance, keeps the temperature 25h；Constant temperature continues 1h again after spraying, after reacting furnace is cooled to room temperature, collects
The product of deposition in pipe；
Y3. it is carbonized：The product of deposition is ground in the pipe of step Y2, and the rotating speed of grinding is 200r/min, grinding when
Between be 2.5h；It after crossing 100~300 mesh sieves, is put into the vacuum tube furnace for being passed through argon gas, is warming up to 750 DEG C, soaking time
For 2h, treat that vacuum tube furnace is cooled to room temperature.
The above-mentioned lithium-sulphur cell positive electrode being prepared, button cell is assembled by cathode of metal lithium sheet in glove box.
Electrolyte is 1M LiTFSI/DOL-DME (volume ratios 1:1), membrane is 2400 microporous barriers of celgard.Using new prestige
(Neware) charge-discharge test instrument carries out battery Xun Huan and high rate performance test, and chemical property test voltage scope is 1.7-
2.8V, current density 0.1C, test temperature are 25 DEG C.Electrochemical property test the results are shown in Table 1.
The preparation of 2 lithium-sulphur cell positive electrode of embodiment
The preparation method of the lithium-sulphur cell positive electrode of the present embodiment, comprises the following steps：
S1. positive electrode, conductive agent and binding agent are taken by 80：10：10 mass ratio is uniformly mixed to form slurry；
S2. slurry is made to be uniformly distributed in nickel foam, and makes the nickel foam by the pretreated nickel foam of slurry again
Load sulfur content be 120mg/cm2, then at 50 DEG C of drying, under vacuum in 100 DEG C of dry 12h；
Wherein, the positive electrode is 1 in mass ratio by graphene and glucose:3.5, through ultrasonic disperse, spray pyrolysis
Processing and carbonization shaping are prepared；The conductive agent is carbon black；The binding agent is PVDF.
Wherein, the preparation of positive electrode comprises the following steps：
Y1. ultrasonic disperse：Graphene and glucose in deionized water solution are mixed, stirred at room temperature in deionized water
Mix 3h；The mass ratio of the gross mass and deionized water of the graphene and glucose is 1:25；Surpassed using electromagnetic acoustic device
Sound disperses, and the power of ultrasonic disperse is 800W；Scattered 0.5h, obtains mixed solution；
Y2. spray pyrolysis is handled：It by the mixed solution of step Y1, is atomized by ultrasonic nebulizer, the flow velocity of the atomization
It for 250cc/min, by the mixed solution after atomization, is passed through and is connected in advance in the vacuum tube furnace of inert gas, carry out at constant temperature
Reason is warming up to 400 DEG C in advance, keeps the temperature 25h；Constant temperature continues 1h again after spraying, after reacting furnace is cooled to room temperature, collects
The product of deposition in pipe；
Y3. it is carbonized：The product of deposition is ground in the pipe of step Y2, and the rotating speed of grinding is 200r/min, grinding when
Between be 2.5h；It after crossing 300 mesh sieves, is put into the vacuum tube furnace for being passed through argon gas, is warming up to 750 DEG C, soaking time 2h,
Treat that vacuum tube furnace is cooled to room temperature.
The preparation and performance test of above-mentioned lithium sulfonium anode are same as Example 1, and electrochemical property test the results are shown in Table
1。
The preparation of 3 lithium-sulphur cell positive electrode of embodiment
The preparation method of the lithium-sulphur cell positive electrode of the present embodiment, it is similar to embodiment, the difference is that, step S1.
Positive electrode, conductive agent and binding agent are taken by 75：14：13 mass ratio is uniformly mixed to form slurry；The positive electrode is by stone
Black alkene and glucose are 1 in mass ratio:3, remaining preparation method is same as Example 1.
Comparative example 1
Application No. CN201310464652.6 disclose the positive electrode that a kind of additives for battery contains the additive and its
Preparation method, additive provided in this comparison are glucose (Glucose) and Super P (or activated carbon, acetylene black, charcoal
It is black) composite material, preparation method is as follows：1g Super P is taken to be scattered in 5g glucose in 80ml deionized waters, in ultrasound
Ultrasonic disperse 10min in cleaning device is transferred in 100mL hydrothermal reaction kettles, 160 DEG C of reaction 48h.It treats after reaction, to filter,
65 DEG C of dryings, grinding, obtain the composite material of glucose and Super P, i.e. additive, are 2 according to mass ratio:3 ratio with
Elemental sulfur mixes and under vacuum tube furnace, after 155 DEG C of calcining 12h, then 300 DEG C of calcining 1h, lithium sulfonium cell positive material is made.
The preparation and performance test of above-mentioned lithium sulfonium anode are same as Example 1, and electrochemical property test the results are shown in Table
1。
Table 1
Claims (4)
1. a kind of preparation method of lithium-sulphur cell positive electrode, which is characterized in that comprise the following steps：
S1. positive electrode, conductive agent and binding agent are taken by 70 ~ 80：10~15：10 ~ 15 mass ratio is uniformly mixed to form slurry；
S2. slurry is made to be uniformly distributed in nickel foam, and makes the nickel foam by the pretreated nickel foam of slurry again
Load sulfur content is 80 ~ 120mg/cm2, then at 50 ~ 100 DEG C of drying, under vacuum in 50 ~ 100 DEG C of dry 12 ~ 20h；
Wherein, the positive electrode is 1 in mass ratio by graphene and glucose:2.5 ~ 3.5, through ultrasonic disperse, spray pyrolysis
Processing and carbonization shaping are prepared；The conductive agent is any one of carbon black, acetylene black and graphene；The binding agent is
At least one of PVDF, PVA, PEO, LA132 polyacrylic acid.
2. the preparation method of lithium-sulphur cell positive electrode according to claim 1, which is characterized in that the positive electrode, conductive agent
Mass ratio with binding agent is 75：14：13.
3. the preparation method of lithium-sulphur cell positive electrode according to claim 1, which is characterized in that the preparation bag of the positive electrode
Include following steps：
Y1. ultrasonic disperse：Graphene and glucose in deionized water solution are mixed, 3 are stirred at room temperature in deionized water
~8h；The mass ratio of the gross mass and deionized water of the graphene and glucose is 1:25；Ultrasound is carried out using electromagnetic acoustic device
Scattered, the power of the ultrasonic disperse is 800 ~ 850W；Scattered 0.5h, obtains mixed solution；
Y2. spray pyrolysis is handled：It by mixed solution described in step Y1, is atomized by ultrasonic nebulizer, the flow velocity of the atomization is
250cc/min by the mixed solution after atomization, is passed through and is connected in advance in the vacuum tube furnace of inert gas, carries out constant temperature processing,
It is pre- to be warming up to 400 DEG C, keep the temperature 25h；Constant temperature until continue 1h, after reacting furnace is cooled to room temperature, collecting pipe again after spraying
The product of interior deposition；
Y3. it is carbonized：The product of deposition is ground in being managed described in step Y2, and the rotating speed of the grinding is 200r/min, described to grind
The time of mill is 2.5h；It after crossing 100~300 mesh sieves, is put into the vacuum tube furnace for being passed through inert gas, is warming up to 750 DEG C, protect
The warm time is 2h, treats that vacuum tube furnace is cooled to room temperature.
4. the preparation method of lithium-sulphur cell positive electrode according to claim 3, which is characterized in that the inert gas for nitrogen,
One kind in argon gas.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104733695A (en) * | 2015-03-27 | 2015-06-24 | 浙江大学 | Carbon/sulfur composite material for lithium-sulfur battery cathode as well as preparation method and application |
| CN106328946A (en) * | 2016-09-05 | 2017-01-11 | 长春劲能科技集团股份有限公司 | Method for preparing nano-micro carbon-sulfur composite by in-situ carbon coating of sulfur |
| CN107403916A (en) * | 2017-07-14 | 2017-11-28 | 贵州鼎玺烯材高科技有限公司 | A kind of positive material for lithium-sulfur battery with the more lithium sulfides of graphene conductive network constraint |
-
2017
- 2017-12-22 CN CN201711415050.6A patent/CN108123102A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104733695A (en) * | 2015-03-27 | 2015-06-24 | 浙江大学 | Carbon/sulfur composite material for lithium-sulfur battery cathode as well as preparation method and application |
| CN106328946A (en) * | 2016-09-05 | 2017-01-11 | 长春劲能科技集团股份有限公司 | Method for preparing nano-micro carbon-sulfur composite by in-situ carbon coating of sulfur |
| CN107403916A (en) * | 2017-07-14 | 2017-11-28 | 贵州鼎玺烯材高科技有限公司 | A kind of positive material for lithium-sulfur battery with the more lithium sulfides of graphene conductive network constraint |
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Application publication date: 20180605 |