CN104319404A - Gel polymer binder for lithium sulfur battery electrode material and preparation method thereof - Google Patents
Gel polymer binder for lithium sulfur battery electrode material and preparation method thereof Download PDFInfo
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- CN104319404A CN104319404A CN201410548535.2A CN201410548535A CN104319404A CN 104319404 A CN104319404 A CN 104319404A CN 201410548535 A CN201410548535 A CN 201410548535A CN 104319404 A CN104319404 A CN 104319404A
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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
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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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
- H01M4/04—Processes of manufacture in general
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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
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Abstract
The invention discloses a gel polymer binder for a lithium sulfur battery electrode material and a preparation method thereof. The preparation method comprises the following steps: (1) weighing 1,3-dichloro-2-propanol and polyethylene glycol, uniformly mixing, introducing N2 to deoxygenize, adjusting temperature, keeping constant temperature, adding a catalyst to accelerate a polymerization reaction, extracting a target product 1,3-dichloro-2-propyl alcohol polyethylene glycol ether, and then adjusting the pH value of the solution with an alkaline solution; (2) weighing a sulfosalt, completely dissolving the sulfosalt in distilled water, adjusting temperature, keeping constant temperature, and adding elemental sulfur to prepare a polysulfide salt; (3) mixing a product 1,3-dichloro-2-propyl alcohol polyethylene glycol ether in the step (1) and a product polysulfide salt in the step (2), adjusting temperature, keeping constant temperature, taking out a gel-like substance, and rotatably evaporating at a certain temperature to obtain a gel polymer binder for a lithium sulfur battery. The gel polymer binder prepared by the invention has the characteristics of easiness in operation, good bonding effect, high electrode active material utilization rate, good battery rate capability and the like.
Description
Technical field
The present invention relates to a kind of lithium sulphur battery electrode material gelatin polymer adhesive and preparation method thereof, belong to lithium sulphur battery electrode field of material preparation.
Background technology
S
8theoretical specific capacity be 1672 mAh/g, the theoretical discharge voltage of Li/S battery is 2.287 V, then theoretical energy density is 3823.9Wh/kg, contrast energy density and the relative price of various material in secondary cell, elemental sulfur is the positive electrode that current energy density is the highest, compared with the lithium ion battery of main flow on market, lithium-sulfur cell has the former theoretical specific capacity of 2 ~ 5 times, and thus lithium-sulfur cell has good application prospect; The positive electrode of lithium ion battery and lithium-sulfur cell is powdered substance, need to add adhesive and be mixed and made into slurry, coat electrode slice battery preparing by collector body, uniformity when adhesive can ensure active material slurrying and fail safe, to between active material particle, and play cementation between active material and collector, although the consumption of adhesive is little in lithium ion battery and lithium-sulfur cell, but the final performance of its caking property to battery has a significant impact, be a kind of important auxiliary material of battery industry.
At present, the 1-METHYLPYRROLIDONE solution of the oil binder mainly Kynoar (PVDF) that lithium-sulfur cell uses, this adhesive has pollution to environment, has certain harm to the health of operating personnel, and expensive, non-conductive; In recent years, the research of aqueous binder also makes some progress, relative oil binder, more friendly to environment, cost also can be lower, but its cycle performance and low temperature serviceability are not as good as oil binder, slightly be short of in practicality, in addition, by the limitation of coating process, in sulfur electrode, the sulphur load capacity of unit are often remains on 10mg/cm
2below, and thick electrode slice needs more a high proportion of adhesive, declines causing sulphur active material ratio in the electrodes; Meanwhile, adhesive is non-conductive, will cause poor high rate performance, and in addition, in charge and discharge process, the dissolving repeatedly of lithium metal and deposition, easily form Li dendrite, and Li dendrite easily comes off from pole plate, causes battery capacity to reduce; If Li dendrite grows gradually, then can pierce through barrier film and extend to positive pole and cause internal short-circuit, cause the unsafe factor such as fire or blast; Simultaneously its activity is too strong, causes it and electrolytical interfacial instability.
In the prior art, PS (DCP-PEG) is as general gel type solid electrolyte, 1,3-bis-chloro-2-propyl alcohol polyethylene glycol ether sulfide PS (DCP-PEG) and lithium perchlorate are dissolved in oxolane according to the ratio that mol ratio is 8:1, and pour in Teflon mould and make composite polymer electrolyte membrane, and PS (DCP-PEG) is characterized, test the ionic conductivity of composite polymer electrolyte membrane, not yet be prepared into battery by actual for this composite electrolyte membrane, carry out electrochemical property test.
Summary of the invention
For solving the problem, the invention provides a kind of lithium sulphur battery electrode material gelatin polymer adhesive and preparation method thereof.
According to an embodiment of the present invention, a kind of lithium-sulfur cell, comprise sulfur electrode, metal lithium electrode and the barrier film be arranged between sulfur electrode and metal lithium electrode and electrolyte, described gelatin polymer is lithium-sulfur cell sulfur electrode adhesive used, belongs to lithium sulphur battery electrode preparation field; Specifically, a kind of lithium sulphur battery electrode material gelatin polymer adhesive, is characterized in that: described gelatin polymer adhesive is PS (DCP-PEG).
According to another embodiment of the present invention, the lithium-sulfur cell preparation method of gelatin polymer adhesive, is characterized in that being completed by following steps:
(1) measure the chloro-2-propyl alcohol of 1,3-bis-and polyethylene glycol, its mol ratio is 1:0.8 ~ 1.5, after mixing, passes into N
2deoxygenation, regulates temperature 110 ~ 150 degrees Celsius, and to add after catalyst constant temperature 1 ~ 5 hour, the extraction chloro-2-propyl alcohol polyglycol ether of target product 1,3-bis-(P (DCP-PEG)), then regulates solution ph to be 5 ~ 9 with alkaline solution.
(2) take sulfosalt to be dissolved in completely in distilled water, add elemental sulfur, the mol ratio of sulfosalt and elemental sulfur is 1:1 ~ 7, regulates temperature 30 ~ 90 degrees Celsius and constant temperature 1 ~ 5 hour, prepares many sulphurizing salts.
(3) product P (DCP-PEG) of step (1) is mixed with the many sulphurizing salts of product of step (2), its mol ratio is 1:1 ~ 1.3, adjustment temperature 45 ~ 90 degrees Celsius also constant temperature takes out gel-like product PS (DCP-PEG) after 1 ~ 6 hour, steam in uniform temperature backspin, revolve after steaming product vacuum drying and can obtain lithium-sulfur cell gelatin polymer adhesive.
According to another embodiment of the present invention, the preparation method of described lithium-sulfur cell gelatin polymer adhesive, is characterized in that: described catalyst is the concentrated sulfuric acid.
According to another embodiment of the present invention, the preparation method of described lithium-sulfur cell gelatin polymer adhesive, is characterized in that: the consumption of the described catalyst concentrated sulfuric acid is the percentage by weight of the chloro-2-propyl alcohol of 1,3-bis-and polyethylene glycol total weight is 5% ~ 15%.
According to another embodiment of the present invention, the preparation method of described lithium-sulfur cell gelatin polymer adhesive, is characterized in that: extraction agent is benzene or toluene.
According to another embodiment of the present invention, the preparation method of described lithium-sulfur cell gelatin polymer adhesive, is characterized in that: alkaline solution is NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, the aqueous solution of one or more materials in potash and saleratus.
According to another embodiment of the present invention, the preparation method of described lithium-sulfur cell gelatin polymer adhesive, is characterized in that: sulfosalt is vulcanized sodium, potassium sulfide, sodium disulfide, one or more in curing potassium.
Described many sulphurizing salts are Na
2s
x, the span of x is 2 ~ 8, and wherein x>2 effect can be better.
According to another embodiment of the present invention, the preparation method of described lithium-sulfur cell gelatin polymer adhesive, is characterized in that: product P S (DCP-PEG) revolves steaming at 50 ~ 100 degrees Celsius, and repeatedly cleans with water.
According to another embodiment of the present invention, lithium sulphur battery electrode sheet, it is characterized in that: it is that the gelatin polymer adhesive adopting described preparation method to be prepared from mixes according to certain ratio with sulphur active material, conductive agent and lithium salts, wherein, gelatin polymer adhesive be mixture quality 4% ~ 30%, lithium salts be mixture quality 4% ~ 30%, conductive agent be mixture quality 5 ~ 10%, lithium-sulfur cell sulphur active material is 30 ~ 87% of mixture quality, above mixture is dissolved in solvent and prepares slurry, and coat drying on collector body equably and form.
Described lithium salts is lithium nitrate, the inorganic or organic lithium salt such as lithium perchlorate.
Adhesive prepared by the present invention can be applied to sulphur active material, and this carbon sulphur composite material is not limited to nucleocapsid structure, can also be mesoporous carbon, carbon nano-tube or other can the carbon guest materials of coated sulphur.
The gelatin polymer adhesive adopting the present invention to prepare has easy to operate, and caking property is good, and electrode active material utilance is high, the features such as the good rate capability of battery; Due in charge and discharge process, polysulfide, easily to sulfur electrode outdiffusion, causes the loss of polysulfide, make the poor stability of lithium-sulfur cell and high rate performance poor, the present invention also adds lithium salts in this kind of adhesive, improve Li
+migration velocity, improve the high rate performance of lithium-sulfur cell.
Electrode material adhesive of the present invention and battery performance thereof and application, with the method for this area routine, be namely assembled into button half-cell or full battery carries out charge-discharge test investigation.
Accompanying drawing explanation
Fig. 1 is the nuclear magnetic resonance spectroscopy spectrogram of the lithium-sulfur cell gelatin polymer adhesive of the embodiment of the present invention 1.
Fig. 2 is the lithium sulphur battery electrode sheet apparent form figure of the embodiment of the present invention 2.
Fig. 3 is the lithium sulphur battery electrode sheet apparent form figure of the embodiment of the present invention 3.
Fig. 4 is the capacitance-voltage curves figure of the embodiment of the present invention 4.
Fig. 5 is the cycle-index-discharge capacity curve chart of the embodiment of the present invention 4.
Fig. 6 is the cycle-index-coulombic efficiency curve chart of the embodiment of the present invention 4.
Embodiment
Below, in conjunction with embodiment, a kind of lithium sulphur battery electrode material of the present invention gelatin polymer adhesive and preparation method thereof is elaborated, but the present invention is not limited to embodiment.
the preparation of gelatin polymer adhesive of embodiment 1 lithium-sulfur cell
(1) measure 1,3-bis-chloro-2-propyl alcohol 5.16g and PEG400 (PEG400) 20.8g, after mixing, pass into N
2deoxygenation 60 minutes, regulate temperature 120 degrees Celsius, to add after the catalyst concentrated sulfuric acid isothermal reaction 3 hours, the consumption of the concentrated sulfuric acid is 1,10% of the chloro-2-propyl alcohol of 3-bis-and polyethylene glycol total weight, the extraction chloro-2-propyl alcohol polyglycol ether of target product 1,3-bis-(P (DCP-PEG400)), then regulates solution ph to be 6.5 with sodium hydroxide solution.
(2) take vulcanized sodium 12.09g to be dissolved in completely in distilled water, add sublimed sulfur 1.92g, regulate temperature 80 degrees Celsius and constant temperature 5 hours, prepare sodium disulfide solution.
(3) product P (DCP-PEG400) of step (1) is mixed with the product sodium disulfide of step (2), its quality is 10g, adjustment temperature 60 degrees Celsius also constant temperature takes out lower floor gel-like product PS (DCP-PEG400) after 2 hours, 1 hour is steamed in 60 degrees Celsius of backspins, vacuumize 48 hours, can obtain lithium-sulfur cell gelatin polymer adhesive.
Test sign is carried out, as the nuclear magnetic resonance spectroscopy collection of illustrative plates of Fig. 1 to gelatin polymer adhesive prepared by above method; Can analyze in this adhesive according to nuclear magnetic resonance spectroscopy collection of illustrative plates has element sulphur to exist, and in charge and discharge process, can reduce polysulfide dissolving in the electrolytic solution, improves the high rate performance of lithium-sulfur cell.
the preparation of embodiment 2 lithium sulphur battery electrode sheet, does not add lithium salts.
The gelatin polymer adhesive of preparation in Example 1, be dissolved in 1-METHYLPYRROLIDONE solvent by a certain percentage with lithium sulfur battery anode material carbon-sulfur compound and conductive agent, ultrasonic 10 minutes, coat in current collector aluminum foil, in 50 degrees Celsius of vacuumizes, obtained lithium sulphur battery electrode sheet; Wherein, in the present invention, use the carbon-sulfur compound of the nucleocapsid structure prepared by solwution method, electrode slice consist of the gelatin polymer adhesive of 10%, the lithium sulfur battery anode material carbon-sulfur compound of 85% and 5% conductive agent.
Carry out apparent form sign to electrode slice prepared by above method, SEM figure as shown in Figure 2, according to apparent form analysis, can find out that the caking property of this adhesive is better.
the preparation of embodiment 3 lithium sulphur battery electrode sheet, adds lithium salts.
The gelatin polymer adhesive of preparation in Example 1, be dissolved in 1-METHYLPYRROLIDONE solvent by a certain percentage with lithium sulfur battery anode material carbon-sulfur compound, lithium salts and conductive agent, ultrasonic 10 minutes, coat in current collector aluminum foil, in 50 degrees Celsius of vacuumizes, obtained lithium sulphur battery electrode sheet; Wherein, the carbon-sulfur compound of the nucleocapsid structure prepared by solwution method is used in the present invention, lithium perchlorate selected by lithium salts, electrode slice consist of 9% gelatin polymer adhesive, 77% lithium sulfur battery anode material carbon-sulfur compound, the lithium salts of 9% and the conductive agent of 5%.
Carry out apparent form analysis to electrode slice prepared by above method, SEM figure as shown in Figure 3; Can find out that the caking property that this adhesive coordinates lithium salts to use is better according to this scanning electron microscope (SEM) photograph, and compare with the scanning electron microscope (SEM) photograph of Fig. 2, add the adhesive of lithium salts, the entirety bonding of sulfur electrode fine, and surface is more smooth.
the performance test of embodiment 4 lithium-sulfur cell
Electrode slice prepared by Example 3, is assembled into button cell and carries out charge-discharge test.
The test curve of button cell is as shown in Fig. 4 ~ 6.
Capacitance-voltage curves according to Fig. 4 can be found out, after being assembled into battery using this gelatin polymer as the sulfur electrode of adhesive, discharge voltage plateau is very stable, second voltage platform discharge capacity is about 3 times of the first voltage platform discharge capacity, meet the theoretical curve of lithium-sulfur cell, thus use this adhesive, the charge and discharge process of sulfur electrode is no problem.
According to cycle-index-specific capacity curve that Fig. 5 tests under 0.5C, 710mAh/g is about the 20th circulation time specific capacity, 620mAh/g is about the 80th circulation time specific capacity, between 20 ~ 80 circulations, the specific capacity of battery is tending towards constant, and the specific capacity loss of each circulation in this intercycle is only 0.021%.
According to cycle-index-coulombic efficiency curve that Fig. 6 tests under 0.5C, test can be found out, in about front 5 cyclic processes, coulombic efficiency fluctuation is larger, from 108% ~ 100%, from the 5th circulation, coulombic efficiency all fluctuates near 100%, and fluctuation range is only 99% ~ 100.5%.
According to the test curve analysis of Fig. 4 ~ 6, the known sulfur electrode prepared with this gelatin polymer adhesive is assembled into battery, and the stability of battery, coulombic efficiency and high rate performance are all better.
Claims (10)
1. a lithium sulphur battery electrode material gelatin polymer adhesive, is characterized in that: described gelatin polymer adhesive is PS (DCP-PEG).
2. the preparation method of a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 1, is characterized in that step is as follows:
(1) measure the chloro-2-propyl alcohol of 1,3-bis-and polyethylene glycol, its mol ratio is 1:0.8 ~ 1.5, after mixing, passes into N
2deoxygenation, regulates temperature 110 ~ 150 degrees Celsius, and to add after catalyst constant temperature 1 ~ 5 hour, the extraction chloro-2-propyl alcohol polyglycol ether of target product 1,3-bis-(P (DCP-PEG)), then regulates solution ph to be 5 ~ 9 with alkaline solution;
(2) take sulfosalt to be dissolved in completely in distilled water, add elemental sulfur, the mol ratio of sulfosalt and elemental sulfur is 1:1 ~ 7, regulates temperature 30 ~ 90 degrees Celsius and constant temperature 1 ~ 5 hour, prepares many sulphurizing salts;
(3) product P (DCP-PEG) of step (1) is mixed with the many sulphurizing salts of product of step (2), its mol ratio is 1:1 ~ 1.3, adjustment temperature 45 ~ 90 degrees Celsius also constant temperature takes out gel-like product PS (DCP-PEG) after 1 ~ 6 hour, steam in uniform temperature backspin, revolve after steaming product vacuum drying and can obtain lithium-sulfur cell gelatin polymer adhesive.
3. the preparation method of a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 2, it is characterized in that: described catalyst is the concentrated sulfuric acid, consumption is the percentage by weight of the chloro-2-propyl alcohol of 1,3-bis-and polyethylene glycol total weight is 5% ~ 15%.
4. the preparation method of a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 2, is characterized in that: extraction agent is benzene or toluene.
5. the preparation method of a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 2, it is characterized in that: alkaline solution is NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, the aqueous solution of one or more materials in potash and saleratus.
6. the preparation method of a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 2, is characterized in that: sulfosalt is vulcanized sodium, potassium sulfide, sodium disulfide, one or more in curing potassium.
7. the preparation method of a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 2, is characterized in that: described many sulphurizing salts are Na
2s
x, the span of x is 2 ~ 8, and wherein x>2 effect can be better.
8. the preparation method of a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 2, is characterized in that: product P S (DCP-PEG) revolves steaming at 50 ~ 100 degrees Celsius, and repeatedly cleans final vacuum drying with water.
9. adopt lithium sulphur battery electrode sheet prepared by a kind of lithium sulphur battery electrode material gelatin polymer adhesive as claimed in claim 1, it is characterized in that: by gelatin polymer adhesive and sulphur active material, conductive agent and lithium salts mix according to certain ratio, wherein, gelatin polymer adhesive is 4% ~ 30% of mixture quality, lithium salts is 4% ~ 30% of mixture quality, conductive agent is 5 ~ 10% of mixture quality, lithium-sulfur cell sulphur active material is 30 ~ 87% of mixture quality, above mixture is dissolved in solvent and prepares slurry, and coat drying on collector body equably and form.
10. lithium sulphur battery electrode sheet as claimed in claim 9, is characterized in that: described lithium salts is lithium nitrate or lithium perchlorate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107863534A (en) * | 2017-10-20 | 2018-03-30 | 电子科技大学 | A kind of polarity bonding agent applied to lithium-sulfur cell and preparation method thereof |
| CN110838577A (en) * | 2018-08-17 | 2020-02-25 | 中国科学院物理研究所 | Sulfur-based positive electrode active material for solid-state battery and preparation method and application thereof |
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| CN101557017A (en) * | 2009-05-08 | 2009-10-14 | 中南大学 | Full solid state polymer electrolyte used for lithium sulphur battery and preparation thereof |
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| CN1499659A (en) * | 2002-10-28 | 2004-05-26 | 三星Sdi株式会社 | Positive electrode of Li-S cell and Li-S cell including such positive electrode |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107863534A (en) * | 2017-10-20 | 2018-03-30 | 电子科技大学 | A kind of polarity bonding agent applied to lithium-sulfur cell and preparation method thereof |
| CN110838577A (en) * | 2018-08-17 | 2020-02-25 | 中国科学院物理研究所 | Sulfur-based positive electrode active material for solid-state battery and preparation method and application thereof |
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Application publication date: 20150128 Assignee: NANTONG HUINENG NICKEL STEEL STRIP CO., LTD. Assignor: Changzhou University Contract record no.: 2018320000127 Denomination of invention: Gel polymer binder for lithium sulfur battery electrode material and preparation method thereof Granted publication date: 20170405 License type: Exclusive License Record date: 20180622 |