CN104319404B - A kind of lithium sulphur battery electrode material gelatin polymer binding agent and preparation method thereof - Google Patents
A kind of lithium sulphur battery electrode material gelatin polymer binding agent and preparation method thereof Download PDFInfo
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- CN104319404B CN104319404B CN201410548535.2A CN201410548535A CN104319404B CN 104319404 B CN104319404 B CN 104319404B CN 201410548535 A CN201410548535 A CN 201410548535A CN 104319404 B CN104319404 B CN 104319404B
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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 kind of lithium sulphur battery electrode material gelatin polymer binding agent and preparation method thereof.1,3 dichloro, 2 propanol and Polyethylene Glycol, and mix homogeneously are measured, N is passed through2Deoxygenation, adjusts temperature constant temperature, adds catalyst to accelerate the carrying out of polyreaction, and 1,3 dichloro of extraction target product, 2 propanol polyglycol ether then adjusts solution ph with alkaline solution；（2）Weigh sulfosalt to be completely dissolved in distilled water, adjust temperature constant temperature, add elemental sulfur, prepare many sulphurizing salts；（3）By step（1）1,3 dichloro of product, 2 propanol polyglycol ether and step（2）The mixing of product many sulphurizing salts, adjust temperature constant temperature, take out spawn, and rotate under uniform temperature, you can lithium-sulfur cell gelatin polymer binding agent is obtained.The gelatin polymer binding agent prepared using the present invention has easy to operate, and caking property is good, and electrode active material utilization rate is high, the features such as the good rate capability of battery.
Description
Technical field
The present invention relates to a kind of lithium sulphur battery electrode material gelatin polymer binding agent and preparation method thereof, belongs to lithium sulfur
Battery electrode material preparation field.
Background technology
S8Theoretical specific capacity be 1672 mAh/g, the theoretical discharge voltage of Li/S batteries is 2.287 V, then theoretical energy
Density is 3823.9Wh/kg, contrasts the energy density and relative price of various materials in secondary cell, and elemental sulfur is current energy
Density highest positive electrode, compared with the lithium ion battery of main flow on market, lithium-sulfur cell possesses the former 2 ~ 5 times of theory ratio
Capacity, thus lithium-sulfur cell has good application prospect；The positive electrode of lithium ion battery and lithium-sulfur cell is powder thing
Matter, needs to add binding agent to be mixed and made into slurry, coats the electrode slice that battery is prepared on collector, and binding agent can ensure that work
Uniformity and safety during property material slurrying, between active material particle, and plays between active substance and collector viscous
Knot is acted on, although in lithium ion battery and lithium-sulfur cell, the consumption of binding agent is little, but final performance of its caking property to battery
Have a significant impact, be a kind of important auxiliary material of battery industry.
At present, the oil binder that lithium-sulfur cell is used is mainly Kynoar（PVDF）N-Methyl pyrrolidone it is molten
Liquid, the binding agent have pollution to environment, have certain harm to the health of operator, and expensive, non-conductive；In recent years
Come, the research of aqueous binder also makes some progress, with respect to oil binder for, to more environment-friendly, cost
Can be lower, but its cycle performance and low temperature performance are not as good as oil binder, are slightly short of in terms of practicality, additionally,
Limited to by coating process, in sulfur electrode, the sulfur load capacity of unit area tends to remain in 10mg/cm2Hereinafter, the electrode of thickness
Piece needs higher proportion of binding agent, and sulfur active material ratio in the electrodes will be caused to decline；At the same time, binding agent is not led
Electricity, will cause poor high rate performance, in addition, in charge and discharge process, the dissolving repeatedly of lithium metal and deposition easily form lithium
Dendrite, Li dendrite easily come off from pole plate, cause battery capacity to reduce；If Li dendrite is grown into, barrier film can be pierced through and extended to
Positive pole causes internal short-circuit, causes the unsafe factors such as fire or blast；Simultaneously its activity is too strong, causes it and electrolyte
Interfacial instability.
In the prior art, as general gel type solid electrolyte, 1,3- bis- chloro- 2- propanol gathers PS (DCP-PEG)
Ethylene glycol ether sulfide PS (DCP-PEG) and lithium perchlorate are 8 according to mol ratio:1 ratio is dissolved in tetrahydrofuran, and is fallen
Composite polymer electrolyte membrane is made in entering Teflon mould, and PS (DCP-PEG) is characterized, tested compound
The ionic conductivity of polymer dielectric film, is not yet prepared into battery by the composite electrolyte membrane actual, carries out chemical property
Test.
The content of the invention
To solve the above problems, the invention provides a kind of lithium sulphur battery electrode material with gelatin polymer binding agent and its
Preparation method.
According to an embodiment of the present invention, a kind of lithium-sulfur cell, including sulfur electrode, metal lithium electrode and it is arranged on sulfur
Barrier film and electrolyte between electrode and metal lithium electrode, described gelatin polymer are the bonding used by lithium-sulfur cell sulfur electrode
Agent, belongs to lithium sulphur battery electrode preparation field；Specifically, a kind of lithium sulphur battery electrode material gelatin polymer binding agent,
It is characterized in that：The gelatin polymer binding agent is PS (DCP-PEG).
Another embodiment of the invention, preparation method of the lithium-sulfur cell with gelatin polymer binding agent, its feature
It is to be completed by following steps：
（1）1,3-, bis- chloro- 2- propanol and Polyethylene Glycol are measured, its mol ratio is 1:0.8 ~ 1.5, after mix homogeneously, it is passed through
N2Deoxygenation, adjusts 110 ~ 150 degrees Celsius of temperature, and after addition catalyst, constant temperature 1 ~ 5 hour, extracts target product 1, bis- chloro- 2- of 3-
Propanol polyglycol ether（P(DCP-PEG)）, it is 5 ~ 9 then to adjust solution ph with alkaline solution.
（2）Weigh sulfosalt to be completely dissolved in distilled water, add elemental sulfur, sulfosalt is 1 with the mol ratio of elemental sulfur:1 ~ 7, adjust
30 ~ 90 degrees Celsius of temperature simultaneously constant temperature 1 ~ 5 hour is saved, many sulphurizing salts are prepared.
（3）By step（1）Product P (DCP-PEG) and step（2）The mixing of product many sulphurizing salts, its mol ratio is 1:1
~ 1.3, adjust 45 ~ 90 degrees Celsius of temperature and constant temperature takes out gel-like product PS (DCP-PEG) after 1 ~ 6 hour, under uniform temperature
Revolving, revolving product vacuum can be prepared by lithium-sulfur cell gelatin polymer binding agent after being dried.
Another embodiment of the invention, the preparation method of described lithium-sulfur cell with gelatin polymer binding agent,
It is characterized in that：Described catalyst is concentrated sulphuric acid.
Another embodiment of the invention, the preparation method of described lithium-sulfur cell with gelatin polymer binding agent,
It is characterized in that：The consumption of described catalyst concentrated sulphuric acid is the weight hundred of bis- chloro- 2- propanol of 1,3- and Polyethylene Glycol gross weight
Divide than being 5% ~ 15%.
Another embodiment of the invention, the preparation method of described lithium-sulfur cell with gelatin polymer binding agent,
It is characterized in that：Extraction agent is benzene or toluene.
Another embodiment of the invention, the preparation method of described lithium-sulfur cell with gelatin polymer binding agent,
It is characterized in that：Alkaline solution is sodium hydroxide, and potassium hydroxide, sodium bicarbonate, sodium carbonate are a kind of in potassium carbonate and potassium bicarbonate
Or the aqueous solution of several materials.
Another embodiment of the invention, the preparation method of described lithium-sulfur cell with gelatin polymer binding agent,
It is characterized in that：Sulfosalt is sodium sulfide, Potassium monosulfide., sodium disulfide, one or more in curing potassium.
Described many sulphurizing salts are Na2Sx, the span of x is 2 ~ 8, wherein x>2 effects can be more preferable.
Another embodiment of the invention, the preparation method of described lithium-sulfur cell with gelatin polymer binding agent,
It is characterized in that：Product PS (DCP-PEG) is rotated at 50 ~ 100 degrees Celsius, and is cleaned multiple times with water.
Another embodiment of the invention, lithium sulphur battery electrode piece, it is characterised in that：It is using the preparation side
Gelatin polymer binding agent that method is prepared from and sulfur active material, conductive agent and lithium salts according to certain ratio mix homogeneously,
Wherein, gelatin polymer binding agent for mixture quality 4% ~ 30%, lithium salts for mixture quality 4% ~ 30%, conductive agent be mixed
Compound quality 5 ~ 10%, lithium-sulfur cell sulfur active material for mixture quality 30 ~ 87%, thing mixed above is dissolved in into solvent system
Standby slurry, and equably coat dry on collector forming.
The lithium salts is lithium nitrate, the inorganic or organic lithium salt such as lithium perchlorate.
Binding agent prepared by the present invention can apply to sulfur active material, and this carbon sulfur composite is not limited to nucleocapsid knot
Structure, can also be mesoporous carbon, CNT or other can coat the carbon guest materials of sulfur.
The gelatin polymer binding agent prepared using the present invention has easy to operate, and caking property is good, and electrode active material is utilized
The features such as rate height, good rate capability of battery；As, in charge and discharge process, polysulfide easily to sulfur electrode external diffusion, is made
Into the loss of polysulfide so that the stability difference of lithium-sulfur cell and high rate performance are poor, and the present invention adds also in this kind of binding agent
Enter lithium salts, improve Li+Migration velocity, improve lithium-sulfur cell high rate performance.
The electrode material binding agent of the present invention and its battery performance and application, in the conventional method in this area, that is, are assembled into
Button half-cell or full battery carry out charge-discharge test investigation.
Description of the drawings
Nuclear magnetic resonance spectroscopy spectrograms of the Fig. 1 for the lithium-sulfur cell gelatin polymer binding agent of the embodiment of the present invention 1.
Lithium sulphur battery electrode piece apparent form figures of the Fig. 2 for the embodiment of the present invention 2.
Lithium sulphur battery electrode piece apparent form figures of the Fig. 3 for the embodiment of the present invention 3.
Capacitance-voltage curves figures of the Fig. 4 for the embodiment of the present invention 4.
Cycle-index-discharge capacity curve charts of the Fig. 5 for the embodiment of the present invention 4.
Cycle-index-coulombic efficiency curve charts of the Fig. 6 for the embodiment of the present invention 4.
Specific embodiment
Below, with reference to specific embodiment to a kind of lithium sulphur battery electrode material of the invention with gelatin polymer binding agent and
Its preparation method elaborates, but the present invention is not limited to embodiment.
Preparation of 1 lithium-sulfur cell of embodiment with gelatin polymer binding agent
（1）Measure bis- chloro- 2- propanol 5.16g of 1,3- and PEG400（PEG400）20.8g, after mix homogeneously, is passed through
N2Deoxygenation 60 minutes, adjusts 120 degrees Celsius of temperature, isothermal reaction 3 hours after addition catalyst concentrated sulphuric acid, and the consumption of concentrated sulphuric acid is
The 10% of 1,3- bis- chloro- 2- propanol and Polyethylene Glycol gross weight, extracts target product 1, bis- chloro- 2- propanol polyglycol ethers of 3-（P
(DCP-PEG400)）, it is 6.5 then to adjust solution ph with sodium hydroxide solution.
（2）Weigh sodium sulfide 12.09g to be completely dissolved in distilled water, add Sublimed Sulfur 1.92g, adjust 80 degrees Celsius of temperature
And constant temperature 5 hours, prepare sodium disulfide solution.
（3）By step（1）Product P (DCP-PEG400) and step（2）The mixing of product sodium disulfide, its quality is
10g, adjusts 60 degrees Celsius of temperature and constant temperature takes out lower floor gel-like product PS (DCP-PEG400) after 2 hours, in 60 degrees Celsius
Lower revolving 1 hour, is vacuum dried 48 hours, you can lithium-sulfur cell gelatin polymer binding agent is obtained.
Test sign, the nuclear magnetic resonance spectroscopy collection of illustrative plates of such as Fig. 1 are carried out to gelatin polymer binding agent prepared by above method；
Can be analyzed with the presence of element sulphur in the binding agent, in charge and discharge process according to nuclear magnetic resonance spectroscopy collection of illustrative plates, can be reduced
Polysulfide dissolving in the electrolytic solution, improves the high rate performance of lithium-sulfur cell.
The preparation of 2 lithium sulphur battery electrode piece of embodiment, is not added with lithium salts.
The gelatin polymer binding agent prepared in Example 1, with lithium sulfur battery anode material carbon-sulfur compound and conduction
Agent is dissolved in N-Methyl pyrrolidone solvent by a certain percentage, ultrasound 10 minutes, is coated in current collector aluminum foil, in 50 degrees Celsius
Vacuum drying, is obtained lithium sulphur battery electrode piece；Wherein, the present invention used in be by solwution method prepare nucleocapsid structure
Carbon-sulfur compound, the consist of 10% gelatin polymer binding agent, 85% lithium sulfur battery anode material carbon sulfur of electrode slice are combined
Thing and 5% conductive agent.
Apparent form sign is carried out to electrode slice prepared by above method, SEM figures are as shown in Fig. 2 according to apparent form point
Analysis, it can be seen that the caking property of the binding agent is preferable.
The preparation of 3 lithium sulphur battery electrode piece of embodiment, plus lithium salts.
The gelatin polymer binding agent prepared in Example 1, with lithium sulfur battery anode material carbon-sulfur compound, lithium salts,
And conductive agent is dissolved in N-Methyl pyrrolidone solvent by a certain percentage, ultrasound 10 minutes is coated in current collector aluminum foil, in 50
Degree Celsius vacuum drying, is obtained lithium sulphur battery electrode piece；Wherein, the present invention used in be by solwution method prepare core-shell structure copolymer
The carbon-sulfur compound of structure, lithium salts select lithium perchlorate, electrode slice consist of 9% gelatin polymer binding agent, 77% lithium
Sulphur cell positive electrode material carbon-sulfur compound, 9% lithium salts and 5% conductive agent.
Apparent form analysis is carried out to electrode slice prepared by above method, SEM figures are as shown in Figure 3；According to the scanning electron microscope
Figure can be seen that the binding agent coordinates the caking property that lithium salts is used preferable, and compare with the scanning electron microscope (SEM) photograph of Fig. 2, add lithium salts
Binding agent, the overall bonding of sulfur electrode it is fine, and surface is more smooth.
4 lithium-sulfur cell performance test of embodiment
Electrode slice prepared by Example 3, being assembled into button cell carries out charge-discharge test.
The test curve of button cell is as shown in Fig. 4 ~ 6.
It is assembled into according to the sulfur electrode that the capacitance-voltage curves of Fig. 4 are can be seen that using the gelatin polymer as binding agent
After battery, discharge voltage plateau is very stable, and second voltage platform discharge capacity is approximately 3 times of first voltage platform discharge capacity,
Meet the theoretical curve of lithium-sulfur cell, thus use the binding agent, the charge and discharge process of sulfur electrode has no problem.
The cycle-index tested under 0.5C according to Fig. 5-specific capacity curve, in the 20th circulation, specific capacity is about
710mAh/g, in the 80th circulation, specific capacity is about 620mAh/g, and between 20 ~ 80 circulations, the specific capacity of battery tends to
Constant, specific capacity loss of each circulation in this intercycle is only 0.021%.
The cycle-index tested under 0.5C according to Fig. 6-coulombic efficiency curve, test is as can be seen that in about front 5 circulations
During, coulombic efficiency fluctuation is larger, from 108% ~ 100%, starts coulombic efficiency from the 5th circulation and all fluctuates near 100%,
Fluctuation range is only 99% ~ 100.5%.
Analyzed according to the test curve of Fig. 4 ~ 6, it is known that electricity is assembled into sulfur electrode prepared by the gelatin polymer binding agent
Pond, the stability of battery, coulombic efficiency and high rate performance are preferable.
Claims (10)
1. a kind of lithium sulphur battery electrode piece, is prepared with gelatin polymer binding agent using a kind of lithium sulphur battery electrode material, described
A kind of lithium sulphur battery electrode material gelatin polymer binding agent, be PS (DCP-PEG), it is characterised in that：By gel polymerisation
Thing binding agent and sulfur active material, conductive agent and lithium salts according to certain ratio mix homogeneously, wherein, gelatin polymer binding agent
For the 4%～30% of mixture quality, lithium salts for mixture quality 4%～30%, conductive agent for mixture quality 5～
10%th, lithium-sulfur cell sulfur active material is the 30～87% of mixture quality, thing mixed above is dissolved in solvent and prepares slurry, and
Equably coat drying on collector to form.
2. a kind of lithium sulphur battery electrode piece as claimed in claim 1, it is characterised in that：The lithium salts is lithium nitrate or perchloric acid
Lithium.
3. a kind of lithium sulphur battery electrode piece as claimed in claim 1, it is characterised in that preparation method is as follows：
(1) 1,3-, bis- chloro- 2- propanol and Polyethylene Glycol are measured, its mol ratio is 1:0.8～1.5, after mix homogeneously, it is passed through N2Row
Oxygen, adjusts 110～150 degrees Celsius of temperature, and after addition catalyst, constant temperature 1～5 hour, extracts target product 1, bis- chloro- 2- third of 3-
Alcohol polyglycol ether (P (DCP-PEG)), it is 5～9 then to adjust solution ph with alkaline solution；
(2) weigh sulfosalt to be completely dissolved in distilled water, add elemental sulfur, sulfosalt is 1 with the mol ratio of elemental sulfur:1～7, adjust
30～90 degrees Celsius of temperature constant temperature 1～5 hour, prepare many sulphurizing salts；
(3) the product P (DCP-PEG) of step (1) is mixed with many sulphurizing salts of product of step (2), its mol ratio is 1:1～
1.3, adjust 45～90 degrees Celsius of temperature and constant temperature takes out gel-like product PS (DCP-PEG) after 1～6 hour, in uniform temperature
Lower revolving, revolving product vacuum can be prepared by lithium-sulfur cell gelatin polymer binding agent after being dried.
4. a kind of lithium sulphur battery electrode piece as claimed in claim 3, it is characterised in that：Described catalyst is concentrated sulphuric acid, is used
Measure for bis- chloro- 2- propanol of 1,3- and Polyethylene Glycol gross weight percentage by weight be 5%～15%.
5. a kind of lithium sulphur battery electrode piece as claimed in claim 3, it is characterised in that：Extraction agent is benzene or toluene.
6. a kind of lithium sulphur battery electrode piece as claimed in claim 3, it is characterised in that：Alkaline solution is sodium hydroxide, hydrogen-oxygen
Change potassium, sodium bicarbonate, sodium carbonate, the aqueous solution of one or more materials in potassium carbonate and potassium bicarbonate.
7. a kind of lithium sulphur battery electrode piece as claimed in claim 3, it is characterised in that：Sulfosalt is sodium sulfide, Potassium monosulfide., two sulfur
Change sodium, one or more in curing potassium.
8. a kind of lithium sulphur battery electrode piece as claimed in claim 3, it is characterised in that：Described many sulphurizing salts are Na2Sx, x's
Span is 2～8.
9. a kind of lithium sulphur battery electrode piece as claimed in claim 8, it is characterised in that：x>2.
10. a kind of lithium sulphur battery electrode piece as claimed in claim 3, it is characterised in that：Product PS (DCP-PEG) 50～
100 degrees Celsius of revolvings, and be vacuum dried after being cleaned multiple times with water.
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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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| 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 |
| CN101420047A (en) * | 2008-12-04 | 2009-04-29 | 清华大学 | Preparation of lithium sulfureous secondary battery |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101420047A (en) * | 2008-12-04 | 2009-04-29 | 清华大学 | Preparation of lithium sulfureous secondary battery |
| 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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| 一种含硫聚合物电解质的合成及性能;高安安等;《高分子材料科学与工程》;20100630;第26卷(第6期);摘要，第1节实验部分 * |
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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 |
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