CN108365210A - A kind of activated carbon carbon-sulfur materials and its preparation method and application - Google Patents
A kind of activated carbon carbon-sulfur materials and its preparation method and application Download PDFInfo
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- CN108365210A CN108365210A CN201810324954.6A CN201810324954A CN108365210A CN 108365210 A CN108365210 A CN 108365210A CN 201810324954 A CN201810324954 A CN 201810324954A CN 108365210 A CN108365210 A CN 108365210A
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- sulphur
- positive electrode
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/36—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
- 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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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 activated carbon sulphur positive electrode, is raw material by diethylene triamine pentacetic acid (DTPA), potassium hydroxide, absolute ethyl alcohol and sulphur, and by grinding, calcining and fusion method activation obtain.Preparation method includes the following steps：1）Diethylene triamine pentacetic acid (DTPA) and potassium hydroxide mixed grinding are uniform；2）Calcination method prepares active carbon powder；3）The melting of activated carbon sulphur positive electrode activates.As the application of lithium-sulphur cell positive electrode, when current density is 835 mA/cm2（0.5C）When high current charge-discharge, electric discharge for the first time is 774.6 mAh/g, and for special capacity fade to 500 ~ 550 mAh/g, average each attenuation rate is 0.28% after 110 cycles.The present invention has the following advantages：1. preparation method is simple, sulfur content greatly improves；2. successfully inhibiting the dissolving of part polysulfide；3. distributed components effectively inhibit negative plate caused by shuttle effect and the internal resistance of cell to increase；Offer specific discharge capacity is provided, the speed of battery capacity decaying is reduced, improves cycle performance.
Description
Technical field
The invention belongs to battery technology fields, and in particular to a kind of activated carbon-sulphur positive electrode and preparation method thereof and answer
With.
Background technology
With social development, the mankind gradually increase the demand of the energy.However as to changes such as coal, oil, natural gases
The lasting acceleration in nearly 200 years of stone fuel source exploit, resource oneself gradually tend to exhaust.Therefore, energy problem and environmental problem at
For global concern and problem in the urgent need to address.Development with high-energy, high density, high security, it is environmentally protective and it is low at
This secondary cell is of great significance in new energy field.Lithium-sulfur cell is that have higher energy density in secondary cell system
One kind, as a positive electrode active material using elemental sulfur or sulphurous materials, theoretical energy density reaches 2600Wh/kg, and has
The advantages that Sulphur ressource is abundant, environmental-friendly, cheap.The lithium-sulfur cell of high sulfur content has high capacity density and energy close
Degree is conducive to the demand of electric vehicle, can realize that the technology for overcoming lithium ion battery energy density that cannot meet electric vehicle is asked
Topic.
Activated carbon is to be used as the porous carbon materials compound with sulphur earliest.Early in 2002, the sulphur that Wang etc. will just be melted
It is penetrated into the pore structure of activated carbon with the mode of distribution step heat treatment（Document 1：J Wang, L Liu, Z Ling, et
al. Polymer lithium cells with sulfur composites as cathode materials[J].
Electrochimica Acta, 2003,48: 1861-1867.）, 0.3 A cm-1Under current density, sulfur content is 30 wt%
When, specific capacity is 800 mAh g for the first time-1, 25 times cycle after specific capacity be maintained at 440 mAh g-1, but when sulfur content is 60.9
When wt%, specific capacity only has 180 mAh g for the first time-1.The material has the following problems：（1）The load sulfur content of positive electrode is relatively low；
（2）：And specific capacity is very low when carrying sulfur content and being more than 50%.
Zhong etc. is carbonized to obtain the carbon material with layer structure using EDTA, by the distribution step heat treatment of the sulphur of melting
Mode penetrate into material（Document 2：M Zhong a, J Guan, Q Feng, et al Accelerated
polysulfide redox kinetics revealed by ternary sandwichtypeS@Co/N-doped
Carbon nanosheet for high-performance lithium-sulfur batteries [J] Carbon,
2008,128 86-96）335mA cm-1Under current density, when sulfur content is 64 wt%, specific capacity is 1150 mAh g for the first time-1,
Special capacity fade is to 650 mAh g after 50 cycles-1.The material has the following problems：（1）Decay very under larger current charge and discharge
Soon；（2）The stratiform carbon material comparatively dense causes sulfur content to be unevenly distributed to be unable to reach lithium ion fast charging and discharging.
Wu Feng etc. has synthesized the ordered mesopore carbon of high-specific surface area and multi-cellular structure using optimize technique（Document 3：F
Wu, S X Wu, R J Chen, et al. Electrochemical performance of sulfur composite
Materials for rechargeable lithium batteries [J] Chinese Chemical Letters,
2009,20: 1255-1258.）, so that elemental sulfur is distilled by the method for heating and deposit in ordered mesopore carbon micropore, obtain
Carbon sulphur composite material sulfur content 49%, 100mA g-1, under current density, first discharge specific capacity is up to 1180.8 mAh g-1,
Specific capacity is also maintained at 720.4 mAh g after recycling 60 weeks-1.The material has the drawback that（1）：Current density is relatively low；（2）：
And it carries sulfur content and is not above 50%.
Song etc. prepares nanometer Mg using sol-gal process0.6Ni0.40 particle inhibits more vulcanizations as the additive of sulphur anode
Dissolving and promotion redox reaction of the object in electrolyte（Document 4：Min-Sang Song, Sang-Cheol Han, Hyun-
Seok Kim, Jin-Ho Kim, Ki-Tae Kim, Yong-Mook Kang, Hyo-Jun Ahn, S. X. Dou,
Jai-Young Lee.Effects of nanosized adsorbing material on electrochemical
properties of sulfur cathodes for Li/S second batteries. Journal of the
Electrochemical Society. 2004,151 (6):A791-A795）.The material has the drawback that（1）：Colloidal sol
Metal alkoxide cost is higher in gel method；（2）：The shortcomings of self-propagating high-temperature synthesis is not easy to control there are reaction process.
There is also following technical problems as next-generation novel energy battery system for lithium-sulfur cell：
1）Elemental sulfur is insulator；
2）It is very low to carry high current charge-discharge specific capacity when sulfur content is more than 50%；
3）Polysulfide is dissolved causes shuttle effect, positive material utilization ratio few with electrolyte.
Invention content
The object of the present invention is to provide a kind of activated carbon-sulphur positive electrodes, solve following technology existing for lithium-sulfur cell and ask
Topic：
One, the problem of elemental sulfur is electronics and ion insulator at room temperature；
Two, anode carries the relatively low problem of sulfur content；
Three, sulphur is easily soluble in organic electrolyte in the intermediate product polysulfide of electrochemical reduction and causes specific capacity and huge decaying
Problem；
Four, lithium sulfur battery anode material, which does not have multichannel nanostructure, leads to large current density electric attenuation quickly.
In order to solve the problems, such as that above-mentioned these make up the low conductance of elemental sulfur herein by the carbon material for preparing high conductivity
Rate prepares carbon material and the compound quick biography that lithium ion may be implemented of sulphur with nitrogen-doped nanometer sheet by activating pyrolysis
It passs, reaches the raising of high rate charge-discharge efficiency.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is：
Activated carbon-sulphur positive electrode, by diethylene triamine pentacetic acid (DTPA), potassium hydroxide, absolute ethyl alcohol and sulphur be raw material with mass ratio
It is 2:1:（2-3）:（1-2）, active carbon powder is made by calcination method, then logical fusion method activation obtains activated carbon-sulphur anode material
The sulfur content of material, resulting materials is 65 ~ 70 %.
The preparation method of activated carbon-sulphur anode positive electrode, includes the following steps：
Step 1）Calcination method prepares active carbon powder, with certain mass ratio, by diethylene triamine pentacetic acid (DTPA), potassium hydroxide and anhydrous
After ethyl alcohol grinds uniform, drying, it is carbonized in certain condition, finally by washing, you can obtain active carbon powder；
Step 2）Fusion method prepares activated carbon-sulphur positive electrode, by step 1）Gained active carbon powder and sulfur powder are centainly to compare
Example grinding is uniform, is thermally treated resulting in activated carbon-sulphur positive electrode under certain condition
Activated carbon-application of the sulphur anode positive electrode as lithium-sulphur cell positive electrode, when current density is 835 mA/cm2When, for the first time
Specific discharge capacity is 700 ~ 800 mAh/g, after 110 cycles, special capacity fade to 500 ~ 550 mAh/g, to discharge for the first time
68.5%, average each attenuation rate is 0.28%.
The present invention compared with the existing technology, has the following advantages：
1, material of the present invention the experiment proved that, sulfur content greatly improves, and up to 65 ~ 70%, high current charge-discharge specific capacity substantially carries
Height, capacity retention ratio are good.Under 835 mA/ g current densities, up to 700 mAh/g-800 mAh/g, cycle performance is also substantially
It improves, after cycle charge-discharge 110 times, specific discharge capacity is 500 mAh/g-550 mAh/g, and coulombic efficiency is relatively stablized close
100%, there is preferable cycle performance；
2, material of the present invention is improved big by the dissolving of the successful absorbed portion polysulfide of the activated carbon flakelike powder for enriching nitrogen source
Current charge-discharge electrical efficiency and electrochemistry cycle performance；
3, activated carbon-sulphur anode composite material ingredient that prepared by the present invention is very uniform, and sulphur can adequately enter mesoporous and micro-
Inside the carbon of hole, compound is highly uniform.To inhibit the active material of electrode to gradually decrease the generation of phenomenon, also effectively inhibit by
The polysulfide dissolved caused by shuttle principle passes through diaphragm to reach caused negative plate and electricity in the cathode lithium piece of battery
The phenomenon that increase of pond internal resistance, occurs, and then improves the cycle performance of lithium-sulfur cell, reduces the speed of battery capacity decaying；
4, the present invention use homemade active carbon powder is at low cost as carrier, have a safety feature, repeatability is high, production efficiency height and
It can be with large-scale commercial production.
Description of the drawings：
The thermogravimetric curve of Fig. 1 activated carbons-sulphur anode；
Fig. 2 is the electrochemical impedance curve of activated carbon-sulphur anode；
Fig. 3 is prepared lithium-sulfur cell cyclic voltammetry curve figure；
Fig. 4 is prepared lithium-sulfur cell test loop capacity curve figure.
Specific implementation mode
The present invention is described in further detail the content of present invention by embodiment, in conjunction with Figure of description, but is not pair
The restriction of the present invention.
Embodiment
A kind of preparation method of activated carbon-sulphur anode positive electrode, includes the following steps：
Step 1）Calcination method prepares active carbon powder, with certain mass ratio, by diethylene triamine pentacetic acid (DTPA), potassium hydroxide and anhydrous
After ethyl alcohol grinds uniform, drying, it is carbonized in certain condition, finally by washing, you can obtain active carbon powder；
Step 2）Fusion method prepares activated carbon-sulphur positive electrode, by step 1）Gained active carbon powder and sulfur powder are centainly to compare
Example grinding is uniform, is thermally treated resulting in activated carbon-sulphur positive electrode under certain condition
The present embodiment lithium sulfur battery anode material (mass fraction for accounting for lithium-sulphur cell positive electrode is 80%), acetylene black conductor (are accounted for
The mass fraction of lithium-sulphur cell positive electrode is that 10%) (mass fraction for accounting for lithium-sulphur cell positive electrode is 10%, and binder is with binder
The Kynoar solution of 15wt%) fully dispersed grinding uniformly obtains anode sizing agent, by anode sizing agent obtained coated in aluminium foil
Electrode slice is made on collector, drying obtains lithium-sulphur cell positive electrode.
Lithium-sulphur cell positive electrode manufactured in the present embodiment, cathode (metal lithium sheet) and diaphragm (polyethylene film) are assembled into together
Lithium-sulfur cell, the electrolyte solution filled in battery are 1,3 one dioxolanes, glycol dimethyl ether, trifluoromethane sulfonic acid imines
The mixed solution of lithium.
The activated carbon of gained-sulphur anode positive electrode is through electro-chemical test, as a result such as Fig. 1, shown in 2, the material have compared with
Good electric conductivity and cycle performance.
In order to verify in activated carbon-sulphur anode positive electrode, element sulphur accounts for the content in positive electrode, by activated carbon-sulphur
Anode has carried out thermogravimetric analysis, and it is 66.5% to measure distillation sulfur content.
Fig. 3 is test loop design sketch of the lithium-sulfur cell in lithium-sulfur cell prepared by the present embodiment, can from Fig. 3
To find out, 835mA/cm2Under current density, the lithium-sulfur cell first discharge specific capacity of the present embodiment is 774.6 mAh/g, 110
Special capacity fade is to 526.9 mAh/g after secondary cycle；The lithium-sulfur cell of the present embodiment has higher specific capacity and cyclicity
Energy.
Claims (7)
1. a kind of activated carbon-sulphur positive electrode, it is characterised in that：With diethylene triamine pentacetic acid (DTPA), potassium hydroxide, absolute ethyl alcohol
It is raw material with sulphur, by grinding, calcination method synthesizing activity carbon powder, then is activated by fusion method and obtain activated carbon-sulphur anode material
The sulfur content of material, the activated carbon-sulphur positive electrode is 65 ~ 70 %.
2. a kind of preparation method of activated carbon-sulphur positive electrode, it is characterised in that include the following steps：
Step 1）Calcination method prepares active carbon powder, with certain mass ratio, by diethylene triamine pentacetic acid (DTPA), potassium hydroxide and anhydrous
After ethyl alcohol grinds uniform, drying, it is carbonized in certain condition, finally by washing, you can obtain active carbon powder；
Step 2）Fusion method prepares activated carbon-sulphur positive electrode, by step 1）Gained active carbon powder and sulfur powder are centainly to compare
Example grinding is uniform, is thermally treated resulting in activated carbon-sulphur positive electrode under certain condition.
3. preparation method according to claim 2, it is characterised in that：The step 1）Diethylene triamine pentacetic acid (DTPA), hydrogen-oxygen
The mass ratio for changing potassium, absolute ethyl alcohol and sulphur is 2:1:（2-3）:（1-2）, the step 1）Carbonization Conditions with heating rate be 5-
10 DEG C/min, 1-3 h are kept the temperature at 700-750 DEG C and are carbonized.
4. preparation method according to claim 2, it is characterised in that：The step 2）Sulphur and step 1）Active powdered carbon
End mass ratio be（3-5）:1.
5. preparation method according to claim 2, it is characterised in that：The step 2）The condition of heat treatment is with heating
Rate is that 2-3 DEG C/min rises to 10~15h of heat preservation at 150-160 DEG C, is continuously heating to 280-300 DEG C and keeps the temperature 30 ~ 40 points
Clock.
6. a kind of activated carbon-application of the sulphur positive electrode as lithium-sulphur cell positive electrode, it is characterised in that：When current density is 835
mA/cm2When, first discharge specific capacity is 700 ~ 800 mAh/g.
7. a kind of activated carbon-application of the sulphur positive electrode as lithium-sulphur cell positive electrode, it is characterised in that：After 110 cycles,
Special capacity fade is to 500 ~ 550 mAh/g, and for 68.5 % to discharge for the first time, average each attenuation rate is 0.28%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112409028A (en) * | 2020-10-28 | 2021-02-26 | 桂林电子科技大学 | CC-NiO-CuCoS composite material and preparation method and application thereof |
| CN112838215A (en) * | 2021-03-04 | 2021-05-25 | 桂林电子科技大学 | Three-dimensional porous carbon nanosheet-sulfur material and preparation method and application thereof |
| CN114583145A (en) * | 2022-03-25 | 2022-06-03 | 江西省纳米技术研究院 | Lithium-sulfur battery positive electrode material, preparation method thereof and lithium-sulfur battery |
| CN114583146A (en) * | 2022-05-06 | 2022-06-03 | 湖南大学 | Preparation method of sodium-sulfur battery positive electrode material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112409028A (en) * | 2020-10-28 | 2021-02-26 | 桂林电子科技大学 | CC-NiO-CuCoS composite material and preparation method and application thereof |
| CN112838215A (en) * | 2021-03-04 | 2021-05-25 | 桂林电子科技大学 | Three-dimensional porous carbon nanosheet-sulfur material and preparation method and application thereof |
| CN114583145A (en) * | 2022-03-25 | 2022-06-03 | 江西省纳米技术研究院 | Lithium-sulfur battery positive electrode material, preparation method thereof and lithium-sulfur battery |
| CN114583145B (en) * | 2022-03-25 | 2023-11-03 | 江西省纳米技术研究院 | Lithium-sulfur battery positive electrode material, preparation method thereof and lithium-sulfur battery |
| CN114583146A (en) * | 2022-05-06 | 2022-06-03 | 湖南大学 | Preparation method of sodium-sulfur battery positive electrode material |
| CN114583146B (en) * | 2022-05-06 | 2022-07-29 | 湖南大学 | Preparation method of sodium-sulfur battery positive electrode material |
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