CN107697901A - A kind of preparation method of high circulation Life Type lithium sulfur battery anode material - Google Patents

A kind of preparation method of high circulation Life Type lithium sulfur battery anode material Download PDF

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Publication number
CN107697901A
CN107697901A CN201710933593.0A CN201710933593A CN107697901A CN 107697901 A CN107697901 A CN 107697901A CN 201710933593 A CN201710933593 A CN 201710933593A CN 107697901 A CN107697901 A CN 107697901A
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parts
prepared
anode material
battery anode
type lithium
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吴迪
季美
史玉兰
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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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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
    • 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 relates to a kind of preparation method of high circulation Life Type lithium sulfur battery anode material, belong to battery material technical field.Luffa is taken, luffa fritter and lithium chloride solution are reacted, filters and collects filter cake, is washed, dries, is prepared into dry loofah fiber；Weigh loofah fiber, peach gum powder, deionized water to be placed in beaker, reaction is poured into mould, is solidified, the demoulding, is excluded air, insulation calcining, is stood cooling, blapharoplast must be carbonized by grinding；Charing blapharoplast is prepared into modified matrix particle with hydrochloric acid reaction, elemental sulfur is mixed with modified matrix particle and is placed in quartz ampoule, sealed silica envelope simultaneously vacuumizes, and heating heating, insulation reaction, stands cooling, collects mixture, obtain composite particles；Weigh liquor kalii iodide, hydrochloric acid and composite particles to be placed in beaker, be stirred and still aging, filter and rinse, vacuum drying can be prepared into a kind of high circulation Life Type lithium sulfur battery anode material.

Description

A kind of preparation method of high circulation Life Type lithium sulfur battery anode material
Technical field
The present invention relates to a kind of preparation method of high circulation Life Type lithium sulfur battery anode material, belong to battery material technology Field.
Background technology
With the progress and development of society, the mankind gradually increase for the demand of the energy.However as to coal, oil, day The fossil fuel resource lasting acceleration of the nearly 200 years exploitation such as right gas, resource progressively tend to exhaust.Meanwhile the fossil such as oil The use of the energy generates substantial amounts of greenhouse gases, generates greenhouse effects, brings serious environmental problem.Accordingly, it is capable to source Problem and environmental problem turn into global concern and it is in the urgent need to address the problem of.China is shortage of resources country, according to relevant information, The occupancy volume per persons such as China's coal, oil, natural gas are only 70%, 11%, the 4% of world occupancy volume per person respectively.With China's economy Increased every year with 8% speed, the non-renewable energy resources such as oil are largely consumed, and the waste gas of discharge equally also brings serious Environmental problem, China major part city is caused haze weather occur, the severe exacerbation living environment of people.Therefore, than it He is national, and craving of the China to new and renewable sources of energy seems particularly urgent.Sub- battery is the secondary cell conduct of representative A kind of energy storage device that easily can be recycled, have been widely used for the side such as mobile phone, notebook computer and electric bicycle Face.In the case of energy crisis getting worse, countries in the world fall over each other to propose the target of development New-energy electric vehicle, and electric There is an urgent need to high-energy-density, the support of secondary cell system again for the exploitation of electrical automobile.So far, lithium ion battery is current The battery system that performance is best in secondary cell is commercialized, but because it mainly uses LiFeO4、LiCoO2And LiNi1/3Co1/ 3Mn1/3O2Deng being used as positive electrode, and the theoretical capacity of these positive electrodes is usually no more than 300mAhg-1, it is difficult to meet mesh The preceding demand for high-specific energy battery, therefore the positive electrode for developing high theoretical specific capacity turns into the emphasis studied now.It is single Matter sulphur is at normal temperatures mainly with S8Form exist, the rich reserves in the earth, have the characteristics that cheap, environment-friendly. By the use of sulphur as the lithium-sulfur cell of positive electrode, its materials theory specific capacity and battery theory are higher than energy, respectively reach 1672mAh·g-1And 2600Whkg-1[12-13], at present the actual energy density of lithium-sulfur cell reached 390Whkg-1, It is expected that 600Whkg is very likely brought up in a few years from now on-1, it is considered to be present most researching value and application prospect One of lithium secondary battery system.Therefore, research high-performance lithium-sulfur cell has important theory and realistic meaning.
The content of the invention
The technical problems to be solved by the invention：For lithium sulfur battery anode material active material utilization it is low, circulation the longevity Order the problem of low, there is provided a kind of preparation method of high circulation Life Type lithium sulfur battery anode material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Take luffa and be cut to luffa fritter, luffa fritter and the lithium chloride solution of mass fraction 5% are stirred mixed Close, heating water bath simultaneously filters, and collects filter cake, washing, dries, be prepared into dry loofah fiber；
（2）Count in parts by weight, respectively weigh 45~50 parts of dry loofah fibers, 10~15 parts of peach gum powder, 55~60 parts Deionized water is placed in beaker, is stirred and is poured into mould, after standing solidification, is stripped and is collected presoma, be placed in pipe In formula atmosphere furnace, lead to nitrogen and exclude air, insulation calcining, standing is cooled to room temperature, and grinding is prepared into charing blapharoplast；
（3）In mass ratio 1:5, charing blapharoplast is stirred with hydrochloric acid, stands, filter, washing, drying are prepared into modification Blapharoplast；
（4）In mass ratio 2:3, elemental sulfur is mixed with modified matrix particle and is placed in quartz ampoule, leads to argon gas and excludes air, it is close Envelope quartz ampoule is simultaneously vacuumized, and heating is heated and is passed through argon gas, and after insulation reaction, standing is cooled to room temperature, and stopping is passed through argon gas simultaneously Mixture is collected, obtains composite particles；
（5）Count in parts by weight, weigh 45~50 parts of liquor kalii iodides, 3~5 parts of hydrochloric acid and 10~15 parts of composite particles respectively and put In beaker, be stirred and still aging, filter filter cake and wash, dry, you can be prepared into a kind of high circulation Life Type Lithium sulfur battery anode material.
Step（2）Described insulation calcining heat is 780~850 DEG C.
Step（4）The described argon gas speed that is passed through is 25~30mL/min.
Step（4）Described vacuumizes to be evacuated to 3~5Pa.
Compared with other method, advantageous effects are the present invention：
The present invention is compound by loofah fiber and peach gum, and forming hole through high temperature carbonization enriches carbon material, due to carbon fiber In contain a large amount of holes, be modified through acidleach, take out its pore interior impurity and by peach gum cured fiber pore interior, pass through acid During leaching, the small proton H of radius+The big cation of radius is displaced, after pickling, by washing regulation pH to neutrality, so as to improve Carbon material internal gutter system, increase specific surface area, increase substantially absorption property, so as to after high temperature deposition, make list Matter sulphur uniform load effectively improves the closely knit performance of material and compatibility performance, had in fast charging and discharging to carbon material pore interior Higher reversible capacity, and the decay of specific capacity is slow.
Embodiment
Take luffa and be cut to luffa fritter, luffa fritter and the lithium chloride solution of mass fraction 5% are stirred mixed Close, at 45~50 DEG C after 3~5h of heating water bath, filter and collect filter cake, washed successively respectively with absolute ethyl alcohol and deionized water Wash 3~5 times, 6~8h is dried at 65~80 DEG C, is prepared into dry loofah fiber；Count in parts by weight, respectively weigh 45~ 50 parts of dry loofah fibers, 10~15 parts of peach gum powder, 55~60 parts of deionized waters are placed in beaker, are stirred and are poured into a mould Into mould, after standing 20~24h of solidification at room temperature, it is stripped and collects presoma and be placed in tube-type atmosphere furnace, lead to nitrogen Air is excluded, at 780~850 DEG C after 2~3h of insulation calcining, standing is cooled to room temperature, and grinding is prepared into charing blapharoplast； In mass ratio 1:5, charing blapharoplast is stirred with 0.2mol/L hydrochloric acid, after standing 3~5h at room temperature, filtering is used in combination Deionized water rinsing 3~5 times, vacuum drying are prepared into modified matrix particle, in mass ratio 2:3, by 200 mesh elemental sulfurs and modification Blapharoplast mixing is placed in quartz ampoule, is led to argon gas and is excluded air, and sealed silica envelope is simultaneously evacuated to 3~5Pa, heating heating To 450~550 DEG C, pressurize is simultaneously passed through argon gas to quartz ampoule, and it is 25~30mL/min to control argon gas flow velocity, and insulation reaction 25~ After 30min, standing is cooled to room temperature, and stopping is passed through argon gas and collects mixture, obtains composite particles；Count in parts by weight, respectively 45~50 parts of liquor kalii iodides of mass fraction 10%, 3~5 parts of hydrochloric acid of mass fraction 5% and 10~15 parts of composite particles are weighed to put In beaker, it is stirred and still aging 3~5h, filters filter cake and to be rinsed 3~5 times with deionized water and absolute ethyl alcohol, Vacuum drying can be prepared into a kind of high circulation Life Type lithium sulfur battery anode material.
Example 1
Take luffa and be cut to luffa fritter, luffa fritter and the lithium chloride solution of mass fraction 5% are stirred, At 45 DEG C after heating water bath 3h, filter and collect filter cake, washed 3 times successively respectively with absolute ethyl alcohol and deionized water, at 65 DEG C Lower dry 6h, is prepared into dry loofah fiber；Count in parts by weight, weigh 45 portions of dry loofah fibers, 10 portions of peaches respectively Rubber powder end, 55 parts of deionized waters are placed in beaker, are stirred and are poured into mould, after standing solidification 20h at room temperature, are taken off Mould is simultaneously collected presoma and is placed in tube-type atmosphere furnace, leads to nitrogen and excludes air, at 780 DEG C after insulation calcining 2h, stands cold But it is prepared into charing blapharoplast to room temperature, grinding；In mass ratio 1:5, charing blapharoplast and 0.2mol/L hydrochloric acid are stirred Mixing, after standing 3h at room temperature, filter and with deionized water rinsing 3 times, be dried in vacuo and be prepared into modified matrix particle, by matter Measure ratio 2:3,200 mesh elemental sulfurs are mixed with modified matrix particle and are placed in quartz ampoule, leads to argon gas and excludes air, sealing quartz Manage and be evacuated to 3Pa, heating is heated to 450 DEG C, and pressurize is simultaneously passed through argon gas to quartz ampoule, and it is 25mL/ to control argon gas flow velocity After min, insulation reaction 25min, standing is cooled to room temperature, and stopping is passed through argon gas and collects mixture, obtains composite particles；By weight Number meter, 45 parts of liquor kalii iodides of mass fraction 10%, 3 parts of hydrochloric acid of mass fraction 5% and 10 parts of composite particles are weighed respectively and are put In beaker, it is stirred and still aging 3h, filters filter cake and to be rinsed 3 times with deionized water and absolute ethyl alcohol, vacuum is done It is dry to be prepared into a kind of high circulation Life Type lithium sulfur battery anode material.
Example 2
Take luffa and be cut to luffa fritter, luffa fritter and the lithium chloride solution of mass fraction 5% are stirred, At 47 DEG C after heating water bath 4h, filter and collect filter cake, washed 4 times successively respectively with absolute ethyl alcohol and deionized water, at 72 DEG C Lower dry 7h, is prepared into dry loofah fiber；Count in parts by weight, weigh 47 portions of dry loofah fibers, 12 portions of peaches respectively Rubber powder end, 57 parts of deionized waters are placed in beaker, are stirred and are poured into mould, after standing solidification 22h at room temperature, are taken off Mould is simultaneously collected presoma and is placed in tube-type atmosphere furnace, leads to nitrogen and excludes air, at 815 DEG C after insulation calcining 2h, stands cold But it is prepared into charing blapharoplast to room temperature, grinding；In mass ratio 1:5, charing blapharoplast and 0.2mol/L hydrochloric acid are stirred Mixing, after standing 4h at room temperature, filter and with deionized water rinsing 4 times, be dried in vacuo and be prepared into modified matrix particle, by matter Measure ratio 2:3,200 mesh elemental sulfurs are mixed with modified matrix particle and are placed in quartz ampoule, leads to argon gas and excludes air, sealing quartz Manage and be evacuated to 4Pa, heating is heated to 500 DEG C, and pressurize is simultaneously passed through argon gas to quartz ampoule, and it is 27mL/ to control argon gas flow velocity After min, insulation reaction 27min, standing is cooled to room temperature, and stopping is passed through argon gas and collects mixture, obtains composite particles；By weight Number meter, 47 parts of liquor kalii iodides of mass fraction 10%, 4 parts of hydrochloric acid of mass fraction 5% and 13 parts of composite particles are weighed respectively and are put In beaker, it is stirred and still aging 4h, filters filter cake and to be rinsed 4 times with deionized water and absolute ethyl alcohol, vacuum is done It is dry to be prepared into a kind of high circulation Life Type lithium sulfur battery anode material.
Example 3
Take luffa and be cut to luffa fritter, luffa fritter and the lithium chloride solution of mass fraction 5% are stirred, At 50 DEG C after heating water bath 5h, filter and collect filter cake, washed 5 times successively respectively with absolute ethyl alcohol and deionized water, at 80 DEG C Lower dry 8h, is prepared into dry loofah fiber；Count in parts by weight, weigh 50 portions of dry loofah fibers, 15 portions of peaches respectively Rubber powder end, 60 parts of deionized waters are placed in beaker, are stirred and are poured into mould, after standing solidification 24h at room temperature, are taken off Mould is simultaneously collected presoma and is placed in tube-type atmosphere furnace, leads to nitrogen and excludes air, at 850 DEG C after insulation calcining 3h, stands cold But it is prepared into charing blapharoplast to room temperature, grinding；In mass ratio 1:5, charing blapharoplast and 0.2mol/L hydrochloric acid are stirred Mixing, after standing 5h at room temperature, filter and with deionized water rinsing 5 times, be dried in vacuo and be prepared into modified matrix particle, by matter Measure ratio 2:3,200 mesh elemental sulfurs are mixed with modified matrix particle and are placed in quartz ampoule, leads to argon gas and excludes air, sealing quartz Manage and be evacuated to 5Pa, heating is heated to 550 DEG C, and pressurize is simultaneously passed through argon gas to quartz ampoule, and it is 30mL/ to control argon gas flow velocity After min, insulation reaction 30min, standing is cooled to room temperature, and stopping is passed through argon gas and collects mixture, obtains composite particles；By weight Number meter, 50 parts of liquor kalii iodides of mass fraction 10%, 5 parts of hydrochloric acid of mass fraction 5% and 15 parts of composite particles are weighed respectively and are put In beaker, it is stirred and still aging 5h, filters filter cake and to be rinsed 5 times with deionized water and absolute ethyl alcohol, vacuum is done It is dry to be prepared into a kind of high circulation Life Type lithium sulfur battery anode material.
A kind of high circulation Life Type lithium sulfur battery anode material being prepared into is detected, drawn to draw a conclusion：
（1）Not plus the circulation specific discharge capacities of battery 200 times of S powder are 533 mAhg-1；After adding S powder, the electric discharge of battery is held Amount is in rise trend always in first 40 times circulations, and capacity is begun to decline after 40 circulations, to 200 circulation specific discharge capacities still There are 948.2 mAhg-1, show excellent cycle performance.
（2）After 200 charge and discharge cycles, SEM tests are carried out to the both positive and negative polarity pole piece of battery, test result indicates that battery Middle addition S powder is easier to form passivating film in negative pole, effectively prevents the generation of Li dendrite；Play and subtract in electrode reaction simultaneously Few Li2S and Li2S2Deng the effect of the deposition of insoluble matter, reduce the loss of active material, improve the electrochemistry of battery Energy.
（3）The LiNO of different content is added in the electrolytic solution3, influence of the electrolyte to AOPC/S battery performances, experiment knot Fruit shows to work as LiNO3Content be 0.1molL-1When, AOPC/S first discharge specific capacity is 1228.6 mAhg-1, 50 times recycle ratio capability retention is 85.8%, has optimal cyclical stability.

Claims (4)

1. a kind of preparation method of high circulation Life Type lithium sulfur battery anode material, it is characterised in that specifically preparation process is：
（1）Take luffa and be cut to luffa fritter, luffa fritter and the lithium chloride solution of mass fraction 5% are stirred mixed Close, heating water bath simultaneously filters, and collects filter cake, washing, dries, be prepared into dry loofah fiber；
（2）Count in parts by weight, respectively weigh 45~50 parts of dry loofah fibers, 10~15 parts of peach gum powder, 55~60 parts Deionized water is placed in beaker, is stirred and is poured into mould, after standing solidification, is stripped and is collected presoma, be placed in pipe In formula atmosphere furnace, lead to nitrogen and exclude air, insulation calcining, standing is cooled to room temperature, and grinding is prepared into charing blapharoplast；
（3）In mass ratio 1:5, charing blapharoplast is stirred with hydrochloric acid, stands, filter, washing, drying are prepared into modification Blapharoplast；
（4）In mass ratio 2:3, elemental sulfur is mixed with modified matrix particle and is placed in quartz ampoule, leads to argon gas and excludes air, it is close Envelope quartz ampoule is simultaneously vacuumized, and heating is heated and is passed through argon gas, and after insulation reaction, standing is cooled to room temperature, and stopping is passed through argon gas simultaneously Mixture is collected, obtains composite particles；
（5）Count in parts by weight, weigh 45~50 parts of liquor kalii iodides, 3~5 parts of hydrochloric acid and 10~15 parts of composite particles respectively and put In beaker, be stirred and still aging, filter filter cake and wash, dry, you can be prepared into a kind of high circulation Life Type Lithium sulfur battery anode material.
2. a kind of preparation method of high circulation Life Type lithium sulfur battery anode material according to claim 1, its feature exist In：Step（2）Described insulation calcining heat is 780~850 DEG C.
3. a kind of preparation method of high circulation Life Type lithium sulfur battery anode material according to claim 1, its feature exist In：Step（4）The described argon gas speed that is passed through is 25~30mL/min.
4. a kind of preparation method of high circulation Life Type lithium sulfur battery anode material according to claim 1, its feature exist In：Step（4）Described vacuumizes to be evacuated to 3~5Pa.
CN201710933593.0A 2017-10-10 2017-10-10 A kind of preparation method of high circulation Life Type lithium sulfur battery anode material Pending CN107697901A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9112240B2 (en) * 2010-01-04 2015-08-18 Nanotek Instruments, Inc. Lithium metal-sulfur and lithium ion-sulfur secondary batteries containing a nano-structured cathode and processes for producing same
CN105375000A (en) * 2015-10-16 2016-03-02 广东烛光新能源科技有限公司 Sulfur-containing electrode material and preparation method thereof
CN105958045A (en) * 2016-06-07 2016-09-21 浙江大学 Positive electrode material for lithium-sulfur battery and preparation method for positive electrode material
CN106047303A (en) * 2016-06-30 2016-10-26 郭舒洋 Preparation method of high-heat-conductivity composite heat storage material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9112240B2 (en) * 2010-01-04 2015-08-18 Nanotek Instruments, Inc. Lithium metal-sulfur and lithium ion-sulfur secondary batteries containing a nano-structured cathode and processes for producing same
CN105375000A (en) * 2015-10-16 2016-03-02 广东烛光新能源科技有限公司 Sulfur-containing electrode material and preparation method thereof
CN105958045A (en) * 2016-06-07 2016-09-21 浙江大学 Positive electrode material for lithium-sulfur battery and preparation method for positive electrode material
CN106047303A (en) * 2016-06-30 2016-10-26 郭舒洋 Preparation method of high-heat-conductivity composite heat storage material

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