CN109461904A - A kind of preparation method of lithium sulfur battery anode material - Google Patents
A kind of preparation method of lithium sulfur battery anode material Download PDFInfo
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- CN109461904A CN109461904A CN201811155201.3A CN201811155201A CN109461904A CN 109461904 A CN109461904 A CN 109461904A CN 201811155201 A CN201811155201 A CN 201811155201A CN 109461904 A CN109461904 A CN 109461904A
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- anode material
- battery anode
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- cobaltosic oxide
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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
- H01M4/366—Composites as layered products
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 invention belongs to the technical fields of lithium-sulfur cell, are specifically related to a kind of preparation method of lithium sulfur battery anode material.The preparation method is the following steps are included: (1) prepares cobaltosic oxide tiny balloon；(2) graphene/cobaltosic oxide composite material is prepared.It is conducive to maintain the integrality of battery structure by lithium sulfur battery anode material prepared by this method, enhances the electric conductivity of electrode material, improve the stability of electrode, there is height ratio capacity.
Description
Technical field
The invention belongs to the technical fields of lithium-sulfur cell, are specifically related to a kind of preparation side of lithium sulfur battery anode material
Method.
Background technique
It being constantly progressive as new energy and green are scientific and technical and power battery and mobile power source equipment is needed
The growth asked, environmentally friendly, have extended cycle life, the research for the lithium ion battery that specific capacity is high become more and more intentionally
Justice.For the lithium ion battery being made of anode, cathode, electrolyte and diaphragm etc., researcher is mainly focused on positive and negative electrode material
The research of material improves its specific capacity, improves its cycle life.After decades of development, conventional lithium ion battery positive electrode
The limitation of (such as LiMn2O4, LiCoO2, LiNiO2, LiFePO4) due to its theoretical specific capacity, it is difficult to obtain in a short time
Biggish breakthrough, the research of novel anode material are just constantly risen.Elemental sulfur is up to 1675mAh/g and reason because of its theoretical specific capacity
2600Wh/kg is up to by energy density receiving and especially pay close attention to, furthermore elemental sulfur also has cheap, rich reserves, nontoxic
The advantages that, therefore elemental sulfur is excellent energy storage material, in terms of the use and mitigation for reducing fossil fuel
There to be very bright prospect.But the shortcomings that lithium-sulfur cell, is also very fatal, wherein positive electrode sulphur is electronics and ion insulation
Body, electronic conductivity are about 5 × 10- 30S•cm- 1；The polysulfide generated in charge and discharge process simultaneously can be dissolved in electricity
It solves in liquid, under the influence of concentration difference, causes shuttle effect, lead to active material loss, capacity fails rapidly.And discharging product
Also electronics and ion insulator, density differ greatly lithium sulfide with elemental sulfur, and electrode can occur in charge and discharge process
Huge volume expansion；Furthermore lithium metal can generate dendrite, dead lithium and electrode dusting, lead to the cyclicity of battery as cathode
It can be deteriorated, cause safety high, thus result in lithium-sulfur cell always and cannot achieve commercialization.
Summary of the invention
Electric conductivity is insufficient when it is an object of the invention to for current metal oxide as lithium sulfur battery anode material
Disadvantage and a kind of preparation method of lithium sulfur battery anode material is provided, by this method prepare lithium sulfur battery anode material be conducive to
The integrality for maintaining battery structure, enhances the electric conductivity of electrode material, improves the stability of electrode, has height ratio capacity.
The technical solution of the present invention is as follows: a kind of preparation method of lithium sulfur battery anode material, comprising the following steps:
(1) it prepares cobaltosic oxide tiny balloon: glucose being dissolved in deionized water first, be placed in reaction kettle 180
Hydro-thermal reaction 2~4 hours at~200 DEG C, it is cooling with room temperature after the reaction was completed, product is collected by centrifugation in gained suspension, is spent
Ion water washing three times after, carbon ball powder is dried to obtain under the conditions of 60 DEG C, it is spare；Then carbon ball powder and four acetate hydrates are taken
Cobalt is placed in deionized water, 30~60min of ultrasonic disperse, is stirred 1~2 hour under the conditions of magnetic agitation, is subsequently placed at baking oven
In dried under the conditions of 60~80 DEG C；Finally will drying products therefrom be placed in tube furnace, under air conditions with 1~2 DEG C/
The heating rate of min is cooling with room temperature after being warming up to 400~600 DEG C, heat preservation 1~2 hour；
(2) graphene/cobaltosic oxide composite material is prepared: hollow by resulting cobaltosic oxide is prepared in the step (1)
Microballoon is placed in graphene aqueous solution, obtains mixed solution within ultrasonic disperse 20~40 minutes；Mixed solution is passed through into spray drying
Machine is dried, and obtains graphene/cobaltosic oxide composite powder.
10~20g glucose is dissolved in 100~200mL deionized water in the step (1) and is placed in 200mL reaction kettle
In.
The mass ratio of carbon ball powder and four acetate hydrate cobalts is 1:1 in the step (1).
1~2g carbon ball powder and 1~2g, tetra- acetate hydrate cobalt is taken to be placed in 40~60mL deionized water in the step (1)
In.
Graphene aqueous solution concentration is 1~3mg/mL in the step (2).
0.5~1g cobaltosic oxide tiny balloon is placed in 200~300mL graphene aqueous solution in the step (2).
The invention has the benefit that the preparation method of lithium sulfur battery anode material of the present invention is prepared first with three
Then the cobaltosic oxide microballoon of layer hollow structure obtains a kind of lithium of height ratio capacity by spray drying composite graphite alkene again
Sulphur cell positive electrode material.
Using cobaltosic oxide microballoon as active ingredient carriers in lithium-sulfur cell, the polar active position on its surface is utilized
Point reduces active matter in reaction process by the more lithium sulfides generated in the effect absorption lithium-sulfur cell discharge process of chemical bond
The loss of matter.Simultaneously compared to common carbon material for, cobaltosic oxide tap density also with higher is more advantageous to dimension
Hold the integrality of battery structure.
There is three layers of hollow ball structure, the well-designed technique of the present invention by the resulting cobaltosic oxide of the preparation method
Parameter, strict control state-variable, cobalt source type in preparation process, precursor concentration, calcination temperature, heat up in calcination process speed
Rate, the common coordinative role of various aspects condition obtain three layers of hollow structure, and the change of each condition can influence end product
Three-decker.The carbon ball surface that gluconate dehydratase condensation reaction obtains has the functional groups such as-OH and-C=0, these polarity
Functional group makes carbon ball surface with negative electrical charge, and therefore, carbon ball is easy the metal ion that absorption has positive charge, more shell hollow spheres
Shell number can be controlled by control presoma in the adsorption deeply and adsorbance of carbosphere.Wherein the selection of reactant with
Reaction condition all has important influence, presoma Co(Ac)2For weak acid and mild base salt, acid and alkali hydrolysis degree is almost the same, molten
Liquid partial neutral, and at this point, carbosphere template surface with a large amount of negative electrical charge, absorbs into the metal ion total amount of carbon ball template
Increase, three shell hollow spheres can be obtained after calcination.In addition precursor solution concentration equally has the formation of more shell hollow spheres
There is important role, when the concentration of metal ions of precursor is excessively high, according to principle of dynamics, the equilibrium constant of hydrolysis increases,
Reaction forward promotes, and when other reaction conditions are consistent, part metals ion is hydrolyzed on carbon ball surface, prevents more metals
Ion enters inside carbon ball, obtains the hollow sphere of the very thick few layer of outer layer.And precursor concentration it is very low when, inside and outside carbon ball
Metal ion concentration reduce, metal ion to carbon ball driving force reduce, it is few into the metal ion quality inside carbon ball,
Depth as shallow, therefore typically result in few shell hollow sphere.In addition, the burning velocity and oxygen of heating rate in calcination to carbon ball
The crystallization rate of compound equally has very big influence.With the increase of calcination temperature, the carbosphere template of metal ion has been adsorbed
Outer layer gradually burns, shrinks, while being exposed to the unformed metal oxide crystal growth of outer surface.When the metal of outer surface
Oxide buildup to a certain extent, forms one layer enough, when resisting carbon ball and burn to the power of contract, outer layer and carbon ball point
From, and carbon ball burns away to contract, equally, the unformed metal oxide crystal growth in contraction process outer surface forms shell
Layer, in cycles, more shell hollow spheres are formed.When as lithium sulfur battery anode material, more shell hollow spheres possess outstanding
Structural advantage, uniform duct ensures that electrolyte enters inside more shells in which can be convenient on shell so that electrolyte with
Active material adequately contacts, and provides more oxidation activity sites, obtains higher specific capacity at higher current densities.Simultaneously
Shell wall is very thin, shortens the transmission path of electronics and charge, and internal free volume can be alleviated in charge and discharge process just
The expansion of pole material makes it possess good cycle life in addition obtained material has good mechanical performance.
The electric conductivity that graphene enhancing electrode material is introduced in the preparation method, simultaneously because the special knot of graphene
Structure can alleviate the volume change problem of active material in lithium-sulfur cell charge and discharge process, improve the stability of electrode.
Detailed description of the invention
Fig. 1 is embodiment 1, embodiment 2, the compound lithium-sulphur cell positive electrode of graphene/cobaltosic oxide obtained by embodiment 3
Material is respectively applied to the specific discharge capacity circulation figure in battery.
Fig. 2 is embodiment 1, embodiment 2, the compound lithium-sulphur cell positive electrode of graphene/cobaltosic oxide obtained by embodiment 3
Material is respectively applied to the high rate performance figure in battery.
Specific embodiment
Below by embodiment, the present invention is described in detail.
Embodiment 1
The preparation method of the lithium sulfur battery anode material, comprising the following steps:
(1) it prepares cobaltosic oxide tiny balloon: 15g glucose is dissolved in 150mL deionized water, be placed in 200mL reaction
In kettle at 190 DEG C hydro-thermal reaction 3 hours, it is cooling with room temperature after the reaction was completed；Product is collected by centrifugation in gained suspension, is spent
Ion water washing three times after, carbon ball powder is dried to obtain under the conditions of 60 DEG C, it is spare.1.5g carbon ball powder is taken, 1.5g tetra- is hydrated
Cobalt acetate is placed in 50mL deionized water, ultrasonic disperse 40min, is stirred 1.5 hours under the conditions of magnetic agitation, is subsequently placed at baking
70 DEG C of drying in case.Then drying products therefrom is placed in tube furnace, with the heating rate liter of 1 DEG C/min under air conditions
Temperature is cooling with room temperature after heat preservation 1.5 hours to 500 DEG C.
(2) it prepares graphene/cobaltosic oxide composite material: taking the graphene aqueous solution 200mL for being available commercially from Aladdin, stone
Black aqueous solution concentration is 1mg/mL, and the three layers of hollow cobaltosic oxide microballoon prepared in 0.5g step (1) are placed in one
To mixed solution, ultrasonic disperse 30 minutes；Mixed solution is dried to obtain graphene/tetra- oxygen by spray dryer
Change three Co composite powders.
Embodiment 2
The preparation method of the lithium sulfur battery anode material, comprising the following steps:
(1) it prepares cobaltosic oxide tiny balloon: 10g glucose is dissolved in 100mL deionized water, be placed in 200mL reaction
In kettle, hydro-thermal reaction 2 hours at 180 DEG C are cooling with room temperature after the reaction was completed.Product is collected by centrifugation in gained suspension, is used
After deionized water washing three times, it is spare under the conditions of 60 DEG C to be dried to obtain carbon ball powder.Take 1g carbon ball powder, tetra- acetate hydrate of 1g
Cobalt is placed in 40mL deionized water, ultrasonic disperse 30min, is stirred 1 hour, is subsequently placed at 60 in baking oven under the conditions of magnetic agitation
DEG C drying.Then drying products therefrom is placed in tube furnace, is warming up under air conditions with the heating rate of 1 DEG C/min
It is cooling with room temperature after 400 DEG C, heat preservation 1 hour.
(2) it prepares graphene/cobaltosic oxide composite material: taking the graphene aqueous solution 200mL for being available commercially from Aladdin, stone
Black aqueous solution concentration is 1mg/mL, and the three layers of hollow cobaltosic oxide microballoon prepared in 0.5g step (1) are placed in one, and is surpassed
Sound disperses 20 minutes.Mixed solution is dried to obtain graphene/cobaltosic oxide composite powder by spray dryer
End.
Embodiment 3
The preparation method of the lithium sulfur battery anode material, comprising the following steps:
(1) it prepares cobaltosic oxide tiny balloon: 20g glucose being dissolved in 200mL deionized water, is set
In 200mL reaction kettle, hydro-thermal reaction 4 hours at 200 DEG C are cooling with room temperature after the reaction was completed.By gained suspension
Product is collected by centrifugation, after being washed with deionized three times, it is spare that carbon ball powder is dried to obtain at 60 DEG C.Take 2g carbon ball powder, 2g
Four acetate hydrate cobalts are placed in 60mL deionized water, ultrasonic disperse 60min, are stirred 2 hours under the conditions of magnetic agitation, with postposition
80 DEG C of drying in baking oven.Then drying products therefrom is placed in tube furnace, with the heating speed of 2 DEG C/min under air conditions
Degree is cooling with room temperature after being warming up to 600 DEG C, heat preservation 2 hours.
(2) graphene/cobaltosic oxide composite material is prepared:
The graphene aqueous solution 300mL for being available commercially from Aladdin is taken, graphene aqueous solution concentration is 3mg/mL, will be in 1g step (1)
Three layers of hollow cobaltosic oxide microballoon of preparation are placed in one, and ultrasonic disperse 40 minutes.Mixed solution is passed through into spray dryer
It is dried to obtain graphene/cobaltosic oxide composite powder.
As seen from Figure 1, lithium under 0.2C current density of graphene/cobaltosic oxide composite material made from embodiment 1
Cell positive material specific discharge capacity in first time circulation is up to 1619 mAh/g, with the continuous progress of circulation, battery ratio
Capacity constantly declines, and still has 1336 mAh/g after 50 circle of circulation, and reflecting the positive electrode has brilliant electrochemistry circulation
Performance.And material result prepared by embodiment 1 is substantially better than embodiment 2 and embodiment 3.
By Fig. 2 as it can be seen that even if under the high current density of 2C, the preparation-obtained lithium-sulfur cell of embodiment 1 still table
Reveal the capacity of 675 mAh/g, and when current density is down to 0.2C again, specific discharge capacity restores again to 1446 mAh/g,
This shows that the positive electrode has excellent high rate performance.Meanwhile contrast effect is consistent with Fig. 1 result.
Claims (6)
1. a kind of preparation method of lithium sulfur battery anode material, comprising the following steps:
(1) it prepares cobaltosic oxide tiny balloon: glucose being dissolved in deionized water first, be placed in reaction kettle 180
Hydro-thermal reaction 2~4 hours at~200 DEG C, it is cooling with room temperature after the reaction was completed, product is collected by centrifugation in gained suspension, is spent
Ion water washing three times after, carbon ball powder is dried to obtain under the conditions of 60 DEG C, it is spare；Then carbon ball powder and four acetate hydrates are taken
Cobalt is placed in deionized water, 30~60min of ultrasonic disperse, is stirred 1~2 hour under the conditions of magnetic agitation, is subsequently placed at baking oven
In dried under the conditions of 60~80 DEG C；Finally will drying products therefrom be placed in tube furnace, under air conditions with 1~2 DEG C/
The heating rate of min is cooling with room temperature after being warming up to 400~600 DEG C, heat preservation 1~2 hour；
(2) graphene/cobaltosic oxide composite material is prepared: hollow by resulting cobaltosic oxide is prepared in the step (1)
Microballoon is placed in graphene aqueous solution, obtains mixed solution within ultrasonic disperse 20~40 minutes；Mixed solution is passed through into spray drying
Machine is dried, and obtains graphene/cobaltosic oxide composite powder.
2. the preparation method of lithium sulfur battery anode material according to claim 1, which is characterized in that will in the step (1)
10~20g glucose is dissolved in 100~200mL deionized water and is placed in 200mL reaction kettle.
3. the preparation method of lithium sulfur battery anode material according to claim 1, which is characterized in that carbon in the step (1)
The mass ratio of ball powder and four acetate hydrate cobalts is 1:1.
4. the preparation method of lithium sulfur battery anode material according to claim 3, which is characterized in that take 1 in the step (1)
~2g carbon ball powder and 1~2g, tetra- acetate hydrate cobalt are placed in 40~60mL deionized water.
5. the preparation method of lithium sulfur battery anode material according to claim 1, which is characterized in that stone in the step (2)
Black aqueous solution concentration is 1~3mg/mL.
6. the preparation method of lithium sulfur battery anode material according to claim 5, which is characterized in that will in the step (2)
0.5~1g cobaltosic oxide tiny balloon is placed in 200~300mL graphene aqueous solution.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110380030A (en) * | 2019-07-18 | 2019-10-25 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN110690448A (en) * | 2019-10-29 | 2020-01-14 | 肇庆市华师大光电产业研究院 | Preparation method of sodium-sulfur battery positive electrode material |
| CN111370658A (en) * | 2020-02-27 | 2020-07-03 | 肇庆市华师大光电产业研究院 | Lithium-sulfur battery positive electrode material and preparation method thereof |
| CN111508720A (en) * | 2020-04-24 | 2020-08-07 | 梁汉日 | polyaniline-Co3O4Composite nanofiber supercapacitor electrode material and preparation method thereof |
| CN112151786A (en) * | 2020-11-04 | 2020-12-29 | 肇庆市华师大光电产业研究院 | Lithium-sulfur battery positive electrode material and preparation method thereof |
| CN112993257A (en) * | 2021-03-11 | 2021-06-18 | 杭州电子科技大学 | rGO coated Co3O4Microsphere composite material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110380030A (en) * | 2019-07-18 | 2019-10-25 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN110380030B (en) * | 2019-07-18 | 2020-07-14 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery positive electrode material |
| CN110690448A (en) * | 2019-10-29 | 2020-01-14 | 肇庆市华师大光电产业研究院 | Preparation method of sodium-sulfur battery positive electrode material |
| CN111370658A (en) * | 2020-02-27 | 2020-07-03 | 肇庆市华师大光电产业研究院 | Lithium-sulfur battery positive electrode material and preparation method thereof |
| CN111370658B (en) * | 2020-02-27 | 2022-06-03 | 肇庆市华师大光电产业研究院 | Lithium-sulfur battery positive electrode material and preparation method thereof |
| CN111508720A (en) * | 2020-04-24 | 2020-08-07 | 梁汉日 | polyaniline-Co3O4Composite nanofiber supercapacitor electrode material and preparation method thereof |
| CN112151786A (en) * | 2020-11-04 | 2020-12-29 | 肇庆市华师大光电产业研究院 | Lithium-sulfur battery positive electrode material and preparation method thereof |
| CN112993257A (en) * | 2021-03-11 | 2021-06-18 | 杭州电子科技大学 | rGO coated Co3O4Microsphere composite material and preparation method thereof |
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Application publication date: 20190312 |