CN109244406A - A kind of cobalt oxide/graphene lithium sulfur battery anode material and preparation method thereof - Google Patents
A kind of cobalt oxide/graphene lithium sulfur battery anode material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of cobalt oxide/graphene material, cobaltosic oxide made from this method is in sea urchin shape, compound with graphene, and graphene sheet layer is supported, the specific surface area of composite material is effectively increased, it is made to possess richer porous structure.And cobaltosic oxide preparation method is simple, hydro-thermal method fast and easy.Material obtained and sulphur is compound, and unique structure effectively can adsorb and hold onto sulphur, it is possible to reduce the contact area and chance of sulphur and electrolyte, the effective generation for reducing polysulfide.Using cobalt oxide/graphene composite material to the adsorption capacity of more sulphions, more sulphions also can be firmly adsorbed on to the surface of composite material.Carrier of the cobalt oxide/graphene composite material as sulphur prepared by the present invention solves the low defect with poor circulation of active material utilization in lithium-sulfur cell.
Description
Technical field
Technical solution of the present invention is related to a kind of preparation method of lithium sulfur battery anode material, in particular to one kind four aoxidizes
Three cobalts/grapheme material preparation method, belongs to technical field of material chemistry.
Background technique
Operating voltage is high, energy density is big, memory-less effect, has extended cycle life and nothing because having for lithium ion secondary battery
The advantages that pollution, has become the preferred power supply of each electronic product in recent years.But come with mobile internet era
Face, electronics miniaturization and electric bicycle, electric car, large-scale energy-accumulating power station enter extensive development and using rank
Section, proposes the requirement of more height ratio capacity to lithium ion secondary battery.In lithium ion secondary battery system, relative to cathode material
Material, the positive electrode of low specific capacity are always the principal element for restricting its development.Therefore, develop that a kind of specific capacity is high, the circulation longevity
The positive electrode that life is long, security performance is high is particularly important.Elemental sulfur has highest specific capacity, theoretical in lithium-sulfur cell
Specific capacity is up to 1675mAh/g, and theoretical specific energy is 2600Wh/kg, than positive materials such as cobalt acid lithiums in conventional lithium ion battery
Material wants 5 times high.In addition, the reserves of sulphur itself are huge, environmental pollution is small, and in the industrial production, sulphur is in energy storage material
Minimum one kind of cost, and the toxicity of sulphur is low, can operating temperature range it is wide.Therefore, lithium/sulphur battery system with development potential,
As the research hotspot and one of emphasis in high-energy density secondary field of batteries in recent years.But lithium-sulfur cell charge and discharge process
In there are some serious problems: first, the conductivity of sulphur and lithium sulfide is lower, and sulphur particle volume in charge and discharge process occurs
Big variation, such variation can destroy electrode structure；Second, intermediate product polysulfide generated is in organic electrolyte
High dissolution, so that active material loss and energy consumption；Third, the polysulfide of dissolution can diffuse to cathode and lithium cathode is sent out
Raw reaction, the discharging product lithium sulfide or curing lithium of formation can be formed in lithium cathode surface to be precipitated；4th, the polysulfide of dissolution
" shuttle effect " easily occurs for compound.The utilization rate that the precipitating of " shuttle effect " and lithium cathode surface will lead to sulphur is low, sulphur is positive
Coulombic efficiency is low and capacity attenuation is very fast.It is existing studies have reported that in, by finding suitable positive electrode, lithium-sulfur cell can be made
Performance is effectively improved.Carbon sulphur composite material is mixed with metal oxide, so-called nano transition metal oxides are exactly benefit
With its distinctive adsorptivity, it is adsorbed on sulphur or carbon surface, the effective contact area for inhibiting sulphur and electrolyte is thus reduced
The chance of polysulfide is formed, to reach ideal effect, common metal oxide has titanium dioxide, nickel oxide etc.,
And cobaltosic oxide research is less.It is few using cobalt oxide/graphene/sulphur composite material as lithium-sulphur cell positive electrode at present
The research of material.CN103579590A discloses a kind of preparation method of the clad anode material of lithium battery, weighs in mass ratio
Elemental sulfur is dissolved in matter aqueous sodium polyacrylate by cobaltosic oxide and elemental sulfur at room temperature, and the dispersion for obtaining sulphur is molten
Cobaltosic oxide is dissolved in aqueous surfactant solution by liquid, obtains the dispersion solution of cobaltosic oxide, by the dispersion solution of sulphur
It is uniformly mixed with the dispersion solution of cobaltosic oxide, obtains mixed solution system, adjust mixed solution system with hydrochloric acid or acetic acid
PH to 7~8, after cobaltosic oxide is coated on the surface of elemental sulfur completely, by obtaining lithium after being filtered, washed and being dried in vacuo
The clad anode material of battery.It is above-mentioned to prepare cobaltosic oxide/sulphur composite material prior art, although changing to a certain extent
It has been apt to the performance of lithium-sulfur cell, but has haveed the defects that active material utilization is low and poor circulation.
Summary of the invention
The purpose of the present invention is problems in view of the prior art, provide a kind of preparation method of lithium sulfur battery anode material.
Cobaltosic oxide made from this method is in sea urchin shape, compound with graphene, and graphene sheet layer is supported, and is effectively increased multiple
The specific surface area of condensation material makes it possess richer porous structure.And cobaltosic oxide preparation method is simple, hydro-thermal method side
Just quickly.Material obtained and sulphur is compound, and unique structure effectively can adsorb and hold onto sulphur, it is possible to reduce sulphur and electricity
Solve the contact area and chance of liquid, the effective generation for reducing polysulfide.Utilize cobalt oxide/graphene composite material pair
More sulphions also can be firmly adsorbed on the surface of composite material by the adsorption capacity of more sulphions.Four oxygen prepared by the present invention
Change carrier of the three cobalts/graphene composite material as sulphur, solves that active material utilization in lithium-sulfur cell is low and cycle performance
The defect of difference.
The technical solution adopted by the present invention is that:
A kind of preparation method of lithium sulfur battery anode material, comprising the following steps:
Step 1: preparing cobaltosic oxide nano particle
Waterless cobaltous chloride and urea are add to deionized water, after 50~70min of magnetic agitation, dispersed using ultrasonic wave
Instrument is made mixed solution, puts it into the high pressure of polytetrafluoroethyllining lining to the mixed dispersion liquid 50~70min of ultrasonic disperse
In reaction kettle, 3~9h is heated at a temperature of 100~200 DEG C；Obtained sample is washed and is filtered, uses deionized water and ethyl alcohol respectively
Washing 2~4 times, then puts it into constant temperature blast drying oven, and dry 5~7h, will obtain under the conditions of 40~60 DEG C of temperature
Sample calcined in batch-type furnace, obtain cobaltosic oxide nano particle；
Step 2: configuration graphene oxide water solution
Configure 1~3g/L graphene oxide water solution, 40~60ml；
Step 3: preparation cobalt oxide/graphene
By 0.05~0.15g cobaltosic oxide nano particle ultrasonic disperse into 40~60ml deionized water, it is poured into
In the graphene oxide water solution configured in second step, after 50~70min of magnetic agitation, 50~70min of ultrasonic disperse will be obtained
Suspension carry out freeze-drying process, by obtained sample in tube furnace 350~450 DEG C of 3~5h of calcining of nitrogen atmosphere,
4~6 DEG C/min of heating rate；
Step 4: preparing the cobalt oxide/graphene of sulfur doping
After being ground cobalt oxide/graphene uniformly together with sulphur simple substance with mortar, it is put into hydro-thermal under an argon atmosphere
11~13h is reacted in kettle at 140~160 DEG C, obtains sulphur/cobalt oxide/graphene, wherein cobalt oxide/graphene
It is 2:1 with sulphur simple substance mass ratio.
Waterless cobaltous chloride dosage is 0.2~0.3g in the above-mentioned first step, and amount of urea is 2~3g, and deionized water volume is
30~50ml.
Calcination temperature is 250~350 DEG C in above-mentioned first step batch-type furnace, and calcination time is 1~3h.
Material and chemical reagent of the present invention are well known materials, commercially available to buy or obtained by known method.
Beneficial effects of the present invention are as follows:
Graphene is a kind of carbon material of two-dimensional structure, and with ideal monoatomic layer thickness, theoretical specific surface area is high
Up to 2630m2/ g, and electric conductivity and chemical stability are good, but the presence of Van der Waals force keeps graphene easy to reunite, and reduce stone
The specific surface area of black alkene introduces the cobaltosic oxide of sea urchin shape and graphene is compound that nanoparticle can be made to be embedded in adjacent graphite
Alkene piece interlayer, increases the distance between lamella, also greatly increases the specific surface area of composite positive pole, effectively prevention stone
Black alkene piece stacks again, more obvious to the constraint and suction-operated of sulphur.Cobalt oxide/graphene preparation process is simple, water
Thermal method operation is easy, and murder by poisoning is small, and preparation time is short.Cobalt oxide/graphene can not only be used for leading for lithium sulfur battery anode material
Electric skeleton structure, the electric conductivity of lift-off sulphur anode, and functional modification can be carried out to limit Li in graphene film layer surface2Sn
Dissolution, so can theoretically significantly improve the chemical property of lithium-sulfur cell.The composite material made from this patent forms
Lithium-sulfur cell, it is close that charge-discharge test initial discharge specific capacity is carried out under 0.1C multiplying power, in 1.7~2.8V voltage range
1100mAh/g, and charge and discharge platform is stablized.Show cobalt oxide/graphene effective solution prepared by the present invention
The shortcomings that active material utilization is low, poor circulation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of cobalt oxide/graphene prepared by embodiment 1 in the present invention.
Fig. 2 is the scanning electron microscope diagram piece of cobaltosic oxide prepared by the embodiment of the present invention 1.
Fig. 3 is the first charge and discharge of sulphur/cobalt oxide/graphene composite material prepared in the embodiment of the present invention 1
Curve.
Specific embodiment
Embodiment 1
Step 1: preparing cobaltosic oxide nano particle:
0.22g waterless cobaltous chloride and 2.4g urea are added in 40ml deionized water, after magnetic agitation 60min, utilized
Ultrasonic wave separating apparatus is made mixed solution, has put it into polytetrafluoroethyllining lining to mixed dispersion liquid ultrasonic disperse 60min
Autoclave in, heat 4h at a temperature of 110 DEG C；Obtained sample is washed and is filtered, is washed respectively with deionized water and ethyl alcohol
It washs 3 times, then puts it into constant temperature blast drying oven, dry 6h under the conditions of 50 DEG C of temperature.By obtained sample box
2h is calcined under the conditions of 300 DEG C in furnace, obtains cobaltosic oxide nano particle；
Step 2: configuration graphene oxide water solution
Configure 2g/L graphene oxide water solution 50ml；
Step 3: preparation cobalt oxide/graphene:
By 0.1g cobaltosic oxide nano particle ultrasonic disperse into 50ml deionized water, it is poured into second step and configures
Graphene oxide water solution in, after magnetic agitation 60min, obtained suspension is freeze-dried by ultrasonic disperse 60min
Processing, by obtained sample in tube furnace 400 DEG C of calcinings 4h, 5 DEG C/min of heating rate of nitrogen atmosphere；
Step 4: preparing the cobalt oxide/graphene of sulfur doping:
After being ground cobalt oxide/graphene uniformly together with sulphur simple substance with mortar, it is put into hydro-thermal under an argon atmosphere
12h is reacted at 150 DEG C in kettle, obtains sulphur/cobalt oxide/graphene, wherein cobalt oxide/graphene and sulphur simple substance
Mass ratio is 2:1.
Fig. 1 is the structural schematic diagram of cobalt oxide/graphene, as seen from the figure, the cobaltosic oxide and graphite of sea urchin shape
It after alkene is compound, is supported between graphene sheet layer, increases the distance between lamella, prevent it from reuniting, improve to active matter
The utilization rate of matter increases the cycle performance of battery.
Fig. 2 is the micro-structure diagram shot by scanning electron microscope, it can be seen from the figure that the present invention prepared
Unique sea urchin shape is presented in cobaltosic oxide material, and specific surface greatly increases, this makes cobaltosic oxide among graphene sheet layer
Can have and significantly support, make cobalt oxide/graphene composite material that there is richer pore structure, it can firmly beam
Sulphur is tied up and adsorbed, sulphur active material is made to be utilized effectively, increases the cycle performance of battery.
Fig. 3 is the first charging and discharging curve of the battery of material prepared assembly.The CT- produced using Shenzhen Xin Wei company
4008 type multi-channel battery test instrument test battery under constant temperature (25 DEG C) in laboratory.It can from figure
Out, under the current density of 0.1C, initial discharge specific capacity has reached 1085mAh/g, and discharge curve shows two surely
Fixed platform illustrates of the invention practical solve that active material utilization is low and the defect of circulating battery stability difference.
Embodiment 2
Step 1: preparing cobaltosic oxide nano particle:
0.22g waterless cobaltous chloride and 2.4g urea are added in 40ml deionized water, after magnetic agitation 60min, utilized
Ultrasonic wave separating apparatus is made mixed solution, has put it into polytetrafluoroethyllining lining to mixed dispersion liquid ultrasonic disperse 60min
Autoclave in, heat 6h at a temperature of 110 DEG C；Obtained sample is washed and is filtered, is washed respectively with deionized water and ethyl alcohol
It washs 3 times, then puts it into constant temperature blast drying oven, dry 6h under the conditions of 50 DEG C of temperature.By obtained sample box
2h is calcined under the conditions of 300 DEG C in furnace, obtains cobaltosic oxide nano particle；
Step 2: configuration graphene oxide water solution
Configure 2g/L graphene oxide water solution 50ml；
Step 3: preparation cobalt oxide/graphene:
By 0.1g cobaltosic oxide nano particle ultrasonic disperse into 50ml deionized water, it is poured into second step and configures
Graphene oxide water solution in, after magnetic agitation 60min, obtained suspension is freeze-dried by ultrasonic disperse 60min
Processing, by obtained sample in tube furnace 400 DEG C of calcinings 4h, 5 DEG C/min of heating rate of nitrogen atmosphere；
Step 4: preparing the cobalt oxide/graphene of sulfur doping:
After being ground cobalt oxide/graphene uniformly together with sulphur simple substance with mortar, it is put into hydro-thermal under an argon atmosphere
12h is reacted at 150 DEG C in kettle, obtains sulphur/cobalt oxide/graphene, wherein cobalt oxide/graphene and sulphur simple substance
Mass ratio is 2:1.
Embodiment 3
Step 1: preparing cobaltosic oxide nano particle:
0.22g waterless cobaltous chloride and 2.4g urea are added in 40ml deionized water, after magnetic agitation 60min, utilized
Ultrasonic wave separating apparatus is made mixed solution, has put it into polytetrafluoroethyllining lining to mixed dispersion liquid ultrasonic disperse 60min
Autoclave in, heat 6h at a temperature of 110 DEG C；Obtained sample is washed and is filtered, is washed respectively with deionized water and ethyl alcohol
It washs 3 times, then puts it into constant temperature blast drying oven, dry 6h under the conditions of 50 DEG C of temperature.By obtained sample box
2h is calcined under the conditions of 300 DEG C in furnace, obtains cobaltosic oxide nano particle；
Step 2: configuration graphene oxide water solution
Configure 2g/L graphene oxide water solution 50ml；
Step 3: preparation cobalt oxide/graphene:
By 0.1g cobaltosic oxide nano particle ultrasonic disperse into 50ml deionized water, it is poured into second step and configures
Graphene oxide water solution in, after magnetic agitation 60min, obtained suspension is freeze-dried by ultrasonic disperse 60min
Processing, by obtained sample in tube furnace 400 DEG C of calcinings 4h, 5 DEG C/min of heating rate of nitrogen atmosphere；
Step 4: preparing the cobalt oxide/graphene of sulfur doping:
After being ground cobalt oxide/graphene uniformly together with sulphur simple substance with mortar, it is put into hydro-thermal under an argon atmosphere
12h is reacted at 150 DEG C in kettle, obtains sulphur/cobalt oxide/graphene, wherein cobalt oxide/graphene and sulphur simple substance
Mass ratio is 2:1.
Unaccomplished matter of the present invention is well-known technique.
Claims (4)
1. a kind of cobalt oxide/graphene lithium sulfur battery anode material, which is characterized in that the positive electrode is by four oxygen
Change three cobalts and graphene is combined, wherein cobaltosic oxide is in sea urchin shape, and graphene sheet layer is supported.
2. a kind of preparation method of cobalt oxide/graphene lithium sulfur battery anode material as described in claim 1, feature
It is, includes the following steps
Step 1: preparing cobaltosic oxide nano particle
Waterless cobaltous chloride and urea are add to deionized water, after 50~70min of magnetic agitation, utilize ultrasonic wave separating apparatus pair
The mixed dispersion liquid 50~70min of ultrasonic disperse is made mixed solution, puts it into the reaction under high pressure of polytetrafluoroethyllining lining
In kettle, 3~9h is heated at a temperature of 100~200 °C；Obtained sample is washed and is filtered, uses deionized water and ethanol washing 2 respectively
It~4 times, then puts it into constant temperature blast drying oven, dry 5~7h, the sample that will be obtained under the conditions of 40~60 °C of temperature
It is calcined in batch-type furnace, obtains cobaltosic oxide nano particle；
Step 2: configuration graphene oxide water solution
Configure 1~3g/L graphene oxide water solution, 40~60ml；
Step 3: preparation cobalt oxide/graphene
By 0.05~0.15g cobaltosic oxide nano particle ultrasonic disperse into 40~60ml deionized water, it is poured into second
In the graphene oxide water solution configured in step, after 50~70min of magnetic agitation, 50~70min of ultrasonic disperse is outstanding by what is obtained
Supernatant liquid carries out freeze-drying process, 350~450 °C of 3~5h of calcining of nitrogen atmosphere, heating in tube furnace by obtained sample
4~6 °C/min of rate；
Step 4: preparing the cobalt oxide/graphene of sulfur doping
After being ground cobalt oxide/graphene uniformly together with sulphur simple substance with mortar, it is put into water heating kettle under an argon atmosphere
11~13h is reacted under 140~160 °C, obtains sulphur/cobalt oxide/graphene, wherein cobalt oxide/graphene and sulphur
Simple substance mass ratio is 2:1.
3. the preparation method of cobalt oxide/graphene lithium sulfur battery anode material according to claim 2, feature exist
In, in the first step waterless cobaltous chloride dosage be 0.2 ~ 0.3g, amount of urea be 2 ~ 3g, deionized water volume be 30 ~
50ml。
4. the preparation method of cobalt oxide/graphene lithium sulfur battery anode material according to claim 2, feature exist
In the calcination temperature of batch-type furnace is 250~350 °C in the first step, and calcination time is 1~3h.
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Cited By (10)
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| CN110416509A (en) * | 2019-07-17 | 2019-11-05 | 肇庆市华师大光电产业研究院 | A kind of lithium ion battery negative material of height ratio capacity and preparation method thereof |
| WO2021008244A1 (en) * | 2019-07-17 | 2021-01-21 | 肇庆市华师大光电产业研究院 | Lithium ion battery negative electrode material with high specific capacity and preparation method therefor |
| CN110752359A (en) * | 2019-10-29 | 2020-02-04 | 肇庆市华师大光电产业研究院 | Preparation method of sulfur-three-dimensional hollow graphene-carbon nanotube composite lithium-sulfur battery positive electrode material |
| CN110752360A (en) * | 2019-10-29 | 2020-02-04 | 肇庆市华师大光电产业研究院 | S-Ni3Preparation method of C/NiO composite lithium-sulfur battery positive electrode material |
| CN110752360B (en) * | 2019-10-29 | 2022-06-17 | 肇庆市华师大光电产业研究院 | S-Ni3Preparation method of C/NiO composite lithium-sulfur battery positive electrode material |
| CN111470546A (en) * | 2020-03-17 | 2020-07-31 | 肇庆市华师大光电产业研究院 | Coating material for functional interlayer of lithium-sulfur battery and preparation method thereof |
| CN111599995A (en) * | 2020-04-28 | 2020-08-28 | 惠州锂威新能源科技有限公司 | Cathode material, preparation method thereof and high-voltage lithium ion battery |
| 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 |
| CN115215380A (en) * | 2022-07-13 | 2022-10-21 | 四川轻化工大学 | Cobaltosic oxide/nitrogen-doped graphene oxide material, preparation method thereof and application thereof in sodium-ion battery |
| CN115215380B (en) * | 2022-07-13 | 2023-12-08 | 四川轻化工大学 | Tricobalt tetraoxide/nitrogen-doped graphene oxide material, preparation method thereof and application thereof in sodium ion battery |
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