CN108666546A - A kind of lithium cell cathode material and preparation method of layered nano-graphene - Google Patents
A kind of lithium cell cathode material and preparation method of layered nano-graphene Download PDFInfo
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- 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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- 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
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/625—Carbon or graphite
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Abstract
The invention belongs to the technical fields of lithium cell cathode material, provide a kind of lithium cell cathode material and preparation method of layered nano graphene.This method takes off lithium in absolute ethyl alcohol by silicon lithium alloy and forms sheet silicon nanometer sheet, it is dispersed in the absolute ethyl alcohol containing graphene oxide through ultrasonic vibration, graphene oxide is wrapped in silicon nanometer sheet surface layer since specific surface area is excessive and spontaneous, graphene oxide is reduced to graphene layer finally by high-temperature heat treatment, the binding force of graphene layer and silicon nanoscale twins is improved simultaneously, and the lithium cell cathode material of layered nano graphene is made.Compared with conventional method, the lithium cell cathode material of the preparation of the present invention, form the sandwich of graphene and silicon chip, make graphene layer alleviation 2d laminar nanos silicon chip in the volume deformation of lithium ion deintercalation process, effectively increase the stability of negative material, and preparation process is simply controllable, is easy to industrialization large-scale production.
Description
Technical field
The invention belongs to the technical fields of lithium cell cathode material, provide a kind of lithium electricity of layered nano-graphene
Pond negative material and preparation method.
Background technology
China's production of energy amount and consumption figure are at the forefront in the world, but in energy resource supply and using there is one in form
Serial outstanding problem improves efficiency of energy utilization, readjusts the energy structure, and it will be China's energy hair to develop and utilize regenerative resource
The inevitable choice of exhibition.In order to solve the problems, such as that China's energy industry is faced, seek to substitute the renewable green of conventional fossil fuel
The color energy seems particularly urgent.At the same time, with people's environmental consciousness be increasingly enhanced and concern to resource utilization, can
Rechargeable battery is increasingly becoming the focus of research, and the successful application of lithium primary cell pushed significantly lithium ion battery research and
Development makes lithium ion battery become the emphasis of concern.
Lithium ion battery is mainly made of anode, cathode, electrolyte and diaphragm.The energy density of battery depends primarily on it
Output voltage and specific capacity, and voltage and the height of specific capacity are determined by electrode material and electrolyte electrochemical performance
, the especially selection of electrode material.Wherein, lithium ion battery negative material is the important component of lithium ion battery, is born
The Nomenclature Composition and Structure of Complexes of pole material has decisive impact the chemical property of lithium ion battery.
Currently used as mainly having for lithium cell cathode material：Carbons negative material, alloy type negative material, oxo transition metal
Compound class negative material, transition metal nitride class negative material, titanium base material etc..In recent years, especially in above-mentioned material
2d anode materials, such as titanium oxide, transition metal oxide, metal phosphide/sulfide/nitride, have been widely used
In lithium ion.In 2d anode materials, 2d silicon is due to its high theoretical lithium memory capacity, faster Li diffusion rates, lower
Discharge potential and lower diffusion energy barrier（0.23 eV）And it gets more and more people's extensive concerning.
It has been achieved in terms of lithium battery composite material technology of preparing, especially silicon based anode material preparation both at home and abroad at present
Certain effect.Wherein Zhao Zhigang et al. has invented a kind of preparation method and the silicium cathode material of lithium ion battery silicium cathode material
Material（Chinese invention patent application number 201610149069.X）, specifically include following steps：Step 1, surface hydroxylation：It will oxidation
Sub- silicon is put into heating in the mixed solution of ammonium hydroxide, hydrogen peroxide and water composition and boils and stir 10 ~ 60min, then wash, filter,
80 ~ 120 DEG C of 2 ~ 12h of vacuum drying；Step 2, it stirs：Desciccate in step 1 is put into the anhydrous absolute ethyl alcohol containing titanium source
In, stir 2 ~ 10h；It adds water and stirs 15 ~ 75min, be subsequently added into graphite, then add containing lithium source without anhydrous water second
Alcohol is eventually adding glacial acetic acid stirring, stops stirring when black sol becomes gel；Step 3, it is aged and dry：Step 2 is given birth to
At gel be aged 12h or 12h or more, then 70 ~ 90 DEG C vacuum drying 8 ~ 16h；Step 4, it calcines：Step 3 is aged and is done
Gel after dry is broken and is calcined under inert atmosphere protection；Finally, it is cooled to room temperature and obtains silicium cathode material.In addition, Jiang Yong
A kind of spherical nano-silicon graphene is compound prepares lithium cell cathode material and preparation method for refined invention（Chinese invention patent application
Numbers 201510969123.0）, spherical high-purity nano level metal or ball prepared by the vapor phase method for being 3 ~ 35% with weight percent
The high-purity nano level metal alloy of shape and 65 ~ 97% graphene flat sheet, 0.1 ~ 15% conducting high polymers object,
0.1-15% water-soluble adhesion agent obtains the compound lithium cell cathode material in lamination multidimensional gap by stirring and emulsifying, prepares
Method is that nano level metal prepared by the vapor phase method that will be weighed or nano level metal alloy and the incorporation of graphene flat sheet are conductive high
After Molecularly Imprinted Polymer first passes through high-speed emulsifying machine emulsification, then moves into dispersion machine and pass through dispersion machine after adding water-soluble adhesion agent
Lithium cell cathode material is combined into after dispersion, advantage is：Can be big with the gap of its manufactured cathode of lithium battery, cycle life reaches
2000 times or more, suitable for preparing cathode of lithium battery.
As it can be seen that there are manufacturing costs is higher for silicon materials in 2d anode materials in the prior art, the process is more complicated,
Prepared by heavy industrialization still have larger challenge, and the volume expansion of silica-base material is very big, it is difficult to individually answer
The shortcomings of for electrode material.
Invention content
For such case, it is proposed that a kind of lithium cell cathode material and preparation method of layered nano-graphene,
The stability of negative material can be effectively improved, reduces cubical expansivity, and be readily produced, has a extensive future.
To achieve the above object, specific technical solution of the present invention is as follows：
A kind of preparation method of the lithium cell cathode material of layered nano-graphene, by silicon lithium alloy in absolute ethyl alcohol
De- lithium forms sheet silicon nanometer sheet, is dispersed in the absolute ethyl alcohol containing graphene oxide through ultrasonic vibration, graphite oxide
Alkene is wrapped in silicon nanometer sheet surface layer since specific surface area is excessive and spontaneous, restores graphene oxide finally by high-temperature heat treatment
For graphene layer, while the binding force of graphene layer and silicon nanoscale twins is improved, the lithium battery of layered nano-graphene is made
Negative material, preparation are as follows：
（1）Silicon lithium alloy powder is scattered in absolute ethyl alcohol, 2 ~ 3h of magnetic agitation is carried out under the conditions of argon gas, makes silicon lithium alloy
Lithium is taken off in absolute ethyl alcohol and forms sheet silicon nanometer sheet, is then added and is dispersed in the absolute ethyl alcohol of graphene oxide, ultrasound
8 ~ 12min is vibrated, graphene oxide is spontaneous in ultrasonic procedure to be wrapped in the surface layer of silicon nanometer sheet, and is dispersed in anhydrous second
In alcohol, dispersion liquid is made；
（2）By step（1）Dispersion liquid obtained is closed, is aged 20 ~ 30h, then filters, dries, negative material presoma is made；
（3）By step（2）Negative material presoma obtained quickly heats up to 800 ~ 1000 DEG C under protection of argon gas, and processing 1 ~
3min makes graphene oxide be reduced to graphene layer, and the negative material of sheet nano-silicon-graphene layer structure is made.
So far, in lithium cell cathode material, the theoretical capacity highest of silica-base material, Li and Si form alloy LixSi
（0<x≤4.4）, at normal temperatures, the rich lithium product that silicium cathode is generated with lithium alloyage is mainly Li3.75Si phases, specific capacity are up to
3572mAh/g is much larger than the theoretical capacity of graphite, but along with huge volume change, volume expansion is up to 280%, silicon
Dusting causes electrode structure unstability and fails, and the avalanche of electrode structure and active material is caused to peel off and so that electrode is lost electricity and connect
It touches, significantly decline is even entirely ineffective therewith for the capacity of electrode.By designing various special nanotopography structures, can effectively delay
Rush sandwich of the volume change by formation graphene and silicon chip.The interlayer knot that the present invention passes through formation graphene and silicon chip
Structure makes graphene layer alleviate volume deformation of 2d laminar nanos silicon chip during lithium ion deintercalation, and then improves negative material
Stability.
Preferably, step（1）The silicon lithium alloy powder is Li12Si7、Li7Si3、Li13Si4At least one of.
Preferably, step（1）In the dispersion liquid, 20 ~ 30 parts by weight of silicon lithium alloy powder, 5 ~ 10 weight of graphene oxide
Part, 60 ~ 75 parts by weight of absolute ethyl alcohol.
Preferably, step（1）The rotating speed of the magnetic agitation is 150 ~ 200r/min.
Preferably, step（1）The ultrasonic frequency of the sonic oscillation is 50 ~ 70kHz, and power density is 0.6 ~ 1.2W/
cm2。
Preferably, step（2）The temperature of the drying is 110 ~ 130 DEG C, and the time is 2 ~ 4h.
Preferably, step（3）The heat temperature raising speed is 60 ~ 100 DEG C/min.
The present invention also provides a kind of cathode of lithium battery for layered nano-graphene that above-mentioned preparation method is prepared
Material.
The material takes off lithium in absolute ethyl alcohol by silicon lithium alloy and forms sheet silicon nanometer sheet, uniformly divides through ultrasonic vibration
It dissipates in the absolute ethyl alcohol containing graphene oxide, graphene oxide is wrapped in silicon nanometer sheet table since specific surface area is excessive and spontaneous
Layer, is reduced to graphene layer, while improving graphene layer and silicon nanoscale twins finally by high-temperature heat treatment by graphene oxide
Binding force, be made layered nano-graphene lithium cell cathode material.Compared with conventional method, preparation of the invention
Lithium cell cathode material forms the sandwich of graphene and silicon chip, and graphene layer is made to alleviate 2d laminar nano silicon chips in lithium
Volume deformation during ion deinsertion effectively increases the stability of negative material, and preparation process is simply controllable, process
Environment friendly and pollution-free, remaining ethyl alcohol containing anhydrous lithium can be recycled and be used as lithium source, and the production time is short, and it is extensive to be easy to industrialization
Production.
The present invention provides a kind of lithium cell cathode materials and preparation method of layered nano-graphene, with existing skill
Art is compared, and the feature and excellent effect protruded is：
1. lithium cell cathode material prepared by the present invention has fabulous application prospect in field of lithium.
2. the preparation method of the present invention, the negative material of the sandwich by forming graphene and silicon chip, make graphene
Layer alleviates volume deformation of 2d laminar nanos silicon chip during lithium ion deintercalation, effectively increases the stability of negative material.
3. the preparation process of the present invention is simply controllable, process is environment friendly and pollution-free, and remaining ethyl alcohol containing anhydrous lithium can recycle
It is used as lithium source, the production time is short, is easy to industrialization large-scale production.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
By 23kg Li12Si7、49kg Li7Si3、28kgLi13Si4It is mixed to get silicon lithium alloy powder, 26kg silicon lithiums is then taken to close
Bronze end is scattered in absolute ethyl alcohol, and magnetic agitation 3h is carried out with the rotating speed of 170r/min under the conditions of argon gas, is then added and is divided
Dissipating has in the absolute ethyl alcohol of 7kg graphene oxides, and the quality of absolute ethyl alcohol is 67kg, is 60kHz in ultrasonic frequency, power is close
Degree is 0.8W/cm2Ultrasonic wave under carry out sonic oscillation 9min, be made dispersion liquid；Dispersion liquid is closed, it is 22 in environment temperature
It is aged 26h at DEG C, then filters, 3h is dried at 118 DEG C, negative material presoma is made；Under protection of argon gas by presoma
800 DEG C are quickly heated up to the heating rate of 67 DEG C/min, handles 2min, sheet nano-silicon-graphene layer structure is made
Negative material.
Test method：
Negative material produced by the present invention is prepared into cathode by collector, is positive material with 622 nickle cobalt lithium manganate of high ni-type
Material mixes setting with conductive agent, binder on plus plate current-collecting body surface, forms anode, and anode and cathode are passed through PP diaphragms interval
And lithium ion battery is assembled into electrolyte infiltration, carry out charge-discharge performance test.Obtained lithium battery carries out charge and discharge cycles
Number is tested, and under 1C multiplying powers, using DahoMeter digital display type cubical expansivity analyzers, measures charge and discharge cycles 100 respectively
Secondary, 500 times, the cubical expansivities of 1000 negative materials.
The data obtained is as shown in table 1.
Embodiment 2
By 20kg Li12Si7、55kg Li7Si3、25kgLi13Si4It is mixed to get silicon lithium alloy powder, 20kg silicon lithiums is then taken to close
Bronze end is scattered in absolute ethyl alcohol, and magnetic agitation 3h is carried out with the rotating speed of 150r/min under the conditions of argon gas, is then added and is divided
Dissipating has in the absolute ethyl alcohol of 5kg graphene oxides, and the quality of absolute ethyl alcohol is 75kg, is 50kHz in ultrasonic frequency, power is close
Degree is 0.6W/cm2Ultrasonic wave under carry out sonic oscillation 12min, be made dispersion liquid；Dispersion liquid is closed, be in environment temperature
It is aged 30h at 18 DEG C, then filters, 4h is dried at 110 DEG C, negative material presoma is made；Presoma is protected in argon gas
Under with the heating rate of 60 DEG C/min quickly heat up to 800 DEG C, handle 3min, sheet nano-silicon-graphene stratiform knot be made
The negative material of structure.
Test method is consistent with embodiment 1, and the data obtained is as shown in table 1.
Embodiment 3
By 25kg Li12Si7、45kg Li7Si3、30kgLi13Si4It is mixed to get silicon lithium alloy powder, 30kg silicon lithiums is then taken to close
Bronze end is scattered in absolute ethyl alcohol, and magnetic agitation 2h is carried out with the rotating speed of 200r/min under the conditions of argon gas, is then added and is divided
Dissipating has in the absolute ethyl alcohol of 10 kg graphene oxides, and the quality of absolute ethyl alcohol is 60kg, is 70kHz, power in ultrasonic frequency
Density is 1.2W/cm2Ultrasonic wave under carry out sonic oscillation 8min, be made dispersion liquid；Dispersion liquid is closed, be in environment temperature
It is aged 20h at 26 DEG C, then filters, 2h is dried at 130 DEG C, negative material presoma is made；Presoma is protected in argon gas
Under with the heating rate of 100 DEG C/min quickly heat up to 900 DEG C, handle 1min, sheet nano-silicon-graphene stratiform knot be made
The negative material of structure.
Test method is consistent with embodiment 1, and the data obtained is as shown in table 1.
Embodiment 4
By 22kg Li12Si7、52kg Li7Si3、26kgLi13Si4It is mixed to get silicon lithium alloy powder, 22kg silicon lithiums is then taken to close
Bronze end is scattered in absolute ethyl alcohol, and magnetic agitation 3h is carried out with the rotating speed of 160r/min under the conditions of argon gas, is then added and is divided
Dissipating has in the absolute ethyl alcohol of 7 kg graphene oxides, and the quality of absolute ethyl alcohol is 71kg, is 55kHz, power in ultrasonic frequency
Density is 0.8W/cm2Ultrasonic wave under carry out sonic oscillation 11min, be made dispersion liquid；Dispersion liquid is closed, in environment temperature
It is to be aged 28h at 19 DEG C, then filters, 4h is dried at 115 DEG C, negative material presoma is made；Presoma is protected in argon gas
850 DEG C are quickly heated up to the heating rate of 65 DEG C/min under shield, handles 3min, sheet nano-silicon-graphene stratiform is made
The negative material of structure.
Test method is consistent with embodiment 1, and the data obtained is as shown in table 1.
Embodiment 5
By 24kg Li12Si7、48kg Li7Si3、28kgLi13Si4It is mixed to get silicon lithium alloy powder, 28kg silicon lithiums is then taken to close
Bronze end is scattered in absolute ethyl alcohol, and magnetic agitation 2h is carried out with the rotating speed of 190r/min under the conditions of argon gas, is then added and is divided
Dissipating has in the absolute ethyl alcohol of 9 kg graphene oxides, and the quality of absolute ethyl alcohol is 63kg, is 65kHz, power in ultrasonic frequency
Density is 1.1W/cm2Ultrasonic wave under carry out sonic oscillation 9min, be made dispersion liquid；Dispersion liquid is closed, be in environment temperature
25 DEG C, relative humidity is 75% time ageing 22h, then filters, 2.5h is dried at 126 DEG C, negative material presoma is made；It will
Presoma quickly heats up to 980 DEG C with the heating rate of 90 DEG C/min under protection of argon gas, handles 1.5min, and obtained sheet is received
The negative material of rice silicon-graphene layer structure.
Test method is consistent with embodiment 1, and the data obtained is as shown in table 1.
Embodiment 6
By 23kg Li12Si7、50kg Li7Si3、27kgLi13Si4It is mixed to get silicon lithium alloy powder, 25kg silicon lithiums is then taken to close
Bronze end is scattered in absolute ethyl alcohol, is carried out magnetic agitation 2.5h with the rotating speed of 180r/min under the conditions of argon gas, is then added
It is dispersed in the absolute ethyl alcohol of 8kg graphene oxides, the quality of absolute ethyl alcohol is 7kg, is 60kHz, power in ultrasonic frequency
Density is 1W/cm2Ultrasonic wave under carry out sonic oscillation 10min, be made dispersion liquid；Dispersion liquid is closed, be in environment temperature
It is aged 25h at 22 DEG C, then filters, 3h is dried at 120 DEG C, negative material presoma is made；Presoma is protected in argon gas
Under with the heating rate of 80 DEG C/min quickly heat up to 900 DEG C, handle 2min, sheet nano-silicon-graphene stratiform knot be made
The negative material of structure.
Test method is consistent with embodiment 1, and the data obtained is as shown in table 1.
Comparative example 1
In negative material forerunner's production procedure, the absolute ethyl alcohol of graphene oxide is not used, does not carry out sonic oscillation and high temperature
Heat treatment, other preparation conditions are consistent with embodiment 6.
Test method is consistent with embodiment 1, and the data obtained is as shown in table 1.
Table 1：
Claims (8)
1. a kind of preparation method of the lithium cell cathode material of layered nano-graphene, which is characterized in that pass through silicon lithium alloy
Lithium is taken off in absolute ethyl alcohol and forms sheet silicon nanometer sheet, and the absolute ethyl alcohol containing graphene oxide is dispersed in through ultrasonic vibration
In, graphene oxide is wrapped in silicon nanometer sheet surface layer since specific surface area is excessive and spontaneous, finally by high-temperature heat treatment by oxygen
Graphite alkene is reduced to graphene layer, while improving the binding force of graphene layer and silicon nanoscale twins, and layered nano-stone is made
The lithium cell cathode material of black alkene, preparation are as follows：
（1）Silicon lithium alloy powder is scattered in absolute ethyl alcohol, 2 ~ 3h of magnetic agitation is carried out under the conditions of argon gas, makes silicon lithium alloy
Lithium is taken off in absolute ethyl alcohol and forms sheet silicon nanometer sheet, is then added and is dispersed in the absolute ethyl alcohol of graphene oxide, ultrasound
8 ~ 12min is vibrated, graphene oxide is spontaneous in ultrasonic procedure to be wrapped in the surface layer of silicon nanometer sheet, and is dispersed in anhydrous second
In alcohol, dispersion liquid is made；
（2）By step（1）Dispersion liquid obtained is closed, is aged 20 ~ 30h, then filters, dries, negative material presoma is made；
（3）By step（2）Negative material presoma obtained quickly heats up to 800 ~ 1000 DEG C under protection of argon gas, and processing 1 ~
3min makes graphene oxide be reduced to graphene layer, and the negative material of sheet nano-silicon-graphene layer structure is made.
2. a kind of preparation method of the lithium cell cathode material of layered nano-graphene according to claim 1, feature
It is：Step（1）The silicon lithium alloy powder is Li12Si7 、Li7Si3 、Li13Si4At least one of.
3. a kind of preparation method of the lithium cell cathode material of layered nano-graphene according to claim 1, feature
It is：Step（1）In the dispersion liquid, 20 ~ 30 parts by weight of silicon lithium alloy powder, 5 ~ 10 parts by weight of graphene oxide, anhydrous second
60 ~ 75 parts by weight of alcohol.
4. a kind of preparation method of the lithium cell cathode material of layered nano-graphene according to claim 1, feature
It is：Step（1）The rotating speed of the magnetic agitation is 150 ~ 200r/min.
5. a kind of preparation method of the lithium cell cathode material of layered nano-graphene according to claim 1, feature
It is：Step（1）The ultrasonic frequency of the sonic oscillation is 50 ~ 70kHz, and power density is 0.6 ~ 1.2W/cm2。
6. a kind of preparation method of the lithium cell cathode material of layered nano-graphene according to claim 1, feature
It is：Step（2）The temperature of the drying is 110 ~ 130 DEG C, and the time is 2 ~ 4h.
7. a kind of preparation method of the lithium cell cathode material of layered nano-graphene according to claim 1, feature
It is：Step（3）The heat temperature raising speed is 60 ~ 100 DEG C/min.
8. the lithium cell cathode material that any one of claim 1 ~ 7 preparation method is prepared.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111446417A (en) * | 2019-01-16 | 2020-07-24 | 通用汽车环球科技运作有限责任公司 | High performance electroactive materials in sandwich structures |
| CN112421035A (en) * | 2020-11-02 | 2021-02-26 | 成都新柯力化工科技有限公司 | Preparation method of silicon oxide nanosheet composite ternary lithium battery cathode material |
| CN114180570A (en) * | 2021-12-07 | 2022-03-15 | 远景动力技术(江苏)有限公司 | Silicon-carbon negative electrode material and preparation method and application thereof |
-
2018
- 2018-04-20 CN CN201810357700.4A patent/CN108666546A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111446417A (en) * | 2019-01-16 | 2020-07-24 | 通用汽车环球科技运作有限责任公司 | High performance electroactive materials in sandwich structures |
| CN111446417B (en) * | 2019-01-16 | 2023-06-06 | 通用汽车环球科技运作有限责任公司 | High performance electroactive materials within sandwich structures |
| CN112421035A (en) * | 2020-11-02 | 2021-02-26 | 成都新柯力化工科技有限公司 | Preparation method of silicon oxide nanosheet composite ternary lithium battery cathode material |
| CN114180570A (en) * | 2021-12-07 | 2022-03-15 | 远景动力技术(江苏)有限公司 | Silicon-carbon negative electrode material and preparation method and application thereof |
| CN114180570B (en) * | 2021-12-07 | 2023-01-31 | 远景动力技术(江苏)有限公司 | Silicon-carbon negative electrode material and preparation method and application thereof |
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