CN109713266A - A kind of novel cathode material for lithium ion battery and preparation method thereof - Google Patents
A kind of novel cathode material for lithium ion battery and preparation method thereof Download PDFInfo
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- CN109713266A CN109713266A CN201811581630.7A CN201811581630A CN109713266A CN 109713266 A CN109713266 A CN 109713266A CN 201811581630 A CN201811581630 A CN 201811581630A CN 109713266 A CN109713266 A CN 109713266A
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- 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 field of lithium ion battery, it is specifically related to a kind of novel cathode material for lithium ion battery and preparation method thereof.The material is the composite material that ZIF67, ZIF8 and graphene oxide three are formed.The material is the composite material with cross-linked structure that ZIF67, ZIF8 and graphene oxide three are compounded to form by hydro-thermal, it is poor to overcome lithium ion battery negative material charging and discharging capacity and cyclical stability in the prior art, the defect that electrode material easily crushes improves the chemical property of lithium ion battery.
Description
Technical field
The invention belongs to the technical field of lithium ion battery, be specifically related to a kind of novel cathode material for lithium ion battery and
Preparation method.
Background technique
The main energy sources approach of mankind nowadays society is still the non-renewable energy resources such as fossil energy, but with complete
The continuous development of ball population sharply expanded with human economic society, it is this non-renewable, and with Heavy environmental pollution
The non-green energy will be eliminated by history, and develop more environmentally friendly, the higher secondary green energy resource of reliability is just
Become the extremely urgent great energy problem for needing to solve of people.The mainstream two that current people develop and successfully utilize
The secondary energy includes wind energy, solar energy, atomic energy etc., but without exception, the storage of these energy and using requiring phase therewith
Matched energy storage device cooperation could be completed, therefore have many advantages, such as big specific energy, the lithium ion secondary electricity of high reliability
Pond becomes people's focus of interest.
Most classic lithium ion battery is made of four parts, anode, cathode, electrolyte, diaphragm.Anode and cathode are usually
Cobalt acid lithium and graphite, electrolyte use the organic solution (solvent is usually material of organic ethers compound) containing lithium ion, and diaphragm is
Play the high-molecular porous polymer material of buffer action.When battery charges normal work, lithium in lithium cobaltate cathode material from
Sub- deintercalation and go out, in the layer structure that negative electrode material graphite is reached by diaphragm, and in external circuit, electronics is moved to by anode
Cathode.Opposite, ion and the electronics flow direction of discharge process are different from charging process.
Metal organic frame (MOFs) is a kind of new material that metal ion and organic ligand are formed by coordinate bond, it
It is a kind of porous material with periodic topographical structure, different central metallic ions are logical from different organic coordination compounds
The MOF material of a large amount of different type and pattern can be formed by crossing self assembly effect.There are many mutual in this porous material
The duct of connection has quite high Kong Rong and specific surface area, it is considered to be a kind of ideal gas separation and storage material.With
Traditional porous material compares, and this novel MOF material has the advantages that very much: (1) many kinds of: metal ion and to have
The selection of machine ligand is varied, and up to up to ten thousand kinds of the type of various combination；(2) functional: different metal ions with have
Machine ligand is combined the MOF material that can synthesize different function；(3) specific surface area is high, and porosity is big: it is reported that highest
MOFs material specific surface area is up to 10000 m2 g–1More than, it is that previous conventional porous materials are incomparable；(4) hole
Diameter size adjustable: the size in MOF material duct and the type and length of organic linker are closely related.These advantages make
Metal organic frame (MOFs) material gas store with separate, be catalyzed, the every field such as sensor and the energy have it is very wide
Application prospect.
But since the low electric conductivity of metal organic frame limits it in the application of field of batteries, it is urgently to be resolved should
Problem.
Summary of the invention
A kind of Fabrication of High Specific Capacitance is provided it is an object of the invention to the deficiency for current lithium ion battery negative material technology
Lithium ion battery negative material of amount and preparation method thereof, the material are that ZIF67, ZIF8 and graphene oxide three pass through hydro-thermal
The composite material with cross-linked structure being compounded to form overcomes lithium ion battery negative material charge and discharge specific volume in the prior art
Amount and cyclical stability are poor, and the defect that electrode material easily crushes improves the chemical property of lithium ion battery.
The technical solution of the present invention is as follows: a kind of novel cathode material for lithium ion battery is ZIF67, ZIF8 and graphene oxide
Three
The composite material of formation.
The material has cross-linked structure.
The material is that ZIF67, ZIF8 and graphene oxide three are compounded to form by hydro-thermal.
According to mass ratio ZIF67:ZIF8 in the material: graphene oxide is 1:1:100~400.
A kind of preparation method of the novel cathode material for lithium ion battery, comprising the following steps: (1) prepare ZIF67；
(2)
Prepare ZIF8；(3) ZIF67@Go@ZIF8 is prepared；The step (3) preparation ZIF67@Go@ZIF8:a. by ZIF67 and
The mixture of ZIF8 is placed in graphene oxide solution, stirs to get mixed liquor after ultrasound, wherein the mass ratio of ZIF67 and ZIF8
For 1:1；B. mixed liquor is placed in reaction kettle, closed, heat preservation；C. reaction is completed after being cooled to room temperature, centrifuge washing, after dry
Up to ZIF67@Go@ZIF8.
It is specific as follows that the step (3) prepares ZIF67@Go@ZIF8: a. sets 1~2mg of mixture of ZIF67 and ZIF8
In the graphene oxide solution that 50~100mL concentration is 2mg/mL, wherein the mass ratio of ZIF67 and ZIF8 is 1:1；It is super
10~30min is stirred after 30~50min of sound obtains mixed liquor；B. mixed liquor is placed in reaction kettle, it is closed, at 150~180 DEG C
Under the conditions of keep the temperature 10~15 hours；C. reaction is completed after being cooled to room temperature, and centrifuge washing, wherein deionization is washed 3 times, and ethyl alcohol is washed
3 times；Up to ZIF67@Go@ZIF8 after drying 12 hours under the conditions of 60~80 DEG C.
The preparation method of the novel cathode material for lithium ion battery, the specific steps are as follows:
(1) preparation ZIF67:a. prepares A liquid first: dispersing 125~250ml methanol for 5~10mmol cabaltous nitrate hexahydrate
In；Then it prepares B liquid: dispersing 20~40mmol 2-methylimidazole in 125~250ml methanol；B. stirring is in A liquid
Under, B liquid is poured into A liquid, stirring 3~5 minutes is to uniform；C. static aging is sealed for 24 hours；D. centrifuge washing, wherein methanol washes 3
Secondary, ethyl alcohol is washed 3 times；12 hours are dried under the conditions of 60~80 DEG C to get ZIF67 is arrived；
(2) preparation ZIF8:a. prepares A liquid first: dispersing 5~10mmol zinc nitrate hexahydrate in 125~250ml methanol；
Then it prepares B liquid: dispersing 20~40mmol 2-methylimidazole in 125~250ml methanol；B. stirring is in A liquid
Under, B liquid is poured into A liquid, stirring 3~5 minutes is to uniform；C. static aging is sealed for 24 hours；D. centrifuge washing, wherein methanol washes 3
Secondary, ethyl alcohol is washed 3 times；12 hours are dried under the conditions of 60~80 DEG C to get ZIF8 is arrived；
(3) preparing ZIF67@Go@ZIF8:a. and 1~2mg of mixture of ZIF67 and ZIF8 is placed in 50~100mL concentration is 2mg/
mL
Graphene oxide solution in, wherein the mass ratio of ZIF67 and ZIF8 be 1:1；After 30~50min of ultrasound stirring 10~
30min
Obtain mixed liquor；B. mixed liquor is placed in reaction kettle, it is closed, 10~15 hours are kept the temperature under the conditions of 150~180 DEG C；
c.
Reaction is completed after being cooled to room temperature, and centrifuge washing, wherein deionization is washed 3 times, and ethyl alcohol is washed 3 times；In 60~80 DEG C of conditions
Under
Up to ZIF67@Go@ZIF8 after 12 hours dry.
The stirring is magnetic agitation, and revolving speed is 100~300r/min.
The invention has the benefit that material of the present invention is that ZIF67, ZIF8 and graphene oxide three pass through hydro-thermal
It is compound
The composite material with cross-linked structure formed.Not only structure is new for the cross-linked structure of ZIF67 and ZIF8 and graphene oxide
Grain husk, while ZIF67 and ZIF8 are porous organic materials, it is possible to synergistic effect sufficiently promotes the transmission of lithium ion, simultaneously
Graphene oxide has high electric conductivity, can increase electric conductivity, overcome lithium ion battery negative material in the prior art and fill
Specific discharge capacity and cyclical stability are poor, the defect that electrode material easily crushes, and improve chemical property.
ZIF67, ZIF8 and graphene oxide three are combined in complex by the invention by one step hydro thermal method
Together, it seems simple, needs the support of many-sided parameter, data, including ZIF67, the mass parameter of ZIF8 actually；There are also temperature
Range must be arranged according to defined parameter area, any one link slightly mistake just can not cannot get in the present invention
As a result.
Detailed description of the invention
Fig. 1 is ZIF67@Go@ZIF8 material obtained by embodiment 1 as lithium ion battery negative material and is applied to lithium ion
Performance when battery.
Fig. 2 is ZIF67@Go@ZIF8 material obtained by embodiment 1 as lithium ion battery negative material and is applied to lithium ion
Impedance when battery before not recycling.
Specific embodiment
Below by embodiment, the present invention is described in detail.
Involved raw material are commercially available.Wherein graphene oxide purchase has in Nanjing Ji Cang nanosecond science and technology
Limit company, zinc nitrate hexahydrate and cabaltous nitrate hexahydrate purchase are in upper object Science and Technology Ltd., Haikang nangzan, methylimidazole purchase
It buys in Tianjin An Lin imidazoles Co., Ltd.
Embodiment 1
The novel cathode material for lithium ion battery is that ZIF67, ZIF8 and graphene oxide three are compounded to form by hydro-thermal
Tool
The composite material of crosslinking structure.
According to mass ratio ZIF67:ZIF8 in the material: graphene oxide 1:1:200.
The preparation method of the novel cathode material for lithium ion battery, the specific steps are as follows:
(1) preparation ZIF67:a. prepares A liquid first: dispersing 5mmol cabaltous nitrate hexahydrate in 125ml methanol, pinkiness；
Then it prepares B liquid: dispersing 20mmol 2-methylimidazole in 125ml methanol, to clarify color；B. at A liquid with stirring,
B liquid is poured into A liquid, stirring 3 minutes is purple to uniform, becomes cloudy with mixing time；C. static aging is sealed for 24 hours；D. from
Heart washing, wherein methanol is washed 3 times, and ethyl alcohol is washed 3 times；12 hours are dried under the conditions of 60 DEG C to get ZIF67 is arrived；
(2) preparation ZIF8:a. prepares A liquid first: dispersing 5mmol zinc nitrate hexahydrate in 125ml methanol；Then B is prepared
Liquid: it disperses 20mmol 2-methylimidazole in 125ml methanol；B. at A liquid with stirring, B liquid is poured into A liquid, stirring 3
Minute to uniform；C. static aging is sealed for 24 hours；D. centrifuge washing, wherein methanol is washed 3 times, and ethyl alcohol is washed 3 times；Under the conditions of 60 DEG C
12 hours are dried to get ZIF8 is arrived；
(3) it prepares ZIF67@Go@ZIF8:a. and the mixture 1mg of ZIF67 and ZIF8 is placed in the oxygen that 50mL concentration is 2mg/mL
In graphite alkene solution, wherein the mass ratio of ZIF67 and ZIF8 is 1:1；10min is stirred after ultrasonic 30min to be mixed
Liquid,
；B. mixed liquor is placed in reaction kettle, it is closed, 10 hours are kept the temperature under the conditions of 150 DEG C；C. reaction is completed to be cooled to room temperature
Afterwards,
Centrifuge washing, wherein deionization is washed 3 times, and ethyl alcohol is washed 3 times；Under the conditions of 60 DEG C after drying 12 hours to obtain the final product
ZIF67@Go@ZIF8。
The stirring is magnetic agitation, and revolving speed is 100~300r/min.
Using ZIF67@Go@ZIF8 powder obtained as active material, carbon dust is conductive agent, and Kynoar (PVDF) is
Adhesive, and press ZIF67@Go@ZIF8: Kynoar=8:1:1 weight ratio is placed in mixing in mortar, grinding uniformly, then
It instills N-methyl pyrrolidinone solvent (NMP) and is ground to pulpous state, slurry is uniformly applied on copper foil, 60 DEG C of constant temperature is then put into
Dry 12h in drying box pushes flakiness in 5MPa pressure using tablet press machine after drying to constant weight, ZIF67 Go is thus made
ZIF8 anode plate for lithium ionic cell;It is to electrode and reference electrode with lithium metal, lithium hexafluoro phosphate is electrolyte, porous polypropylene
For diaphragm, CR2025 button cell is assembled in the glove box full of argon gas.
By Fig. 1 it is known that when the material is applied to lithium ion battery as lithium ion battery negative material, from its head
Circle capacity is up to 860 mAh/mg, and cyclical stability is also relatively strong, and after 50 circulations, capacity retention still has 70% or so.
As seen in Figure 2, resistance value of the material before no circulation is about 100 or so, so small resistance
Value is to reduce the dissolution of the negative electrode material before not recycling because of the good electric conductivity of ZIF67@Go@ZIF8 material, improves energy
The chemical property of battery is increased while density again.
Embodiment 2
The preparation method of the novel cathode material for lithium ion battery, the specific steps are as follows:
(1) preparation ZIF67:a. prepares A liquid first: dispersing 10mmol cabaltous nitrate hexahydrate in 250ml methanol；Then it makes
Standby B liquid: it disperses 40mmol 2-methylimidazole in 250ml methanol；B. at A liquid with stirring, B liquid is poured into A liquid, stirred
5 minutes are mixed to uniform；C. static aging is sealed for 24 hours；D. centrifuge washing, wherein methanol is washed 3 times, and ethyl alcohol is washed 3 times；In 80 DEG C of items
12 hours are dried under part to get ZIF67 is arrived；
(2) preparation ZIF8:a. prepares A liquid first: dispersing 10mmol zinc nitrate hexahydrate in 250ml methanol；Then B is prepared
Liquid: it disperses 40mmol 2-methylimidazole in 250ml methanol；B. at A liquid with stirring, B liquid is poured into A liquid, stirring 5
Minute to uniform；C. static aging is sealed for 24 hours；D. centrifuge washing, wherein methanol is washed 3 times, and ethyl alcohol is washed 3 times；Under the conditions of 80 DEG C
12 hours are dried to get ZIF8 is arrived；
(3) preparing ZIF67@Go@ZIF8:a. and the mixture 2mg of ZIF67 and ZIF8 is placed in 100mL concentration is 2mg/mL
Graphene oxide solution in, wherein the mass ratio of ZIF67 and ZIF8 be 1:1；30min is stirred after ultrasonic 50min to obtain
It is mixed
Close liquid；B. mixed liquor is placed in reaction kettle, it is closed, 15 hours are kept the temperature under the conditions of 180 DEG C；C. reaction is completed to be cooled to
Room
Wen Hou, centrifuge washing, wherein deionization is washed 3 times, and ethyl alcohol is washed 3 times；Under the conditions of 80 DEG C after drying 12 hours to obtain the final product
ZIF67@Go@ZIF8。
The stirring is magnetic agitation, and revolving speed is 100~300r/min.
Using ZIF67@Go@ZIF8 powder obtained as active material, carbon dust is conductive agent, and Kynoar (PVDF) is
Adhesive, and press ZIF67@Go@ZIF8: Kynoar=8:1:1 weight ratio is placed in mixing in mortar, grinding uniformly, then
It instills N-methyl pyrrolidinone solvent (NMP) and is ground to pulpous state, slurry is uniformly applied on copper foil, 60 DEG C of constant temperature is then put into
Dry 12h in drying box pushes flakiness in 5MPa pressure using tablet press machine after drying to constant weight, ZIF67 Go is thus made
ZIF8 anode plate for lithium ionic cell;It is to electrode and reference electrode with lithium metal, lithium hexafluoro phosphate is electrolyte, porous polypropylene
For diaphragm, CR2025 button cell is assembled in the glove box full of argon gas.
Claims (8)
1. a kind of novel cathode material for lithium ion battery, which is characterized in that the material is ZIF67, ZIF8 and graphene oxide three
The composite material that person is formed.
2. novel cathode material for lithium ion battery according to claim 1, which is characterized in that the material has crosslinking knot
Structure.
3. novel cathode material for lithium ion battery according to claim 1, which is characterized in that the material is ZIF67, ZIF8
It is compounded to form with graphene oxide three by hydro-thermal.
4. novel cathode material for lithium ion battery according to claim 1, which is characterized in that according to mass ratio in the material
ZIF67:ZIF8: graphene oxide is 1:1:100~400.
5. a kind of preparation method of novel cathode material for lithium ion battery described in claim 1, comprising the following steps: (1) prepare
ZIF67；(2) ZIF8 is prepared；(3) ZIF67@Go@ZIF8 is prepared；It is characterized in that, the step (3) prepares ZIF67@Go@
ZIF8:a. the mixture of ZIF67 and ZIF8 are placed in graphene oxide solution, stir to get mixed liquor after ultrasound, wherein
The mass ratio of ZIF67 and ZIF8 is 1:1；B. mixed liquor is placed in reaction kettle, closed, heat preservation；C. reaction is completed to be cooled to room
Wen Hou, centrifuge washing, up to ZIF67 Go ZIF8 after drying.
6. the preparation method of novel cathode material for lithium ion battery according to claim 5, which is characterized in that the step
(3) it is specific as follows to prepare ZIF67@Go@ZIF8: 1~2mg of mixture of ZIF67 and ZIF8 is placed in 50~100mL concentration and is by a.
In the graphene oxide solution of 2mg/mL, wherein the mass ratio of ZIF67 and ZIF8 is 1:1；After 30~50min of ultrasound stirring 10~
30min obtains mixed liquor；B. mixed liquor is placed in reaction kettle, it is closed, 10~15 hours are kept the temperature under the conditions of 150~180 DEG C；
C. reaction is completed after being cooled to room temperature, and centrifuge washing, wherein deionization is washed 3 times, and ethyl alcohol is washed 3 times；Under the conditions of 60~80 DEG C
Up to ZIF67@Go@ZIF8 after 12 hours dry.
7. the preparation method of novel cathode material for lithium ion battery according to claim 6, which is characterized in that specific steps are such as
Under:
(1) preparation ZIF67:a. prepares A liquid first: dispersing 125~250ml methanol for 5~10mmol cabaltous nitrate hexahydrate
In；Then it prepares B liquid: dispersing 20~40mmol 2-methylimidazole in 125~250ml methanol；B. stirring is in A liquid
Under, B liquid is poured into A liquid, stirring 3~5 minutes is to uniform；C. static aging is sealed for 24 hours；D. centrifuge washing, wherein methanol washes 3
Secondary, ethyl alcohol is washed 3 times；12 hours are dried under the conditions of 60~80 DEG C to get ZIF67 is arrived；
(2) preparation ZIF8:a. prepares A liquid first: dispersing 5~10mmol zinc nitrate hexahydrate in 125~250ml methanol；
Then it prepares B liquid: dispersing 20~40mmol 2-methylimidazole in 125~250ml methanol；B. stirring is in A liquid
Under, B liquid is poured into A liquid, stirring 3~5 minutes is to uniform；C. static aging is sealed for 24 hours；D. centrifuge washing, wherein methanol washes 3
Secondary, ethyl alcohol is washed 3 times；12 hours are dried under the conditions of 60~80 DEG C to get ZIF8 is arrived；
(3) preparing ZIF67@Go@ZIF8:a. and 1~2mg of mixture of ZIF67 and ZIF8 is placed in 50~100mL concentration is 2mg/
mL
Graphene oxide solution in, wherein the mass ratio of ZIF67 and ZIF8 be 1:1；After 30~50min of ultrasound stirring 10~
30min
Obtain mixed liquor；B. mixed liquor is placed in reaction kettle, it is closed, 10~15 hours are kept the temperature under the conditions of 150~180 DEG C；
c.
Reaction is completed after being cooled to room temperature, and centrifuge washing, wherein deionization is washed 3 times, and ethyl alcohol is washed 3 times；In 60~80 DEG C of conditions
Under
Up to ZIF67@Go@ZIF8 after 12 hours dry.
8. according to the preparation method of any one of the claim 5-7 novel cathode material for lithium ion battery, which is characterized in that institute
Stating stirring is magnetic agitation, and revolving speed is 100~300r/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022021643A1 (en) * | 2020-07-31 | 2022-02-03 | 广东凯金新能源科技股份有限公司 | Novel lithium-ion battery negative electrode material and preparation method therefor |
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