CN107305949A - A kind of porous graphite negative material and preparation method and application - Google Patents
A kind of porous graphite negative material and preparation method and application Download PDFInfo
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- CN107305949A CN107305949A CN201610259976.XA CN201610259976A CN107305949A CN 107305949 A CN107305949 A CN 107305949A CN 201610259976 A CN201610259976 A CN 201610259976A CN 107305949 A CN107305949 A CN 107305949A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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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- 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 discloses a kind of porous graphite negative material and preparation method and application.The porous graphite negative material includes porous graphite, to being available for the freely through nano pore of lithium ion less than being distributed between the stratiform face of graphite crystal in the porous graphite.It is preferred that, the aperture of the nano pore is 1 500 nm, and the specific surface area of the porous graphite is 1 8m3/g.The present invention on the stratiform face of graphite and end face by etching metal or metallic compound, obtain more hole, the specific surface area of graphite is effectively increased on the basis of reduction graphitic conductive is not apparent from, the speed that lithium ion enters graphite is added simultaneously, reducing graphite surface electrolyte under high power charging-discharging, quickly consumption and lithium deposit negative effect, hence it is evident that improve the fast charging and discharging capacity of graphite cathode.The preparation method for the porous graphite negative material that the present invention is provided is simple, and condition is easily-controllable, and the heat treatment temperature used is relatively low, meets energy-saving and emission-reduction and Green Chemistry principle.
Description
Technical field
The present invention relates to a kind of porous graphite negative material and preparation method and application, belong to field of lithium ion battery material.
Background technology
With the progressively enhancing of environmental consciousness, using lithium ion battery as the electric automobile of power source and the application model of portable type electronic product
Enclose and progressively expand, but be due to current lithium ion battery specific capacity it is relatively low, wanting for electric automobile and electronic product can not have been met
The endurance asked.Therefore, quick charge turns into can alleviate the effective way of this case at present.At present, battery fills process soon
Graphite cathode material is most commonly used that in middle lithium ion battery.The micron-sized lamellar structure of graphite causes what lithium ion spread in graphite
Distance is very long, and this seriously constrains the performance that lithium ion is quickly embedded in graphite cathode material, and substantial amounts of lithium ion can be on the surface of graphite
Active lithium metal crystallite or big dendrite are reduced to, while active lithium metal easily reacts with electrolyte and releases heat,
Not only can also there is the hidden danger of thermally-induced cells burst in consumption electrolyte reduction battery capacity.
In order to improve the quick embedding lithium performance of graphite cathode, the porosity of graphite material can be increased to alleviate.For example, Zhang et al.
(J.Mater.Chem.A, 2014,2,10161-10168) is obtained using conductive black and organic carbon source as raw material by being spray-dried
Porous carbon ball, is then prepared for the graphited carbon micron-spheres of porous highly of core shell structure by (2800 DEG C) processing of high temperature.But it is high
Warm condition can cause substantial amounts of energy resource consumption, not meet energy-saving and emission-reduction and Green Chemistry principle.In another example, there is researcher to pass through poly-
The Louis acid catalysis on phenylethylene micro ball surface is carbonized to obtain porous graphite microballoon, but is due to that heat treatment temperature is relatively low, its stone
Blackization degree is relatively low.In another example, there is researcher to etch stone with reaction solid/liquid/gas reactions with metal or metallic compound catalytic graphite
Black surface, obtains preferable porous graphite, but its reaction temperature is still higher.
The content of the invention
It is an object of the invention to provide a kind of porous graphite negative material and preparation method thereof, to overcome deficiency of the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
A kind of porous graphite negative material is provided in the embodiment of the present invention, it is included in porous graphite, the porous graphite to being less than
It is distributed between the stratiform face of graphite crystal and is available for the freely through nano pore of lithium ion.
Further, the nano pore is distributed between the stratiform face of graphite crystal and on stratiform face in the porous graphite, and
And the nano pore is mainly distributed between the stratiform face of graphite
A kind of preparation method of porous graphite negative material is additionally provided in the embodiment of the present invention to be included：
In graphite surface uniform load metal and/or compound comprising metallic element, compound is formed；
The compound is heat-treated in oxygen-containing atmosphere, porous graphite material is formed.
The purposes of the porous graphite negative material is additionally provided in the embodiment of the present invention.
For example, the embodiments of the invention provide a kind of lithium ion battery, it is comprising described porous graphite negative material or by foregoing
Porous graphite negative material prepared by a kind of method.
Compared with prior art, advantages of the present invention includes：
(1) the porous graphite negative material provided is obtained by etching metal or metallic compound on the stratiform face of graphite and end face
More hole, the specific surface area that graphite is effectively increased on the basis of reduction graphitic conductive is not apparent from is (reachable
8m3/ g), while adding the speed that lithium ion enters graphite, reduce graphite surface electrolyte under high power charging-discharging and quickly consume
Deposit and negatively affect with lithium, hence it is evident that improve the fast charging and discharging capacity of graphite cathode.
(2) preparation method of the porous graphite negative material provided is simple, and condition is easily-controllable, and the heat treatment temperature used is relatively low, symbol
Close energy-saving and emission-reduction and Green Chemistry principle.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, embodiment or prior art will be retouched below
The accompanying drawing used required in stating is briefly described, it should be apparent that, drawings in the following description are only described in the present invention
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to these
Accompanying drawing obtains other accompanying drawings.
Fig. 1 is ESEM (SEM) figure that the embodiment of the present invention 2 obtains Delanium porous material；
Fig. 2 is ESEM (SEM) figure that the embodiment of the present invention 4 obtains Delanium porous material；
Fig. 3 is ESEM (SEM) figure that the embodiment of the present invention 5 obtains Delanium porous material；
Fig. 4 a- Fig. 4 b are ESEM (SEM) figures that the embodiment of the present invention 6 obtains Delanium porous material；
Fig. 5 a- Fig. 5 b are ESEM (SEM) figures that the embodiment of the present invention 7 obtains Delanium porous material；
Fig. 6 is the discharge-rate performance map of obtained half-cell in the embodiment of the present invention 3；
Fig. 7 is the discharge-rate performance map of obtained half-cell in the embodiment of the present invention 6；
Fig. 8 is the discharge-rate performance map of obtained half-cell in the embodiment of the present invention 7.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, the embodiment to the present invention is entered below in conjunction with the accompanying drawings
Row is described in detail.The example of these preferred embodiments is illustrated in the accompanying drawings.The sheet described shown in accompanying drawing and with reference to the accompanying drawings
What the embodiment of invention was merely exemplary, and the present invention is not limited to these embodiments.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, illustrate only in the accompanying drawings
With according to the solution of the present invention closely related structure and/or process step, and eliminate with the little other details of relation of the present invention.
Provided in the embodiment of the present invention in a kind of porous graphite negative material, including porous graphite, the porous graphite to less than stone
It is distributed between the stratiform face of smoky quartz body and is available for the freely through nano pore of lithium ion.
Further, the nano pore is distributed between the stratiform face of graphite crystal and on stratiform face in the porous graphite, and
And the nano pore is mainly distributed between the stratiform face of graphite.
It is preferred that, the aperture of the nano pore is 1-500nm.
It is preferred that, the specific surface area of the porous graphite is 1-8m3/g。
A kind of preparation method of porous graphite negative material is additionally provided in the embodiment of the present invention to be included：
In graphite surface uniform load metal and/or compound comprising metallic element, compound is formed；
The compound is heat-treated in oxygen-containing atmosphere, porous graphite material is formed；
The metal that removing is remained in the porous graphite material and/or the compound comprising metallic element, obtain the porous graphite and bear
Pole material.
In one more preferred embodiment, the preparation method of the porous graphite negative material includes：
1) colloidal solution or uniform dispersion of metal or metallic compound are prepared；
2) by colloidal solution or dispersion liquid and graphite combination drying, compound is obtained；
3) under oxygenous gas atmosphere, compound in 2) is heat-treated, makes graphite and metal or metallic compound anti-
Should, obtain the graphite porous material with nano pore；
4) metal or metallic compound of residual are removed with dilute acid soln, porous graphite cathode material is obtained after drying.
More preferred, the metal or the compound comprising metallic element include any one in Fe, Co, Ni, Cu, Zn
Or two or more combinations, but not limited to this.
More preferred, the compound comprising metallic element includes oxide, hydroxide, halide, nitrate, sulfuric acid
Any one in salt, carbonate, acylate or metal acid-salt or two or more combinations, but not limited to this.
Further, the compound includes 2wt%-50wt% metals and/or the compound comprising metallic element.
More preferred, the graphite is selected from native graphite or Delanium.
It is more preferred, mixed Daqu of the oxygen-containing atmosphere by oxygen or comprising oxygen, preferably air atmosphere.
Further, the temperature used that is heat-treated is 400 DEG C~1000 DEG C.
Further, the temperature that the heat treatment is used is more than or equal to 450 DEG C and is less than 500 DEG C.
Further, the time of the heat treatment is 0.5h~50h.
Further, the metal that remains in the porous graphite material and/or the chemical combination comprising metallic element are removed using pickling mode
Thing.
It is more preferred, the acid used in the pickling mode include hydrochloric acid, sulfuric acid, nitric acid into any one or it is two or more
Combination, but not limited to this.
By being etched along the direction parallel to graphite laminate face in the present invention, i.e., end face is etched, with the extension of etch period, stratiform
Space between face can be more and more, because the key reaction of etching makes generation at the edge (i.e. end face) in graphite laminate face, so may be used
So that the exposed area of end face is significantly increased, so as to so that Li ions quickly embedded graphite, and then graphite cathode can be significantly improved
Fast charging and discharging capacity.
Present invention also offers the purposes of described porous graphite negative material.For example, the embodiment of the present invention additionally provide a kind of lithium from
Sub- battery, its porous graphite negative material prepared comprising described porous graphite negative material or by foregoing any method.
The technology of the present invention is further explained below in conjunction with drawings and examples.
Embodiment 1：Take 0.68g FeCl3·6H2O is dissolved into 80ml water, then adds 20ml ethanol and 20g graphite (graphite
Initial specific surface be 0.95m3/ g) and 3h is stirred, it is 9-10 or so to add ammoniacal liquor and adjust the pH value of solution, continues to stir
Mix and 3h is stood after solution 3-5h, filter and dried in 80 DEG C of baking ovens, obtain surface deposition Fe (OH)3Graphite composite wood
Material；The compound is placed in Muffle furnace again and 0.5h is kept at 500 DEG C, the graphite material with etching duct has been obtained；Most
100 DEG C of drying in remaining iron oxide reactant, baking oven are removed with dilute HCl solution afterwards, is made and contains 1wt%Fe2O3Delanium
Porous material.
It is coated in after the Delanium porous material is mixed with acetylene black, binding agent on copper foil and cathode pole piece is made, is assembled with lithium piece
Button half-cell is made, constant current charge-discharge test high rate performance (1C=370mAh/g) is carried out in 25 DEG C, 0.02-2V voltage ranges,
The charging process that discharge process in half-cell corresponds in full battery.
Embodiment 2：Take 2.03g FeCl3·6H2O is dissolved into 80ml water, then adds 20ml ethanol and 20g graphite and stirring
It is 9-10 or so that 3h, which adds ammoniacal liquor and adjusts the pH value of solution, continues to stand 3h after stirring solution 3-5h, refilter and
Dried in 80 DEG C of baking ovens, obtain surface deposition Fe (OH)3Graphite composite material；Again by the compound be placed in Muffle furnace and
0.5h is kept at 500 DEG C, the graphite material with etching duct has been obtained, it is anti-finally to remove remaining iron oxide with dilute HCl solution
100 DEG C of drying in thing, baking oven are answered, is made and contains 3wt%Fe2O3Delanium porous material.Shown in Figure 1 is the artificial stone
ESEM (SEM) figure of black porous material.
Embodiment 3：Take 3.38g FeCl3·6H2O is dissolved into 80ml water, is then added the graphite of 20ml ethanol and 20g and is stirred
It is 9-10 or so to mix 3h and add ammoniacal liquor and adjust the pH value of solution, continues to stir being refiltered simultaneously after standing 3h after solution 3-5h
Dried in 80 DEG C of baking ovens, obtain surface deposition Fe (OH)3Graphite composite material；Again by the compound be placed in Muffle furnace and
0.5h is kept at 500 DEG C, the graphite material with etching duct has been obtained, it is anti-finally to remove remaining iron oxide with dilute HCl solution
100 DEG C of drying in thing, baking oven are answered, is made and contains 5wt%Fe2O3Delanium porous material.
It is coated in after the Delanium porous material is mixed with acetylene black, binding agent on copper foil and cathode pole piece is made, is assembled with lithium piece
Button half-cell is made, constant current charge-discharge test high rate performance (1C=370mAh/g) is carried out in 25 DEG C, 0.02-2V voltage ranges,
The charging process that discharge process in half-cell corresponds in full battery.Referring to the discharge-rate performance that Fig. 6 is obtained half-cell
Figure.
Embodiment 4：Take 2.03g FeCl3·6H2O is dissolved into 80ml water, is then added the graphite of 20ml ethanol and 20g and is stirred
It is 9-10 or so to mix 3h and add ammoniacal liquor and adjust the pH value of solution, continues to stir standing 3h after solution 3-5h and filters afterwards again simultaneously
Dried in 80 DEG C of baking ovens, obtain surface deposition Fe (OH)3Graphite composite material；Again by the compound be placed in Muffle furnace and
2h is kept at 500 DEG C, the graphite material with etching duct has been obtained, finally removing remaining iron oxide with dilute HCl solution reacts
100 DEG C of drying in thing, baking oven, are made and contain 3wt%Fe2O3Delanium porous material.It is that the Delanium is porous referring to Fig. 2
ESEM (SEM) figure of material.
Embodiment 5：Take 3.38g FeCl3·6H2O is dissolved into 4ml water and forms saturated solution, is added dropwise to shape in 80ml boiling water
Into stable colloidal solution, then 20g graphite is added thereto and stirring 3h makes the two uniformly mix, continuing heating makes colloidal coagulation exist
Graphite surface, then filtering and the drying in 80 DEG C of baking ovens after 3h are stood, obtain surface deposition Fe (OH)3Graphite composite material it
The compound is placed in Muffle furnace afterwards and 6h is kept at 500 DEG C, the graphite material with etching duct has been obtained, finally with dilute
HCl solution removes 100 DEG C of drying in remaining iron oxide reactant, baking oven, is made and contains 5wt%Fe2O3The porous material of Delanium
Material.The specific surface area of material is 3.06m3/g.Referring to ESEM (SEM) figure that Fig. 3 is the Delanium porous material.
Embodiment 6：Take 3.38g FeCl3·6H2O is dissolved into 4ml water and forms saturated solution, is added dropwise to shape in 80ml boiling water
Into stable colloidal solution, then 20g graphite is added thereto and stirring 3h makes the two uniformly mix, continuing heating makes colloidal coagulation exist
Graphite surface, then filtering and the drying in 80 DEG C of baking ovens after 3h are stood, obtain surface deposition Fe (OH)3Graphite composite material it
The compound is placed in Muffle furnace afterwards and 12h is kept at 500 DEG C, the graphite material with etching duct has been obtained, has finally used
Dilute HCl solution removes 100 DEG C of drying in remaining iron oxide reactant, baking oven, is made and contains 5wt%Fe2O3Delanium it is porous
Material.Referring to ESEM (SEM) figure that Fig. 4 a- Fig. 4 b are the Delanium porous material.
It is coated in after the Delanium porous material is mixed with acetylene black, binding agent on copper foil and cathode pole piece is made, is assembled with lithium piece
Button half-cell is made, constant current charge-discharge test high rate performance (1C=370mAh/g) is carried out in 25 DEG C, 0.02-2V voltage ranges,
The charging process that discharge process in half-cell corresponds in full battery.Referring to the discharge-rate performance that Fig. 7 is obtained half-cell
Figure.
Embodiment 7：Take 3.38g FeCl3·6H2O is dissolved into 4ml water and forms saturated solution, is added dropwise to shape in 80ml boiling water
Into stable colloidal solution, then 20g graphite is added thereto and stirring 3h makes the two uniformly mix, continuing heating makes colloidal coagulation exist
Graphite surface, then filtering and the drying in 80 DEG C of baking ovens after 3h are stood, obtain surface deposition Fe (OH)3Graphite composite material it
The compound is placed in Muffle furnace afterwards and 20h is kept at 500 DEG C, the graphite material with etching duct has been obtained, has finally used
Dilute HCl solution removes 100 DEG C of drying in remaining iron oxide reactant, baking oven, is made and contains 5wt%Fe2O3Delanium it is porous
Material, its specific surface area is 4.73m3/g.Referring to ESEM (SEM) figure that Fig. 5 a- Fig. 5 b are the Delanium porous material.
It is coated in after the Delanium porous material is mixed with acetylene black, binding agent on copper foil and cathode pole piece is made, is assembled with lithium piece
Button half-cell is made, constant current charge-discharge test high rate performance (1C=370mAh/g) is carried out in 25 DEG C, 0.02-2V voltage ranges,
The charging process that discharge process in half-cell corresponds in full battery.Referring to the discharge-rate performance that Fig. 8 is obtained half-cell
Figure.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with technique
Personage can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all smart according to the present invention
The equivalent change or modification that refreshing essence is made, should all be included within the scope of the present invention.
Claims (13)
- It is distributed between 1. the stratiform face of graphite crystal is extremely less than in a kind of porous graphite negative material, it is characterised in that including porous graphite, the porous graphite and is available for the freely through nano pore of lithium ion.
- 2. porous graphite negative material according to claim 1, it is characterised in that：The nano pore is distributed between the stratiform face of graphite crystal and on stratiform face in the porous graphite, and the nano pore is mainly distributed between the stratiform face of graphite；And/or, the aperture of the nano pore is 1-500 nm；And/or, the specific surface area of the porous graphite is 1-8m3/g。
- 3. a kind of preparation method of porous graphite negative material, it is characterised in that including：In graphite surface uniform load metal and/or compound comprising metallic element, compound is formed；The compound is heat-treated in oxygen-containing atmosphere, porous graphite material is formed；The metal that removing is remained in the porous graphite material and/or the compound comprising metallic element, obtain the porous graphite negative material.
- 4. preparation method according to claim 3, it is characterised in that：The metal or compound comprising metallic element include any one or two or more combinations in Fe, Co, Ni, Cu, Zn.
- 5. the preparation method according to claim 3 or 4, it is characterised in that：The compound comprising metallic element includes any one or two or more combinations in oxide, hydroxide, halide, nitrate, sulfate, carbonate, acylate or metal acid-salt.
- 6. preparation method according to claim 3, it is characterised in that：The compound includes 2wt%-50wt% metals and/or the compound comprising metallic element.
- 7. preparation method according to claim 3, it is characterised in that：The graphite is selected from native graphite or Delanium.
- 8. preparation method according to claim 3, it is characterised in that：Mixed Daqu of the oxygen-containing atmosphere by oxygen or comprising oxygen, preferably air atmosphere.
- 9. preparation method according to claim 3, it is characterised in that：The temperature used that is heat-treated is less than 500 DEG C for 400 DEG C~1000 DEG C, preferably greater than or equal to 450 DEG C；And/or, the time of the heat treatment is 0.5h~50h.
- 10. preparation method according to claim 3, it is characterised in that including：The metal that remains in the porous graphite material and/or the compound comprising metallic element are removed using pickling mode.
- 11. preparation method according to claim 10, it is characterised in that the acid used in the pickling mode includes any one or the two or more combinations of hydrochloric acid, sulfuric acid, nitric acid into.
- 12. preparation method according to claim 3, it is characterised in that including：Metal and/or the colloidal solution or uniform dispersion of the compound comprising metallic element are provided；The colloidal solution or uniform dispersion are uniformly applied to graphite surface, so that in graphite surface uniform load metal and/or compound comprising metallic element.
- 13. a kind of lithium ion battery, it is characterised in that comprising the porous graphite negative material any one of claim 1-2 or porous graphite negative material prepared by the method as any one of claim 3-12.
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| CN114477158B (en) * | 2020-10-27 | 2023-08-04 | 武汉大学 | C-axis pore-forming graphite and preparation method and application thereof |
| CN112952070A (en) * | 2021-04-08 | 2021-06-11 | 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 | Graphite lithium battery negative electrode material and preparation method thereof |
| CN113903902A (en) * | 2021-09-14 | 2022-01-07 | 三目新材料科技(河南)有限公司 | Preparation method of porous magnetic graphite negative electrode material for lithium ion battery |
| CN113903902B (en) * | 2021-09-14 | 2023-11-28 | 三目新材料科技(河南)有限公司 | Preparation method of porous magnetic graphite anode material for lithium ion battery |
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