CN106299290A - A kind of amorphous Mn oxide/graphite composite nano materials and preparation method thereof and the application in lithium ion battery - Google Patents
A kind of amorphous Mn oxide/graphite composite nano materials and preparation method thereof and the application in lithium ion battery Download PDFInfo
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- CN106299290A CN106299290A CN201610816354.2A CN201610816354A CN106299290A CN 106299290 A CN106299290 A CN 106299290A CN 201610816354 A CN201610816354 A CN 201610816354A CN 106299290 A CN106299290 A CN 106299290A
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- 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
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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
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
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- 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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Abstract
The invention discloses a kind of amorphous Mn oxide/graphite composite nano materials and preparation method thereof and the application in lithium ion battery, belong to lithium ion battery material technical field.This preparation method is: by graphite, potassium permanganate ball milling in aqueous, be washed out, ultrasonic, be dried to obtain amorphous Mn oxide/graphite composite nano materials.In resulting materials of the present invention, the mass fraction of graphite is 5.2 ~ 58.6%, when lithium ion battery negative, has the electrical property of excellence, at 200mA g‑1Electric current density under circulate 250 circle after, remain to keep 977 mA h g‑1Reversible capacity, and at high current density (1000 mA g‑1Under conditions of), after circulation 200 circle, reversible capacity is maintained to 300 mA h g‑1Above.
Description
Technical field
The invention belongs to lithium ion battery material technical field, be specifically related to that a kind of amorphous Mn oxide/graphite is compound to be received
Rice material and preparation method thereof and the application in lithium ion battery.
Background technology
Currently, the highly desirable exploitation of society being the theme with the energy, information and environment efficiently, cleaning and reusable edible
Novel energy.Rechargeable lithium ion batteries, as one of green energy resource, has been a great concern.Design, synthesis has height can
Inverse capacity, excellent high rate performance, the cycle life of overlength and cheap lithium cell cathode material are that lithium ion battery is important
One of developing direction.There is the transition metal oxide of high theoretical capacity, including CoO, Co3O4、Fe2O3、SnO2、Mn3O4、MoO2
Deng, it is promising new ideas lithium cell cathode material.Wherein Mn oxide (MnOx), including MnO, Mn3O4、Mn2O3、MnO2,
Because it has low voltage platform (0.2V～0.4V), high theoretical capacity (such as MnO2Theoretical capacity be 1223mAh g-1)、
The features such as environmental friendliness, are increasingly subject to the concern of people.Mn oxide negative material is lithium and Mn oxide in charge and discharge process
The redox reaction occurred, reaction equation is as follows:
In de-/process of intercalation, there is huge stereomutation in Mn oxide, causes material capacity to decay rapidly；Separately
Outward, the electric conductivity of Mn oxide difference makes high rate performance the best.Therefore, the volumetric expansion of inhibitory activity material and increase electric conductivity
It it is the important means improving material electrochemical performance.Engineer of the present invention, synthesize the amorphous state Mn oxide of mineral carbon load
Nano-particle is to improve the chemical property of material.
There are some researches show, amorphous material is provided that more storage lithium position and shorter lithium ion the evolving path.
Juchen Guo et al. utilizes spray drying method to be prepared for amorphous phase MnOxThe nano-particle of-C, and it is applied to lithium-ion electric
Pond negative material.In de-, process of intercalation, the MnO of amorphous phasexReaction rate is big, at 200mA g-1135 are circulated under electric current density
After circle, its reversible capacity is maintained as 650mAh g-1。
The present invention passes through simple ball-milling technology, successfully synthesizes uniform load amorphous phase MnO on graphite flakexNanometer
Granule.When for lithium ion battery negative material, amorphous phase Mn oxide/graphite composite nano materials has the circulation of excellence
Stability, at 200mA g-1Electric current density under circulate 250 circle after, material can keep 977mAh g-1Reversible capacity.This
Bright have the advantages such as technique is simple, cheaper starting materials is easy to get, low cost, environmental friendliness, efficiency are high, can be with large-scale industrial application.
Summary of the invention
In order to make up the deficiencies in the prior art, primary and foremost purpose of the present invention is to provide a kind of amorphous Mn oxide/graphite and is combined
Nano material.
Another object of the present invention be to provide the above-mentioned amorphous Mn oxide/low cost of graphite composite nano materials, high efficiency,
The method that can prepare on a large scale.
Still a further object of the present invention be to provide above-mentioned amorphous phase Mn oxide/graphite composite nano materials as high-performance lithium from
The application of sub-cell negative electrode material.
The object of the invention is achieved through the following technical solutions.
A kind of preparation method of amorphous Mn oxide/graphite composite nano materials, the method is ball-milling method, specifically include with
Lower step:
(1) graphite and KMnO are weighed4, add water and zirconium ball (mill is situated between), ball milling 2～100h；
(2) then product is separated, ultrasonic, filter, wash, be dried, obtained amorphous Mn oxide/graphite composite Nano
Material.
Preferably, more than one during described graphite is native graphite, expanded graphite and Delanium.
Preferably, rotating speed during described ball milling is 300～500rpm.
Preferably, in described amorphous Mn oxide/graphite composite nano materials the mass fraction of graphite be 5.2%～
58.6%.
It is further preferred that the mass fraction of graphite is in described amorphous Mn oxide/graphite composite nano materials
26.7%～43.2%.
It is furthermore preferred that the mass fraction of graphite is 38.3% in described amorphous Mn oxide/graphite composite nano materials.
Preferably, described zirconium ball is 3:1～25:1 with the mass ratio of raw material；Described raw material is graphite and KMnO4。
In above-mentioned preparation method, ball milling mainly has following three kinds of effects；(1) KMnO is made4With graphite generation oxidoreduction
Reaction, generates Mn oxide；(2) number of plies of graphite is efficiently reduced；(3) make amorphous Mn oxide be evenly dispersed in shell
From graphite flake on.
In above-mentioned preparation method, the main purpose of washing is to wash the potassium salt generated in course of reaction off.
A kind of amorphous Mn oxide/graphite composite nano materials prepared by above-described preparation method.
Above-described a kind of amorphous Mn oxide/graphite composite nano materials answering as lithium ion battery negative material
With.
Preferably, above concrete application process is: by amorphous Mn oxide/graphite composite nano materials, carbon black and PVDF
Mixed pulp, is coated on Copper Foil, obtains lithium ion battery negative.
It is further preferred that described application process is: weigh 0.2g amorphous Mn oxide/graphite composite nano materials,
0.025g PVDF, 0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, and magnetic agitation 4h, by material
It is coated on Copper Foil and makes electrode, use lithium metal as electrode is assembled in glove box CR2016 type button cell.
Compared with prior art, the invention have the advantages that and beneficial effect:
(1) present invention uses simple ball-milling method, and one-step synthesis amorphous Mn oxide/graphite composite nano materials also becomes
Merit is applied to lithium ion battery negative material.Amorphous manganese oxide particle is dispersed in the graphite surface of stripping, effectively alleviates
The change in volume that Mn oxide produces in charge and discharge process, the reunion of suppression manganese and oxygen compound, add electric conductivity, improve
The electrochemical stability of material.
(2) present invention uses simple ball-milling method, utilizes the strong oxidation of mechanical force and potassium permanganate, successfully by sky
So graphite peels off into the graphite (10～15 layers) of few number of plies.
(3) the raw material KMnO used by the present invention4The most cheap with graphite, and the method used by the present invention is ball milling
Method, can substantial amounts of synthesize.In addition, the features such as the present invention also has technique simple, pollution-free.Thus, the present invention has greatly
The potential that technical scale produces.
(4) the amorphous Mn oxide/graphite composite nano materials of the present invention has good when lithium ion battery negative
Cycle performance: described composite nano materials, when mass content of graphite is 11.9～43.2%, is 200mA in electric current density
g-1After lower circulation 50～250 circle, reversible capacity is 510～977mAh g-1.Ion cathode material lithium prepared by the visible present invention
Cycle performance is preferable, it is possible to bear the charge and discharge cycles of more than 200 times.
(5) when the amorphous Mn oxide/graphite composite nano materials of the present invention is for lithium ion battery negative, graphite
Amount mark be 26.7～38.3% sample be 1000mA g in electric current density-1After lower circulation 200～250 circle, reversible capacity is
301～331mAh g-1.Lithium ion battery negative material prepared by the visible present invention is still suitable under larger current density, for lithium
Ion battery use under relatively high power provides safeguard.
Accompanying drawing explanation
Fig. 1, Fig. 2 are the amorphous Mn oxide/graphite composite nano materials of the embodiment of the present invention 3 different amplification
TEM schemes.
Fig. 3 is the SEM figure of the embodiment of the present invention 4 gained amorphous Mn oxide/graphite composite nano materials.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
Embodiment 1
Weigh 0.75g graphite, 14.25g potassium permanganate, 75g zirconium ball (mill is situated between) successively, add in ball grinder, more wherein
Add 50ml water, add sealing ring, under 400rpm, react 48h, by the sample obtained after screen cloth leaches the ultrasonic 2h of zirconium ball, use
Distilled water centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 2
Weigh 1.5g graphite, 13.5g potassium permanganate, 75g zirconium ball (mill is situated between) successively, add in ball grinder, then add wherein
Enter 50ml water, add sealing ring, under 400rpm, react 48h, sample will be obtained after screen cloth leaches the ultrasonic 2h of zirconium ball, with distillation
Water centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 3
Weigh 4.5g graphite, 10.5g potassium permanganate, 75g zirconium ball (mill is situated between) successively, add in ball grinder, then add wherein
Enter 50ml water, add sealing ring, under 400rpm, react 48h, sample will be obtained after screen cloth leaches the ultrasonic 2h of zirconium ball, with distillation
Water centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Amorphous Mn oxide/graphite the composite nano materials that the present embodiment prepares TEM under different amplification schemes such as
Shown in Fig. 1, Fig. 2, as seen from the figure, the present invention uses simple ball-milling method, utilizes the strong oxidation of mechanical force and potassium permanganate,
Successfully native graphite is peeled off into the graphite (10～15 layers) of few number of plies.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 4
Weigh 3.75g graphite, 11.25g potassium permanganate, 75g zirconium ball (mill is situated between) successively, add in ball grinder, more wherein
Add 50ml water, add sealing ring, under 400rpm, react 48h, sample will be obtained after screen cloth leaches the ultrasonic 2h of zirconium ball, with steaming
Distilled water centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
The SEM of the amorphous Mn oxide/graphite composite nano materials of the present embodiment gained schemes as shown in Figure 3.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 5
Weigh 3g graphite, 12g potassium permanganate, 75g zirconium ball (mill is situated between) successively, add in ball grinder, then be added thereto to
50ml water, adds sealing ring, reacts 48h, will obtain sample after screen cloth leaches the ultrasonic 2h of zirconium ball, and use distilled water under 400rpm
Centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 6
Weigh 5.25g graphite, 9.75g potassium permanganate, 75g zirconium ball (mill is situated between) successively, add in ball grinder, then add wherein
Enter 50ml water, add sealing ring, under 400rpm, react 48h, sample will be obtained after screen cloth leaches the ultrasonic 2h of zirconium ball, with distillation
Water centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 7
Weigh 7.5g graphite, 7.5g potassium permanganate, 75g zirconium ball (mill is situated between) successively, add in ball grinder, then be added thereto to
50ml water, adds sealing ring, reacts 48h, will obtain sample after screen cloth leaches the ultrasonic 2h of zirconium ball, and use distilled water under 400rpm
Centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 8
Weigh 3g graphite, 12g potassium permanganate, 45g zirconium ball (mill is situated between) successively, add in ball grinder, then be added thereto to
50ml water, adds sealing ring, reacts 2h at 500 rpm, will obtain sample after screen cloth leaches the ultrasonic 2h of zirconium ball, and use distilled water
Centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Embodiment 9
Weigh 3g graphite, 12g potassium permanganate, 375g zirconium ball (mill is situated between) successively, add in ball grinder, then be added thereto to
50ml water, adds sealing ring, reacts 100h at 300 rpm, will obtain sample after screen cloth leaches the ultrasonic 2h of zirconium ball, with distillation
Water centrifuge washing 4 times, is dried 12h at 60 DEG C and obtains amorphous Mn oxide/graphite composite nano materials.
Weigh the amorphous Mn oxide/graphite composite nano materials obtained by 0.2g the present embodiment, 0.025g PVDF,
0.025g carbon black, proceeds to after mixed grinding in vial, adds 1ml NMP, magnetic agitation 4h, is coated on Copper Foil by material
Making electrode, employing lithium metal is as electrode is assembled in glove box CR2016 type button cell, and carries out electrochemistry
Can test.
Performance test:
Material use X-ray diffraction technology (XRD) prepared by above-described embodiment, Raman spectrum (Raman Spectra), Fu
Vertical leaf transformation infrared spectrum (FT-IR), scanning electron microscope (SEM), transmission electron microscope (TEM), thermogravimetric analysis (TGA) are as table
Levy means, its composition, pattern, particle diameter and content of graphite are analyzed.
Battery prepared by above-described embodiment, after shelving 12h, uses cell tester (the new prestige in Shenzhen) and BTS7.5.5 soft
Part, test temperature is room temperature, and electric current density is 50mA g-1～1000mA g-1In the case of, it is carried out constant current charge-discharge and (puts
Electricity blanking voltage is 0.01V, and charging voltage is 3V), the cycle performance of test battery and high rate performance.The electrical property of sample refers to
Table 1.Utilize electrochemical workstation (CHI600E, Shanghai occasion China) that it is circulated voltammetry (CV) and ac impedance measurement.
Table 1
Note: in table, " content of graphite " refers to the mass fraction of graphite in product, is obtained by thermal analyzer.
The present invention utilizes ball-milling method to be prepared for amorphous Mn oxide/graphite composite nano materials, by the ratio of feed change
Example and ratio of grinding media to material carry out the synthesis condition of research material, and the chemical property that have studied respective material includes cycle performance and multiplying power
Performance etc..By comparing 9 embodiments, find that when ratio of grinding media to material is 5:1, mass content of graphite is the sample of 26.7%～43.2%
Product, have good cycle performance, all can be at 200mA g-1500mA h g is kept after circulating 50 circles under electric current density-1With
Upper reversible capacity；And along with the increase of cycle-index, capacity constantly rises, especially mass content of graphite is the sample of 38.3%
Product are after circulation 250 circle, and reversible capacity reaches 977mA h g-1.Meanwhile, even if the sample that mass content of graphite is 43.2% exists
Bigger electric current density (1000mA g-1Under), after circulation 200 circle, also can maintain 331mA h g-1Reversible capacity.
Embodiment is the present invention preferably embodiment, but embodiments of the present invention are not limited by above-described embodiment
System, the change made, modifies, substitutes, combines, simplifies, all under other any spirit without departing from the present invention and principle
Should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. the preparation method of amorphous Mn oxide/graphite composite nano materials, it is characterised in that comprise the following steps:
(1) graphite and KMnO are weighed4, adding water and zirconium ball, ball milling 2 ~ 100h, described zirconium ball is situated between for mill；
(2) then product is separated, ultrasonic, filter, wash, be dried, obtained amorphous Mn oxide/graphite composite Nano material
Material.
Preparation method the most according to claim 1, it is characterised in that described graphite is native graphite, expanded graphite and people
Make in graphite more than one.
Preparation method the most according to claim 1, it is characterised in that rotating speed during described ball milling is 300 ~ 500 rpm.
Preparation method the most according to claim 1, it is characterised in that described amorphous Mn oxide/graphite composite Nano material
In material, the mass fraction of graphite is 5.2% ~ 58.6%.
Preparation method the most according to claim 1, it is characterised in that described amorphous Mn oxide/graphite composite Nano material
In material, the mass fraction of graphite is 26.7% ~ 43.2%.
Preparation method the most according to claim 1, it is characterised in that described amorphous Mn oxide/graphite composite Nano material
In material, the mass fraction of graphite is 38.3%.
Preparation method the most according to claim 1, it is characterised in that described zirconium ball is 3:1 ~ 25 with the mass ratio of raw material:
1；Described raw material is graphite and KMnO4。
8. a kind of amorphous Mn oxide/graphite composite Nano material prepared by the preparation method described in any one of claim 1-7
Material.
9. a kind of amorphous Mn oxide/graphite composite nano materials described in claim 8 is as lithium ion battery negative material
Application.
Application the most according to claim 9, it is characterised in that concrete application process is: by amorphous Mn oxide/graphite
Composite nano materials, carbon black and PVDF mixed pulp, be coated on Copper Foil, obtain lithium ion battery negative.
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| CN114950361A (en) * | 2022-04-29 | 2022-08-30 | 上海交通大学 | Method for preparing composite adsorbent by waste lithium batteries |
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