CN107959004A - A kind of anode material of lithium battery and preparation method of nitrogen-doped graphene and lithium molybdate - Google Patents
A kind of anode material of lithium battery and preparation method of nitrogen-doped graphene and lithium molybdate Download PDFInfo
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- CN107959004A CN107959004A CN201710990860.8A CN201710990860A CN107959004A CN 107959004 A CN107959004 A CN 107959004A CN 201710990860 A CN201710990860 A CN 201710990860A CN 107959004 A CN107959004 A CN 107959004A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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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- 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
- H01M4/48—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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 present invention is suitable for technical field of lithium batteries, there is provided a kind of anode material of lithium battery and preparation method of nitrogen-doped graphene and lithium molybdate, graphite oxide, nitrogen source are dispersed in water to form dispersion liquid, are added ascorbic acid and are thermally formed gel；Appropriate molybdenum trioxide and lithium electricity ternary material are added to stir in above-mentioned mixed gel and is evaporated and is calcined in atmosphere of inert gases, the lithium battery tertiary cathode material that nitrogen-doped graphene and lithium molybdate coat altogether is obtained after cooling.Molybdenum trioxide of the present invention and Graphene gel are total to clad in material surface formation nitrogen-doped graphene and lithium molybdate lithium ion conductor, the good electric conductivity of nitrogen-doped graphene improves the chemical property of material, the use of ascorbic acid additionally aids the processing performance for reducing part residual alkali improvement positive electrode, in addition the clad of lithium salt form can greatly increase diffusion admittance of the lithium ion in electrode material, the transmission rate of lithium ion is improved, so as to improve the high rate performance of material.This method technique is simple, and chemical property improvement is notable.
Description
Technical field
The invention belongs to technical field of lithium ion, more particularly to the lithium battery of a kind of nitrogen-doped graphene and lithium molybdate
Positive electrode and preparation method.
Background technology
Compared to other battery systems, lithium ion battery has high energy density, good cycle and memory-less effect etc.
Advantage, it has been widely used for portable electric appts, electric tool and electronic traffic as a kind of important energy storage device
The fields such as instrument.With developing rapidly for new-energy automobile, wanting for higher is proposed to providing the lithium ion battery of energy for it
Ask, the requirement of especially power-performance and cycle performance is more harsh.Positive electrode is to influence battery performance in lithium ion battery
Key factor, preferable anode material for lithium-ion batteries should possess high power capacity, high magnification, high circulation performance, while should also
Possesses the environmental-friendly advantage such as low with cost, however, current anode material for lithium-ion batteries can't meet electricity well
Requirement of the electrical automobile to high rate performance, security performance and cycle performance.
The anode material for lithium-ion batteries reported at present can't meet the above-mentioned high request to lithium ion battery well,
Volumetric properties and cycle performance are the key indexes for evaluating cell positive material quality in above-mentioned requirements, in current research,
The two indexs are often difficult to meet at the same time, therefore find and meeting the lithium ion battery for the cycle performance that high power capacity is become reconciled just at the same time
Pole material becomes the main target of each researcher.At present, tertiary cathode material, particularly nickelic ternary material are excellent due to its cost
Gesture and electrical property feature are increasingly becoming research hotspot.However as the increase of nickel content, the stability of material in the electrolytic solution is got over
Difference, the cycle performance of prepared battery are poorer.Meanwhile higher residual alkali is unfavorable for the processing of battery material.In order to improve these
Problem, is doped material and coating modification is effective method.Wherein, surface cladding is common modified method, research
It was found that clad can alleviate corrosion of the electrolyte to positive electrode as protective layer, suppress structure collapses, significantly improve ternary material
The cyclical stability and heat endurance of material.By select different covering materials realize tertiary cathode material heat endurance, times
Rate performance and stable circulation performance are obviously improved.The covering material of common ternary material has carbon material, oxide, fluorination
Thing, phosphate, lithiumation thing and polymer etc. (Zhou P F, Zhang Z, Meng H J, et al.Nanoscale, 2016,8,
19263-19269).But current most covering material is lithium " insulator ", and the lithium ion of material passes usually under big multiplying power
Defeated speed and its stability are poor, cause its high rate performance poor, while material cladding inhomogeneity significantly affects the electrical property of material
Play.
The content of the invention
In view of the above problems, it is an object of the invention to provide the lithium that a kind of nitrogen-doped graphene and lithium molybdate coat altogether from
Sub- tertiary cathode material and preparation method thereof, it is intended to which the processing performance and discharge and recharge for solving existing cobalt nickel lithium manganate ternary material are followed
The not bery preferable technical problem of ring, high rate performance.
On the one hand, the anode material of lithium battery preparation method of the nitrogen-doped graphene and lithium molybdate comprises the following steps：
1) graphite oxide, nitrogen source are dispersed in water to form dispersion liquid, add ascorbic acid and heat to obtain gel；
2) take molybdenum source, lithium electricity ternary material to add stirring in the gel to be evaporated to obtain mixed material；
3) mixed material is calcined in inert atmosphere, obtains nitrogen-doped graphene after cooling and lithium molybdate coats altogether
Anode material of lithium battery
Further, in step 1), graphite oxide additive amount is the 0.1%~5% of anode material of lithium battery quality, described
The concentration of dispersion liquid is 0.1~5mg/mL, and the nitrogen source is urea or thiocarbamide.
Further, in step 1), the heating-up temperature that heating obtains gel is 50~100 DEG C, heating time for 0.5~
10h。
Further, in step 2), the additive amount of molybdenum element is 500~3000ppm.
Further, in step 2), stirring evaporated temperature is 80~100 DEG C, and the time is 0.5~2h.
Further, in step 3), inert gas is argon gas or the gaseous mixture of argon gas and hydrogen, calcining heat for 500~
900 DEG C, the time is 3~12h.
On the other hand, the anode material of lithium battery of the nitrogen-doped graphene and lithium molybdate is prepared by the above method,
Its kernel is lithium electricity ternary material, and outer layer loads the compound coating layer of lithium molybdate for nitrogen-doped graphene conductive network.
Further, the lithium electricity ternary material is one kind in NCM523, NCM622, NCM811.
The beneficial effects of the invention are as follows：The present invention is dispersed in cathode in cladding process using Graphene gel and molybdenum source
Material surface, realizes that nitrogen-doped graphene and lithium molybdate generate at the same time in inert atmosphere；One side of formation of nitrogen-doped graphene
Face forms conductive network on positive electrode surface, and N doping is conducive to electric transmission, and special network structure is conducive to discharge and recharge
The transmission of lithium ion and electrolyte in cyclic process, greatly improves the transmission rate of lithium ion, Vitamin C needed for Graphene gel
The addition of acid helps to reduce part residual alkali, and molybdenum source also contributes to reduce residual alkali with the reaction of surface residual alkali, improves the processing of material
Performance.In addition, lithium molybdate lithium ion conductor clad helps to improve the transmission performance of lithium ion, therefore obtain just
Pole material electrochemical performance is greatly improved, and cyclical stability and high rate performance all make moderate progress.
Brief description of the drawings
Fig. 1 is embodiment one and the circulation figure of the tertiary cathode material of comparative example one.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.
The anode material of lithium battery preparation method of nitrogen-doped graphene and lithium molybdate provided by the invention comprises the following steps：
1) graphite oxide, nitrogen source are dispersed in water to form dispersion liquid, add ascorbic acid and heat to obtain gel.
In final obtained anode material of lithium battery of the invention, the additive amount of nitrogen-doped graphene is calculated with graphite oxide,
Graphite oxide additive amount is the 0.1%~5% of anode material of lithium battery quality, and the graphite oxide and nitrogen source are dispersed in water
The concentration of the dispersion liquid arrived is 0.1~5mg/mL, and the nitrogen source is urea or thiocarbamide.
2) take molybdenum source, lithium electricity ternary material to add stirring in the gel to be evaporated to obtain mixed material.
The molybdenum source is molybdenum trioxide, and wherein the additive amount of molybdenum element is 500~3000ppm, i.e., contains by quality than molybdenum member
Element accounts for the 3000/500/1000000ths~million of lithium electricity ternary material, i.e., and 30/5ths to ten thousand/10000ths.The lithium electricity ternary
Material is one kind in NCM523, NCM622, NCM811.It is 80~100 DEG C to stir evaporated temperature, and the time is 0.5~2h.
3) mixed material is calcined in inert atmosphere, obtains nitrogen-doped graphene after cooling and lithium molybdate coats altogether
Anode material of lithium battery.
Inert gas is argon gas or the gaseous mixture of argon gas and hydrogen, and calcining heat is 500~900 DEG C, and the time is 3~12h.
The anode material of lithium battery kernel finally obtained is lithium electricity ternary material, and outer layer is nitrogen-doped graphene conductive network
Load the compound coating layer of lithium molybdate.Wherein on the one hand nitrogen-doped graphene forms conductive network on positive electrode surface, and nitrogen is mixed
Miscellaneous to be conducive to electric transmission, special network structure is conducive to the transmission of lithium ion and electrolyte during charge and discharge cycles, greatly
The big transmission rate for improving lithium ion, the addition of ascorbic acid needed for Graphene gel help to reduce part residual alkali, molybdenum source with
Surface residual alkali reaction also contributes to reduce residual alkali, improves the processing performance of material.In addition, lithium molybdate lithium ion conductor clad
Help to improve the transmission performance of lithium ion, therefore obtained positive electrode chemical property is greatly improved, circulation
Stability and high rate performance all make moderate progress.
Illustrated below by specific embodiment and comparative example.
Embodiment one：
200mg graphite oxides, 2g urea are added in 100mL water and form dispersion liquid, addition 0.75g ascorbic acid, 90
DEG C stirring 1.5h forms semigel shape, then adds 40mg molybdenum trioxides and 20g NCM622 positive electrodes thereto, then exists
Dry 2h is stirred at 80 DEG C.Dry material is transferred to 600 DEG C of heat treatment 5h, cooling in argon gas atmosphere Muffle furnace to acquire nitrogen and mix
The anode material of lithium battery that miscellaneous graphene and lithium molybdate coat altogether.
Embodiment two：
500mg graphite oxides, 4g urea are added in 100mL water and form dispersion liquid, addition 1.5g ascorbic acid, 80 DEG C
Stir 2h and form semigel shape, 1.0g molybdenum trioxides and 500gNCM622 positive electrodes are then added thereto, then at 70 DEG C
The lower dry 5h of stirring.Dry material is transferred to 700 DEG C of heat treatment 5h in argon gas atmosphere Muffle furnace, N doping is acquired after cooling
The anode material of lithium battery that graphene and lithium molybdate coat altogether.
Embodiment three：
400mg graphite oxides, 4g urea are added in 100mL water and form dispersion liquid, addition 1.5g ascorbic acid, 100
DEG C stirring 1h forms semigel shape, 0.4g molybdenum trioxides and 200g NCM622 positive electrodes is then added thereto, then 80
Dry 2h is stirred at DEG C.Dry material is transferred to 550 DEG C of heat treatment 6h in argon gas atmosphere Muffle furnace, nitrogen is acquired after cooling and mixes
The anode material of lithium battery that miscellaneous graphene and lithium molybdate coat altogether.
Comparative example one：
Take the nickel-cobalt-manganternary ternary anode material NCM622 of uncoated nitrogen-doped graphene and lithium molybdate.
Electrochemical property test is carried out to resulting materials by the following method：
For the ternary material synthesized respectively using embodiment one and comparative example one as positive active material, lithium piece is anode, assembling
Into button cell.The composition of positive plate is m (active material)：M (acetylene black)：M (PVDF)=80:12:8, using blue electrical testing
System is tested, and charging/discharging voltage is 2.75~4.3V, and charge-discharge magnification 1.0C, carries out cycle performance under normal temperature environment
Test.
The cycle-index under the voltage of 2.75~4.3V is kept embodiment one with capacity with the material prepared by comparative example one
The relation of rate is as shown in Figure 1.
After 50 cycle charge-discharges, nitrogen-doped graphene and lithium molybdate coat ternary material capacity retention ratio and are altogether
97.8%, undoped tertiary cathode material capacity retention ratio is 94.6%.According to test result and diagrammatically shown curve, sheet
Embodiment anode material of lithium battery is compared to the nickel-cobalt-manganternary ternary anode material of uncoated nitrogen-doped graphene and lithium molybdate, charge and discharge
Electric cycle performance is obviously improved.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (8)
- A kind of 1. anode material of lithium battery preparation method of nitrogen-doped graphene and lithium molybdate, it is characterised in that the method bag Include following step：1) graphite oxide, nitrogen source are dispersed in water to form dispersion liquid, add ascorbic acid and heat to obtain gel；2) take molybdenum source, lithium electricity ternary material to add stirring in the gel to be evaporated to obtain mixed material；3) mixed material is calcined in inert atmosphere, the lithium that nitrogen-doped graphene and lithium molybdate coat altogether is obtained after cooling Cell positive material.
- 2. the anode material of lithium battery preparation method of nitrogen-doped graphene as claimed in claim 1 and lithium molybdate, it is characterised in that In step 1), graphite oxide additive amount is the 0.1%~5% of anode material of lithium battery quality, graphite oxide in the dispersion liquid Concentration be 0.1~5mg/mL, the nitrogen source is urea or thiocarbamide.
- 3. the anode material of lithium battery preparation method of nitrogen-doped graphene as claimed in claim 1 and lithium molybdate, it is characterised in that In step 1), the heating-up temperature that heating obtains gel is 50~100 DEG C, and heating time is 0.5~10h.
- 4. the anode material of lithium battery preparation method of nitrogen-doped graphene as claimed in claim 1 and lithium molybdate, it is characterised in that In step 2), the additive amount of molybdenum element is 500~3000ppm.
- 5. the anode material of lithium battery preparation method of nitrogen-doped graphene as claimed in claim 1 and lithium molybdate, it is characterised in that In step 2), stirring evaporated temperature is 80~100 DEG C, and the time is 0.5~2h.
- 6. the anode material of lithium battery preparation method of nitrogen-doped graphene as claimed in claim 1 and lithium molybdate, it is characterised in that In step 3), inert gas is argon gas or the gaseous mixture of argon gas and hydrogen, and calcining heat is 500~900 DEG C, the time for 3~ 12h。
- A kind of 7. anode material of lithium battery of nitrogen-doped graphene and lithium molybdate, it is characterised in that the anode material of lithium battery It is prepared by such as any one of claim 1-6 the methods, its kernel is lithium electricity ternary material, and outer layer is nitrogen-doped graphene Conductive network loads the compound coating layer of lithium molybdate.
- 8. anode material for lithium-ion batteries as claimed in claim 7, it is characterised in that the lithium electricity ternary material for NCM523, One kind in NCM622, NCM811.
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| CN115528228A (en) * | 2022-09-28 | 2022-12-27 | 安徽博石高科新材料股份有限公司 | Lithium molybdate coated modified lithium manganate material and preparation method and application thereof |
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Application publication date: 20180424 |