CN107293742A - A kind of preparation method of the electric positive electrode of the lithium of stratiform monoclinic phase-Spinel integrated morphology - Google Patents
A kind of preparation method of the electric positive electrode of the lithium of stratiform monoclinic phase-Spinel integrated morphology Download PDFInfo
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- CN107293742A CN107293742A CN201710614159.6A CN201710614159A CN107293742A CN 107293742 A CN107293742 A CN 107293742A CN 201710614159 A CN201710614159 A CN 201710614159A CN 107293742 A CN107293742 A CN 107293742A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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 belongs to inorganic material and technical field of energy material, there is provided a kind of method of simple anode material for lithium-ion batteries of the synthesis with multiphase integrated morphology.Synthesis has the rich lithium material of the manganese base of stratiform monocline phase structure first；The rich lithium material of the above-mentioned manganese base with stratiform monocline phase structure is deployed into rheology phase system with reducing agent；By the rheology phase system of gained under reducing atmosphere or inert atmosphere low-temperature heat a few hours, by the material clean after heating, drying, that is, obtain the material with Spinel and stratiform monoclinic phase integrated morphology.When the material of this multiphase integrated morphology is used as anode material for lithium-ion batteries, it is provided simultaneously with the premium properties of a variety of phase structure materials so that the active material has high working voltage, height ratio capacity, high charge-discharge efficiencies, excellent high rate capability and cycle performance simultaneously.This preparation method is simple, and required synthesis temperature is low, and product pattern is easy to regulation and control, can be readily available various special nanostructureds, and suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation side of the electric positive electrode of lithium with Spinel and stratiform monoclinic phase integrated morphology
Method, belongs to inorganic material and technical field of energy material.
Background technology
To meet the great demand of removable new energy, inexpensive, the environment-friendly secondary electricity of excellent performance, safety is developed
Pond has caused extensive concern.Most of current driving force type anode material for lithium-ion batteries is to use LiFePO4 and ternary material.
LiFePO4 is inexpensive safely, environment-friendly, but its specific capacity is low, and high rate capability is poor, and operating voltage is not high；Ternary material ratio
Capacity is of a relatively high, but due to containing elements such as cobalt, nickel, making its expensive, security poor, and job insecurity.Manganese base is rich
Lithium material xLi2MnO3·(1-x)LiMO2(0≤x≤1, M=CoyNizMn1-y-z, the operating voltage of 0≤y≤1,0≤z≤1) is high,
Specific capacity height is that a class has the electric positive electrode of the lithium of development potentiality very much.Li particularly in the rich lithium material of manganese base2MnO3(i.e.
xLi2MnO3·(1-x)LiMO2(x=1)), its theoretical specific capacity is up to 458mAh/g, and required transition metal manganese is a kind of
Rich content, cheap metal.But Li2MnO3Also there is its weak point：Its high rate capability and cycle performance are poor.It is another
The electric positive electrode of lithium that kind is based entirely on manganese is LiMn2O4 (LiMn2O4), its chemical property and Li2MnO3Contrast, it is followed
Ring performance is stable, high rate capability is excellent, but its specific capacity in conventional voltage range is relatively low.The electrification of lithium electricity positive electrode
It is all by its structures shape to learn performance.Manganese base richness lithium material is stratiform monocline phase structure, and LiMn2O4 is Spinel structure.Tool
The positive electrode of the layer structure of the standby rich lithium material of manganese base and the integrated morphology of the spinel structure of LiMn2O4, then be provided simultaneously with work
Make that voltage is high, specific capacity is big, high rate capability is good, good cycling stability the features such as.By the positive electrode system of this integrated morphology
Into lithium ion battery be pure electric automobile (EV) or hybrid vehicle (HEV), mobile phone, laptop computer, portable shooting
The excellent power source of machine etc..
Co-precipitation-high temperature is used mostly at present with Spinel and the electric positive electrode of the lithium of stratiform monoclinic phase integrated morphology
Solid phase synthesis, i.e., obtain manganese source (generally carbonate or hydroxide containing manganese) and lithium source first by Co deposited synthesis
(generally lithium carbonate or lithium hydroxide), then using high temperature solid-state method by manganese source and lithium source at high temperature in air atmosphere plus
Heat.(such as Electrochemistry Communications, 2007,9,262-268；Chemistry of Materials,
2012,24,600-612 etc. uses this synthetic method.) in addition, there is considerably less collosol and gel synthetic method.This synthesis
Method has two kinds of different ways, and a kind of is the material for synthesizing first stratiform monocline phase structure, is then using colloidal sol
Stratiform monocline material is added in the sol system during the material of gel method synthetic spinel phase structure, most
Sol-gel system is heated at high temperature in air atmosphere afterwards.(such as Phys.Chem.Chem.Phys., 2015,17,1257-
1264.) another is that each source material directly is deployed into sol-gel system, then by sol gel precursor in air atmosphere
System's high-temperature heating.(such as ChemElectroChem, 2015,2,1821-1829.) above-mentioned several synthetic methods have some common
Shortcoming：One be will more than 750 DEG C at a high temperature of in air or oxygen long-time heating, two be synthesis final product one
As be micron-sized particle, it is difficult to obtain nanosized, have the product of special pattern, so as to be unfavorable for positive pole material needed for improving
The chemical property of material.
The content of the invention
Problem to be solved by this invention be to provide a kind of lithium with stratiform monoclinic phase and Spinel integrated morphology from
The preparation method of sub- cell positive material.Synthesis temperature needed for the preparation method is low, can synthesize it is various needed for sizes and
The material of pattern, can obtain various nanosizeds, the positive electrode of special appearance, so as to obtain being provided simultaneously with work electricity
Pressure is high, specific capacity is big, high rate capability is good, the electric positive electrode of good cycling stability lithium.
The technical scheme that the present invention is provided is：
Synthesize the rich lithium material of the manganese base with stratiform monocline phase structure using various synthetic methods；
The rich lithium material of the above-mentioned manganese base with stratiform monocline phase structure is mixed with reducing agent, dripped into mixed powder
Solubilizer, rheology phase system is deployed into by mixture；
By the rheology phase system of gained under reducing atmosphere or inert atmosphere low-temperature heat a few hours；
By the powder cleaning after heating, dry.
As a preferred embodiment,
In such scheme, the rich lithium material of the manganese base with stratiform monocline phase structure is xLi2MnO3·(1-x)LiMO2
(0<X≤1, M=CoyNizMn1-y-z, 0≤y≤1,0≤z≤1), including special case Li2MnO3, i.e. xLi2MnO3·(1-x)
LiMO2(x=1).
The reducing agent has graphite, activated carbon, CNT, graphene, polyethylene glycol or stearic acid.
It is described be deployed into rheology phase system needed for solvent have water, ethanol or acetone.
The low temperature is 300-500 DEG C.
The a few hours are 3-24 hours.
The beneficial effects of the invention are as follows：
1. it is readily synthesized out various nanosizeds, with special appearance, with stratiform monoclinic phase and the integrated knot of Spinel
The positive electrode of structure.
2. the positive electrode of the integrated phase structure of tool synthesized is provided simultaneously with the operating voltage of Spinel lithium manganate material
High, high rate capability is good, good cycling stability advantage and possess stratiform monocline phase structure rich lithium material specific capacity it is big
Advantage.
3. synthesis temperature is low, the heat time is short.
4. synthetic method is very simple, synthesis condition is easily-controllable, suitable for scale industrial production.
Brief description of the drawings
Stratiform-spinelle integrated morphology positive electrode 0.1LiMn of the gained of Fig. 1 embodiments 12O4·0.9Li2MnO3Nanometer
ESEM (SEM) figure of rod.
Stratiform-spinelle integrated morphology positive electrode 0.1LiMn of the gained of Fig. 2 embodiments 12O4·0.9Li2MnO3Nanometer
High magnification transmission electron microscope (TEM) figure of rod, the Fourier transformation (FFT) and its index calibrating of high magnification transmission electron microscope.
Stratiform-spinelle integrated morphology positive electrode 0.1LiMn of the gained of Fig. 3 embodiments 12O4·0.9Li2MnO3Nanometer
Rod is assembled into the constant current charge-discharge curve of simulated battery as positive electrode active materials.L-Li in figure2MnO3To introduce Spinel knot
Parent material before structure, SL-Li2MnO3To introduce the integrated phase structure material of stratiform-spinelle after Spinel structure.
Stratiform-spinelle integrated morphology positive electrode 0.1LiMn of the gained of Fig. 4 embodiments 12O4·0.9Li2MnO3Nanometer
Rod is assembled into the cycle performance of simulated battery as positive electrode active materials.L-Li in figure2MnO3To introduce before Spinel structure
Parent material, SL-Li2MnO3To introduce the integrated phase structure material of stratiform-spinelle after Spinel structure.
Stratiform-spinelle integrated morphology positive electrode 0.1LiMn of the gained of Fig. 5 embodiments 12O4·0.9Li2MnO3Nanometer
Rod is assembled into the high rate capability of simulated battery as positive electrode active materials.L-Li in figure2MnO3For introduce Spinel structure it
Preceding parent material, SL-Li2MnO3To introduce the integrated phase structure material of stratiform-spinelle after Spinel structure.
Stratiform-spinelle integrated morphology positive electrode 0.2LiMn of the gained of Fig. 6 embodiments 22O4·0.8Li2MnO3Nanometer
Transmission electron microscope (TEM) figure of band.
Stratiform-spinelle integrated morphology positive electrode 0.2LiMn of the gained of Fig. 7 embodiments 22O4·0.8Li2MnO3Nanometer
High magnification transmission electron microscope (TEM) figure of band.
Embodiment
There is Spinel the invention discloses a kind of introduced in the rich lithium material of the manganese base of stratiform monocline phase structure
Structure, obtains the preparation method of the electric positive electrode of the lithium with the integrated phase structure of stratiform-spinelle, is specially：
Synthesize the rich lithium material of the manganese base with stratiform monocline phase structure first；
The rich lithium material of the above-mentioned manganese base with stratiform monocline phase structure is mixed with reducing agent, dripped into mixed powder
Solubilizer, rheology phase system is deployed into by mixture；
By the rheology phase system of gained under reducing atmosphere or inert atmosphere low-temperature heat a few hours；
By the powder cleaning after heating, dry.
Below by embodiment, the present invention is furture elucidated.
Embodiment 1
Synthesis flow is as follows：
α-MnO are obtained using hydrothermal synthesis method2Nano wire：By 4 mMs of MnSO4·H2O and 6 mM of KMnO4It is molten successively
In 60 milliliters of distilled water.By 2 milliliters of H2SO4(60%) above-mentioned solution is added, is stirred 30 minutes.The solution prepared is transferred to 100
Milliliter autoclave, is heated 12 hours in 120 DEG C.By the precipitation obtained cleaning, dry.
With α-MnO2Nano wire is manganese source, and the Li with stratiform monocline phase structure is obtained using rheological phase reaction method2MnO3Receive
Rice rod：By α-MnO2Nano wire, LiOHH2O and appropriate water mixing, grinding, are deployed into rheology phase system.Afterwards by the rheology
Phase system is heated 5 hours in 600 DEG C in air atmosphere.After Temperature fall, that is, obtain Li2MnO3Nanometer rods.
In the Li of stratiform monocline phase structure2MnO3The LiMn of Spinel structure is introduced in nanometer rods2O4Synthetic method such as
Under：Take 11.7g Li2MnO3Nanometer rods, 5.0g polyethylene glycol and appropriate water mixing, grinding, are deployed into rheology phase system.Should
Rheology phase system is transferred to tube furnace, is heated 4 hours in 350 DEG C in argon atmosphere.It is cooled to obtained powder after room temperature
Clean, dry.Then heat 4 hours, be cooled to obtained powder cleaning, drying after room temperature in 350 DEG C in argon atmosphere.
The product that above-mentioned synthetic method is obtained is characterized with XRD, it was demonstrated that product has Li2MnO3(layer structure) and
LiMn2O4(spinel structure)；Characterized with SEM and TEM, it was demonstrated that the nanosized and pattern that product maintains monodimension nano stick are (attached
Fig. 1).Characterized with high magnification TEM, it was demonstrated that product has stratiform-spinelle integrated morphology, its Selected area electron electronic diffraction and high power
Rate TEM Fourier transformation (accompanying drawing 2) all shows that product has stratiform-spinelle integrated morphology.Use inductively coupled plasma
The molecular formula that body atomic emission spectrum (ICP-AES) analysis obtains material should be 0.1LiMn2O4·0.9Li2MnO3.Gained
0.1LiMn2O4·0.9Li2MnO3Material is used as positive-active material
Material is assembled into simulated battery, and electrochemical property test is carried out in new prestige (Shenzhen) high accuracy battery test system.
When under current density is 20mA/g in constant current charge-discharge in 2.0-4.8 voltage ranges, its first charge-discharge curve such as accompanying drawing 3,
Li is shown in initial charge curve simultaneously2MnO3Electrochemical activation platform (~4.5V) and LiMn2O4Charge and discharge platform
(~4.1V and~4.2V), not only testimonial material has two phase structures, and the material of this tool integrated morphology simultaneously again
The specific capacity of material, cycle efficieny, coulombic efficiency, high rate capability ratio introduce LiMn2O4Parent material Li before2MnO3It is better
Many (see accompanying drawing 4 and accompanying drawings 5).
Embodiment 2
Synthesis flow is as follows：
Na is synthesized using lava method0.44MnO2Nanobelt：By 1mmol MnCO3、0.23mmol Na2CO3It is mixed with 5g NaCl
Close, grind, mixture is transferred to alumina crucible afterwards, heated 5 hours at 850 DEG C in air.Finally by products therefrom
Cleaning for several times, dry.
With Na0.44MnO2Nanobelt is manganese source, and the Li of stratiform monocline phase structure is obtained using ion-exchange2MnO3Nanometer
Band：By 2mmol Na0.44MnO2With 10g LiNO3+LiCl(LiNO3:LiCl=0.88:0.12) mix, grind, afterwards will be mixed
Compound is transferred to alumina crucible, is heated 1 hour at 500 DEG C in air.Finally by products therefrom cleaning for several times, dry.
In the Li of stratiform monocline phase structure2MnO3The LiMn of Spinel structure is introduced in nanobelt2O4Synthetic method such as
Under：Take 10.0g Li2MnO3Nanobelt, 3.0g stearic acid and appropriate ethanol mixing, grinding, are deployed into rheology phase system.Should
Rheology phase system is transferred to tube furnace, is heated 3 hours in 400 DEG C in argon atmosphere.It is cooled to obtained powder after room temperature
Clean, dry.Then heat 5 hours, be cooled to obtained powder cleaning, drying after room temperature in 450 DEG C in argon atmosphere.
The product that above-mentioned synthetic method is obtained is characterized with XRD, it was demonstrated that product has Li2MnO3(layer structure) and
LiMn2O4(spinel structure)；Characterized with SEM and TEM, it was demonstrated that product maintains the size and pattern (accompanying drawing of 1-dimention nano band
6).Characterized with high magnification TEM, it was demonstrated that product has stratiform-spinelle integrated morphology, its Selected area electron electronic diffraction (accompanying drawing 7)
All show that product has stratiform-spinelle integrated morphology.Use inductively coupled plasma atomic emission spectrum (ICP-AES) point
The molecular formula that analysis obtains material should be 0.2LiMn2O4·0.8Li2MnO3。
Embodiment 3
Synthesis flow is as follows：
The Li for having stratiform monocline phase structure is obtained using coprecipitation1.2Mn0.54Ni0.13Co0.13O2(it can also be written as
0.5Li2MnO3·0.5LiCo1/3Ni1/3Mn1/3O2) nano particle：0.25mol/L is prepared by Mn (CH3COO)2、Co(CH3COO)2
With Ni (CH3COO)2(wherein Mn, Co, Ni mol ratio are 0.54 to the mixed solution of composition:0.13:
0.13).Under continuous stirring, above-mentioned solution is added drop-wise in 0.5mol/L LiOH solution.Then will be mixed
Alkaline solution water-bath at 60 DEG C is co-precipitated for 6 hours.Finally, by coprecipitated product and LiOHH2O is according to mol ratio
Mixing, in being heated 10 hours at 900 DEG C in air atmosphere, cleans after cooling, dries, that is, obtain having stratiform monocline phase structure
Li1.2Mn0.54Ni0.13Co0.13O2Nano particle.
In the Li of stratiform monocline phase structure1.2Mn0.54Ni0.13Co0.13O2Spinel structure is introduced in nano particle
LiMn2O4Synthetic method it is as follows：Take 10.0g Li1.2Mn0.54Ni0.13Co0.13O2Nano particle, 5.0g activated carbons and appropriate
Water mixing, grinding, are deployed into rheology phase system.The rheology phase system is transferred to tube furnace, added in argon atmosphere in 300 DEG C
Heat 4 hours.It is cooled to obtained powder cleaning, drying after room temperature.Then heated 4 hours in 400 DEG C in argon atmosphere, it is cold
But to after room temperature by obtained powder cleaning, drying.
Above-described embodiment illustrates that this synthetic method is applied to the rich lithium material of all manganese bases with stratiform monocline phase structure,
Including Li2MnO3、xLi2MnO3·(1-x)LiMO2(0<X≤1, M=CoyNizMn1-y-z,0≤y≤1,0≤z≤1).Synthesis side
Different types of reducing agent can be used in method, the temperature used during introducing Spinel structure is low, and required time is short.
Claims (6)
1. a kind of synthetic method of the anode material for lithium-ion batteries with stratiform monoclinic phase and Spinel integrated morphology, it is special
Levy and be：
The rich lithium material of manganese base of the synthesis with stratiform monocline phase structure；
The rich lithium material of the above-mentioned manganese base with stratiform monocline phase structure is mixed with reducing agent, is added dropwise into mixed powder molten
Agent, rheology phase system is deployed into by mixture；
By the rheology phase system of gained under reducing atmosphere or inert atmosphere low-temperature heat a few hours；
By the powder cleaning after heating, dry.
2. preparation method as claimed in claim 1, it is characterised in that：The rich lithium material of manganese base with stratiform monocline phase structure
Expect for xLi2MnO3·(1-x)LiMO2(0<X≤1, M=CoyNizMn1-y-z, 0≤y≤1,0≤z≤1), including special case
Li2MnO3, i.e. xLi2MnO3·(1-x)LiMO2(x=1).
3. preparation method as claimed in claim 1 or 2, it is characterised in that：The reducing agent includes common inorganic and organic
Reducing agent, common inorganic reducing agent includes graphite, activated carbon, CNT, graphene etc., and the machine reducing agent of common are includes
Polyethylene glycol, stearic acid etc..
4. preparation method as claimed in claim 1 or 2, it is characterised in that：It is described that mixture is deployed into rheology phase system institute
The solvent needed includes the common solvents such as water, ethanol, acetone.
5. preparation method as claimed in claim 1 or 2, it is characterised in that：The low temperature is 300-500 DEG C.
6. preparation method as claimed in claim 1 or 2, it is characterised in that：The a few hours are 3-24 hours.
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| CN108264090A (en) * | 2018-01-18 | 2018-07-10 | 林立（武汉）新能源科技有限公司 | A kind of non-electrochemical activates Li2MnO3Method |
| CN109904402A (en) * | 2017-12-11 | 2019-06-18 | 中国科学院大连化学物理研究所 | A kind of lithium-rich manganese base material and its preparation and application |
| CN113443653A (en) * | 2021-06-29 | 2021-09-28 | 哈尔滨工业大学 | Ball milling-heat treatment activation method for lithium dimanganese oxide three-positive electrode material |
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| CN107994226A (en) * | 2017-12-14 | 2018-05-04 | 桑顿新能源科技有限公司 | A kind of lithium-rich anode material of Mn adulterated lithium manganate and preparation method thereof |
| CN108264090A (en) * | 2018-01-18 | 2018-07-10 | 林立（武汉）新能源科技有限公司 | A kind of non-electrochemical activates Li2MnO3Method |
| CN113443653A (en) * | 2021-06-29 | 2021-09-28 | 哈尔滨工业大学 | Ball milling-heat treatment activation method for lithium dimanganese oxide three-positive electrode material |
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Application publication date: 20171024 |