CN106784657A - A kind of method that sodium and iron codope prepare High-performance lithium manganate anode material - Google Patents

A kind of method that sodium and iron codope prepare High-performance lithium manganate anode material Download PDF

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Publication number
CN106784657A
CN106784657A CN201611075105.9A CN201611075105A CN106784657A CN 106784657 A CN106784657 A CN 106784657A CN 201611075105 A CN201611075105 A CN 201611075105A CN 106784657 A CN106784657 A CN 106784657A
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sodium
source
lithium
iron
manganese
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李超
肖顺华
占涛涛
林刚
罗晓冬
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Guilin University of Technology
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Guilin University of Technology
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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
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
    • 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

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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of method that sodium and iron codope prepare High-performance lithium manganate anode material.（1）Manganese source and strong oxidizer are dissolved in distilled water, are fully transferred in reactor after dissolving, then reactor is placed in baking oven, reaction obtains MnO2Powder；（2）Manganese dioxide, lithium source, sodium source and source of iron are fully ground and obtain black mixture；（3）Mixture is carried out into first time high temperature sintering in Muffle furnace, room temperature is cooled to the furnace, after grinding after carry out the sintering of higher temperature, be naturally cooling to room temperature, that is, obtain LiNaxMn2‑yFeyO4, wherein：X=0.01 ~ 0.2, y=0.01 ~ 0.2.The present invention can prepare that particle is tiny, the composite mixed manganate cathode material for lithium of even closer sodium, iron is contacted between excellent in crystallinity and crystal grain, and the high rate performance and cycle performance of material are greatly improved.

Description

A kind of method that sodium and iron codope prepare High-performance lithium manganate anode material
Technical field
The present invention relates to a kind of composite mixed method for preparing high performance manganate cathode material for lithium of sodium and iron.
Background technology
At present, lithium ion battery turns into the main power source of notebook computer, smart mobile phone and digital camera, as research Focus.Compared with lead-acid battery and Ni-MH battery, lithium ion battery has that operating voltage is high, energy density is higher, cycle life The advantages such as length, memory-less effect.LiCoO2The positive electrode of research earliest in lithium ion battery, but its security it is poor, to ring Border has pollutes and expensive.The more anode material for lithium-ion batteries of recent research has LiNiO2、LiMn2O4And LiFePO4 Deng, wherein spinel lithium manganate with its low cost, environmental protection, good security the advantages of be considered as most being hopeful that cobalt acid lithium can be substituted simultaneously Commercialized positive electrode, but dissolving, the decomposition of electrolyte, Jahn-Teller effects due to manganese in the electrolytic solution are realized, Its capacity attenuation is serious in charge and discharge process.
Currently in order to solving the capacity fade problem of spinel lithium manganate, research is concentrated mainly on these aspects：Improve and close Into method, adulterate and Surface coating.Cation doping refers to introduce some transition elements or rare earth element.As Fe, Al, Mg, Cu, Zn, Ni, Cr and Co etc..Na+Introducing instead of the part Li of tetrahedron 8a positions+, inverse spinel structure is formd, reduce Li in charge and discharge process+Deintercalation repeatedly reduces charge and discharge process so as to the structure destruction for causing Lattice Contraction and expansion to bring The dissolving of middle manganese, improves the portion capacity of material.After Fe is introduced, Fe3+Instead of part Mn3+, cause the damage of certain capacity Lose, but due to the raising of manganese element average valence, it is suppressed that the dissolving of manganese and Jahn-Teller effects, the crystal structure of material More stablize, cycle performance is improved.
The present invention is first using hydro-thermal method synthesis nanometer acanthosphere shape MnO2, thorn surface with rounded structures product more greatly, can be with lithium Source and doped source are fully contacted, and promote final product to have spherical morphology, and spherical structure can aid in raising LiMn2O4 material The tap density and energy density of material, so as to improve its chemical property.
The content of the invention
The present invention seeks to stablize the crystal structure of lithium manganate material, suppress on the basis of Jahn-Teller effects, make It is standby go out capacity be not susceptible to the excellent manganate cathode material for lithium of decay, high rate performance.
Concretely comprise the following steps：
（1）0.01 ~ 0.2 mol manganese sources and 0.01 ~ 0.2 mol strong oxidizers are stoichiometrically weighed, both are placed in beaker In, the deionized water of 40 ~ 200 mL is subsequently adding, at ambient temperature will with DF-101S type heat collecting types constant temperature blender with magnetic force Strong oxidizer and manganese source are thoroughly mixed, and then mixed liquor is transferred in the polytetrafluoroethyllining lining of 50 ~ 300 mL, then will Polytetrafluoroethyllining lining is sealed in stainless steel cauldron, and under the conditions of the temperature for setting is as 100 ~ 200 DEG C, insulation 8 ~ 24 is small When, room temperature is naturally cooled to, filter, dried 18 ~ 48 hours under the conditions of 60 ~ 120 DEG C, obtain manganese source presoma black powder.
（2）0.001 ~ 0.2 mol steps are weighed according to mol ratio（1）Resulting manganese source presoma, 0.001-0.2 mol lithiums The source of iron in source, the sodium source of 0.0001 ~ 0.1 mol doping and 0.0001 ~ 0.1 mol doping, is placed in four in beaker and adds The absolute ethyl alcohol of 40-100 mL, is put into the drying under conditions of 60 ~ 120 DEG C in baking oven, then after ultrasonic vibration 20-60 minutes Ground 10 ~ 120 minutes in mortar respectively.
（3）By step（2）After gains grinding, be placed in Muffle furnace 250 ~ 650 DEG C of pre-sintering 2-10 hours, it is pre-sintered after Be ground and in Muffle furnace 650 ~ 850 DEG C calcine 10 ~ 30 hours, cool to room temperature with the furnace, obtain final product sodium and iron codope Manganate cathode material for lithium LiNaxMn2-yFeyO4, wherein：X=0.01 ~ 0.2, y=0.01 ~ 0.2.
The strong oxidizer be ammonium persulfate, potassium hyperchlorate, potassium permanganate, analyze in pure hydrogen peroxide and sodium peroxydisulfate one Plant or various.
The manganese source is one or more in manganese acetate, Manganous sulfate monohydrate and manganese carbonate.
The lithium source is one or more in lithium acetate, a hydronium(ion) lithia and lithium carbonate.
The source of iron of the doping is one or more in iron hydroxide, iron oxide, ferrous oxide and ferroso-ferric oxide.
The sodium source of described doping is one or more in sodium acetate, sodium carbonate and NaOH.
The present invention prepares nanometer thorn spherical manganese dioxide using the simple hydro-thermal method of operation, add lithium source and sodium contaminated, Ferro element, then by controlling time and the temperature of sintering, prepare that particle is tiny, crystallinity is high, the regular homogeneous sodium of pattern, iron The composite mixed positive electrode of ion.The chemical property of material is significantly improved by sodium, iron ion codope, makes its capacity Decay is inhibited and under big multiplying power still with larger specific discharge capacity.When voltage range is 3.0 ~ 4.4 V, LiNaxMn4-yFeyO4Material under 0.2 C multiplying powers first discharge specific capacity up to 128.22 mAh/g；Followed under 0.5 C multiplying powers After ring 100 is enclosed, specific discharge capacity conservation rate is 92.13%, with excellent cyclical stability；In 10 C multiplying powers, material is put Electric specific capacity can reach 60.79 mAh/g.From difference sweep speed under CV figures as can be seen that in 3.6 V and 4.5 V, after doping, Five curve is substantially coincidence；And during undoped p, then with the increase for sweeping speed, curve is gradually offset when sweeping speed for 0.1 mV/s Curve, it was demonstrated that there is electric capacity to produce, after illustrating sodium, Fe2O3 doping, more preferably, lithium ion deintercalation is more prone to for the stability of material, and The cycles samples invertibity of undoped p is poor, lithium ion diffusion hindered.Compared with traditional battery material preparation technology, this preparation Method need not too high cost, environmental pollution be few, material electrochemical performance is preferable, and the positive electrode of synthesis is led in electrical source of power The application prospect in domain is very wide, it is adaptable to produced in large quantity.
Brief description of the drawings
Fig. 1 is the XRD of manganate cathode material for lithium before and after sodium, the iron ion doping that embodiment 1 is obtained.
Fig. 2 is the SEM figures of the manganese dioxide presoma that embodiment 1 is obtained, and illustration is corresponding high magnification enlarged drawing.
Fig. 3 is the SEM figures of the undoped p sample that embodiment 1 is obtained, and illustration is corresponding high magnification enlarged drawing.
Fig. 4 is the SEM figures of sample after sodium, the iron ion doping that embodiment 1 is obtained, and illustration amplifies for corresponding high magnification Figure.
Fig. 5 is the EDS figures of manganate cathode material for lithium before and after sodium, the iron ion doping that embodiment 1 is obtained.
Fig. 6 is manganate cathode material for lithium high rate performance figure before and after sodium, the iron ion doping that embodiment 1 is obtained.
Fig. 7 is circulation of the manganate cathode material for lithium under 0.5 C multiplying powers before and after sodium, the iron ion doping that embodiment 1 is obtained Performance map.
Fig. 8 is manganate cathode material for lithium AC impedance figure before and after sodium, the iron ion doping that embodiment 1 is obtained.
Fig. 9 and Figure 10 be before and after sodium, the iron ion doping that embodiment 1 is obtained manganate cathode material for lithium in the case where difference sweeps speed Cyclic voltammogram.
Specific embodiment
Embodiment：
（1）0.025 mol sodium peroxydisulfates and 0.025 mol manganese sulfates are mixed and is dissolved in 80 mL deionized waters, used at room temperature DF-101S type heat-collecting magnetic stirring devices are thoroughly mixed.Then mixed liquor is transferred to the polytetrafluoroethyl-ne of 100 mL In alkene liner, then liner is sealed in stainless steel cauldron, 15 hours are incubated when the temperature for setting is as 120 DEG C, it is naturally cold But to room temperature, filtering is dried more than 20 hours under the conditions of 80 DEG C, obtains black MnO2Powder.
（2）Weigh 0.009202 mol steps（1）Gained MnO2Powder, by LiNa0.06Mn1.94Fe0.06O4Stoichiometry Than weighing 0.0002846 mol sodium acetates, 0.000142 mol di-iron trioxides and 0.00223 mol lithium carbonates, by mixture It is placed in beaker, to the absolute ethyl alcohol that 30 mL are added in beaker, ultrasonic vibration 45 minutes, then drying grinds in agate mortar Mill 50 minutes.
(3) by step（2）It is put into Muffle furnace after gains grinding, is sintered 5 hours at 500 DEG C, sintering completes laggard Row sufficiently grinding, then sinters 18 hours at 750 DEG C, finally cools to room temperature with the furnace, is obtained after hand-ground LiNa0.06Mn1.94F0.06O4。
Synthesized final sample is made the circular pole piece of 15 mm, is assembled into button cell.
Concrete operations are as follows：It is 8 according to mass ratio: 1 :1 ratio weighs active material, PVDF and acetylene respectively It is black, it is sufficiently mixed and mills, appropriate NMP is added, electrode slurry is made, slurry is uniformly coated on aluminium foil with spreader, in After being dried 15 hours in 120 DEG C of vacuum drying chambers, the circular pole piece that multiple quality are 1.7mg is washed into.Electrolyte used is l The LiPF of mol/L6(volume ratio is l to/EC+EMC+DMC: l :L), Celgard2400 microporous polypropylene membranes are barrier film, with gold Category lithium piece is negative pole, full of argon gas, relative humidity are less than 5% and oxygen is forced down and assembled in certain sequence in the glove box of 10 pp Into CR2016 type button cells, after standing 16 hours, ac impedance measurement, charge-discharge test and cyclic voltammetric can be carried out and surveyed Examination.Charging/discharging voltage scope is 3.0 ~ 4.4 V during test material cycle performance, and the multiplying power for using is 0.5 C, the sample after doping Its first discharge specific capacity reaches 124.59 mAh/g.After circulation 100 times, specific discharge capacity is 114.78 mAh/g, and capacity is protected Holdup is 92.13%.
Wherein, the manganate cathode material for lithium that undoped p is obtained is labeled as：LMO；Sodium that embodiment 1 is obtained, iron ion are mixed Miscellaneous manganate cathode material for lithium is labeled as：LMO-NF；PVDF：Kynoar NMP：METHYLPYRROLIDONE；EC：Carbonic acid Vinyl acetate；EMC：Methyl ethyl carbonate DMC：Dimethyl carbonate.

Claims (1)

1. a kind of method that sodium and iron codope prepare High-performance lithium manganate anode material, it is characterised in that concretely comprise the following steps：
（1）0.01 ~ 0.2 mol manganese sources and 0.01 ~ 0.2 mol strong oxidizers are stoichiometrically weighed, both are placed in beaker In, it is subsequently adding the deionized water of 40 ~ 150 mL；At ambient temperature will with DF-101S type heat collecting types constant temperature blender with magnetic force Manganese source and strong oxidizer are thoroughly mixed, and then mixed liquor is transferred in the polytetrafluoroethyllining lining of 50 ~ 200 mL, then will Polytetrafluoroethyllining lining is sealed in stainless steel cauldron, and under the conditions of the temperature for setting is as 100 ~ 200 DEG C, insulation 8 ~ 24 is small When, room temperature is naturally cooled to, filter, dried 18 ~ 48 hours under the conditions of 60 ~ 120 DEG C, obtain manganese source presoma black powder；
（2）Step is weighed according to mol ratio（1）Resulting manganese source presoma 0.001 ~ 0.2 mol, 0.001-0.1 mol lithium sources, The source of iron and 0.0001 ~ 0.1 mol sodium sources of 0.0001 ~ 0.1 mol doping；Four are placed in beaker and 40-100 mL are added Absolute ethyl alcohol, be put into after ultrasonic vibration 20-60 minutes in baking oven and dried under conditions of 60 ~ 120 DEG C, then ground in mortar Mill 10 ~ 120 minutes；
（3）By step（2）Be placed in Muffle furnace 250 ~ 650 DEG C of pre-sintering 2-10 hours after gains grinding, it is pre-sintered after carry out Grind and in Muffle furnace 650 ~ 850 DEG C calcine 10 ~ 30 hours, cool to room temperature with the furnace, obtain final product sodium and the composite mixed manganese of iron Sour lithium anode material LiNaxMn2-yFeyO4, wherein：X=0.01 ~ 0.2, y=0.01 ~ 0.2；
The strong oxidizer be ammonium persulfate, potassium hyperchlorate, potassium permanganate, the one kind analyzed in pure hydrogen peroxide and sodium peroxydisulfate or It is various；
The manganese source is one or more in manganese acetate, Manganous sulfate monohydrate and manganese carbonate；
The lithium source is one or more in lithium acetate, a hydronium(ion) lithia and lithium carbonate；
The source of iron of the doping is one or more in iron hydroxide, iron oxide, ferrous oxide and ferroso-ferric oxide；
The sodium source of the doping is one or more in sodium acetate, sodium carbonate and NaOH.
CN201611075105.9A 2016-11-29 2016-11-29 A kind of method that sodium and iron codope prepare High-performance lithium manganate anode material Withdrawn CN106784657A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109119607A (en) * 2018-08-04 2019-01-01 浙江瓦力新能源科技有限公司 A kind of polypyrrole nanotube cladding nickel lithium manganate cathode material and preparation method thereof
CN112897584A (en) * 2021-01-21 2021-06-04 湘潭大学 Lithium-rich manganese-based cathode material with divalent cations doped in lithium layer and preparation method thereof
CN115180652A (en) * 2022-07-14 2022-10-14 西安交通大学 Manganese-based multi-element multi-position doped positive electrode material of sodium ion battery and preparation method
CN117457892A (en) * 2023-12-22 2024-01-26 宁波容百新能源科技股份有限公司 Positive electrode active material, preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103794775A (en) * 2014-01-24 2014-05-14 国家纳米科学中心 Preparation method of positive electrode material of iron-doped lithium manganate acid lithium ion battery
CN105428641A (en) * 2015-12-10 2016-03-23 桂林理工大学 Method for preparing lithium manganese oxide cathode material by synergistically doping aluminum and sodium with high rate performance
CN105932244A (en) * 2016-05-21 2016-09-07 桂林理工大学 Method for preparing iron-fluorine composite doped lithium manganate positive electrode material by combination of hydrothermal method and two-step sintering method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103794775A (en) * 2014-01-24 2014-05-14 国家纳米科学中心 Preparation method of positive electrode material of iron-doped lithium manganate acid lithium ion battery
CN105428641A (en) * 2015-12-10 2016-03-23 桂林理工大学 Method for preparing lithium manganese oxide cathode material by synergistically doping aluminum and sodium with high rate performance
CN105932244A (en) * 2016-05-21 2016-09-07 桂林理工大学 Method for preparing iron-fluorine composite doped lithium manganate positive electrode material by combination of hydrothermal method and two-step sintering method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109119607A (en) * 2018-08-04 2019-01-01 浙江瓦力新能源科技有限公司 A kind of polypyrrole nanotube cladding nickel lithium manganate cathode material and preparation method thereof
CN109119607B (en) * 2018-08-04 2022-04-01 浙江金鹰瓦力新能源科技有限公司 Polypyrrole nanotube coated lithium nickel manganese oxide positive electrode material and preparation method thereof
CN112897584A (en) * 2021-01-21 2021-06-04 湘潭大学 Lithium-rich manganese-based cathode material with divalent cations doped in lithium layer and preparation method thereof
CN115180652A (en) * 2022-07-14 2022-10-14 西安交通大学 Manganese-based multi-element multi-position doped positive electrode material of sodium ion battery and preparation method
CN115180652B (en) * 2022-07-14 2023-07-25 西安交通大学 Manganese-based multi-element multi-position doped positive electrode material of sodium ion battery and preparation method thereof
CN117457892A (en) * 2023-12-22 2024-01-26 宁波容百新能源科技股份有限公司 Positive electrode active material, preparation method and application thereof
CN117457892B (en) * 2023-12-22 2024-04-12 宁波容百新能源科技股份有限公司 Positive electrode active material, preparation method and application thereof

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Application publication date: 20170531