CN109616620A - A kind of method of the nickelic positive electrode of magnesia coated lithium ion battery - Google Patents

A kind of method of the nickelic positive electrode of magnesia coated lithium ion battery Download PDF

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Publication number
CN109616620A
CN109616620A CN201811201866.3A CN201811201866A CN109616620A CN 109616620 A CN109616620 A CN 109616620A CN 201811201866 A CN201811201866 A CN 201811201866A CN 109616620 A CN109616620 A CN 109616620A
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China
Prior art keywords
magnesia
beaker
positive electrode
dissolved
nickelic positive
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CN201811201866.3A
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Chinese (zh)
Inventor
李伟伟
徐云军
宋二虎
陈丹凤
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Henan Kelong New Energy Ltd By Share Ltd
Xinxiang University
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Henan Kelong New Energy Ltd By Share Ltd
Xinxiang University
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Priority to CN201811201866.3A priority Critical patent/CN109616620A/en
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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
    • 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
    • H01M4/52—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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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 & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention relates to a kind of methods of nickelic positive electrode of magnesia coated lithium ion battery to obtain colourless transparent solution comprising steps of magnesia is dissolved in acetic acid solution by (1), after magnesia is completely dissolved, is dissolved in 250ml volumetric flask surely with dehydrated alcohol；(2) it weighs nickelic positive electrode to be put into beaker, ethyl alcohol is added, and stir under blender；(3) in the step (3), the mass percent that magnesia accounts for anode material for lithium-ion batteries is 0.01~1wt%, evaporating to close to completely in beaker；(4) lasting stirring, until evaporating completely in beaker；(5) product obtained in above-mentioned steps (4) is 1~4 hour, 80 DEG C~110 DEG C of temperature dry in drying box；(6) product obtained in above-mentioned steps (5) is heat-treated, heat treatment time 2~6 hours, 500 DEG C~800 DEG C of temperature.Raw material sources of the present invention are cheap, and technical process is simple, and the period is short, and improve the performance of material.

Description

A kind of method of the nickelic positive electrode of magnesia coated lithium ion battery
Technical field
The present invention relates to material and chemical field, in particular to a kind of nickelic positive electrode of magnesia coated lithium ion battery Method.
Background technique
The performance of anode material for lithium-ion batteries has become the critical issue for restricting lithium ion battery development and application One of.Nickel-base anode material is because it has the characteristics that high specific discharge capacity, at low cost, environmental-friendly, by the wide of researchers General concern.Relative to common anode material for lithium-ion batteries LiCoO2, LiFePO4, LiMn2O4, Li (Ni0.5Co0.2Mn0.3) O2 etc., nickelic positive electrode have higher specific discharge capacity (> 180mAhg).
Currently, there are the pH value higher, poor circulation of nickel-base anode material.The disadvantages of safety is lower.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of method of nickelic positive electrode of magnesia coated lithium ion battery, Method raw material sources are cheap, and technical process is simple, and the period is short, and improve the performance of material.
To solve the above-mentioned problems, the method for a kind of nickelic positive electrode of magnesia coated lithium ion battery of the invention, Include the following steps:
(1), magnesia is dissolved in acetic acid solution, acetic acid and magnesia molar ratio are 2:1~2.1:1, are obtained colorless and transparent Solution after magnesia is completely dissolved, is dissolved in 250ml volumetric flask, concentration is calculated as 21.96mg/ with magnesia surely with dehydrated alcohol ml；
(2), it weighs nickelic positive electrode 20g to be put into beaker, ethyl alcohol 20ml is added, and stir under blender；
(3), in the step (3), magnesia account for anode material for lithium-ion batteries mass percent be 0.01~ 1wt%, evaporating to close to complete in beaker；
Covering amount according to magnesia is 0.2%, takes step (1) acquired solution 1.82ml, and the beaker of step (2) is added In, stirring；
(4), lasting stirring, until evaporating completely in beaker；
(5), product obtained in above-mentioned steps (4) is 1~4 hour, 80 DEG C~110 DEG C of temperature dry in drying box；
(6), product obtained in above-mentioned steps (5) is heat-treated, heat treatment time 2~6 hours, 500 DEG C of temperature ~800 DEG C.
Wherein, in the step (3), further comprising the steps of: according to the covering amount of magnesia is 0.2%, is taken obtained by step (1) Solution 1.82ml is added in the beaker of step (2), stirring.
Detailed description of the invention
Fig. 1: the scanning electron microscope map of nickelic positive electrode before coating:
Fig. 2: the scanning electron microscope map of nickelic positive electrode after cladding:
Fig. 3: the XRD spectrum of 1 gained target product of embodiment；
Fig. 4: the map of the first charge-discharge curve of the chemical property of 1 gained target product of embodiment；
Fig. 5: the map of 50 weeks discharge capacitances of circulation of the chemical property of 1 gained target product of embodiment:
Fig. 6: the scanning electron microscope map of 1 gained target product of reference examples.
Specific embodiment
To keep the present invention clearer, clear, the present invention is described in more detail below.It should be appreciated that this place is retouched The specific embodiment stated is only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1:
1. weighing magnesia 5.5g to be put into beaker, acetic acid solution about 40ml is added, after magnesia is completely dissolved, uses ethyl alcohol Surely it is dissolved in 250ml volumetric flask, concentration is 21.96mg/ml (in terms of magnesia)；
2. weighing nickelic positive electrode (LiNi0.9Co0.1O2) about 20g to be put into beaker, ethyl alcohol 20ml is added, and stirring It mixes and is stirred under device；
3. the covering amount according to magnesia is 0.2%, step (1) acquired solution about 1.82ml is taken, the burning of step (2) is added In cup, stirring；
4. lasting stirring, until evaporating to close to completely in beaker；
5. product obtained in step (4) is 2 hours, 100 DEG C of temperature dry in drying box；
6. product obtained in step (5) is heat-treated, heat treatment time 4 hours, 750 DEG C of temperature.
Embodiment 2:
1. weighing magnesia 5.5g to be put into beaker, acetic acid solution about 40ml is added, after magnesia is completely dissolved, uses ethyl alcohol Surely it is dissolved in 250ml volumetric flask, concentration is 21.96mg/ml (in terms of magnesia)；
2. weighing nickelic positive electrode (LiNi0.9Co0.1O2) about 20g to be put into beaker, ethyl alcohol 20ml is added, and stirring It mixes and is stirred under device；
3. the covering amount according to magnesia is 0.2%, step (1) acquired solution about 1.82ml is taken, the burning of step (2) is added In cup, stirring；
4. lasting stirring, until evaporating to close to completely in beaker；
5. product obtained in step (4) is 1 hour, 80 DEG C of temperature dry in drying box；
6. product obtained in step (5) is heat-treated, heat treatment time 2 hours, 500 DEG C of temperature；
Embodiment 3:
1. weighing magnesia 5.5g to be put into beaker, acetic acid solution about 40ml is added, after magnesia is completely dissolved, uses ethyl alcohol Surely it being dissolved in 250ml volumetric flask, concentration is 21.96mg/ml (in terms of magnesia),
2. weighing nickelic positive electrode (LiNi0.9Co0.1O2) about 20g to be put into beaker, ethyl alcohol 20ml is added, and stirring It mixes and is stirred under device,
3. the covering amount according to magnesia is 0.2%, step (1) acquired solution about 1.82ml is taken, the burning of step (2) is added In cup, stirring,
4. lasting stirring, until evaporating to close to completely in beaker,
5. product obtained in step (4) is 4 hours dry in drying box, 110 DEG C of temperature,
6. product obtained in step (5) is heat-treated, heat treatment time 6 hours, 800 DEG C of temperature.
The SEM figure of the nickelic positive electrode in cladding front and back is shown in Fig. 1 -- before cladding, seeing Fig. 2 -- after cladding (i.e. target product). From Fig. 1,2: before cladding, the sharpness of border of material surface particle；After cladding, the obscurity boundary of material surface particle；Known to Material surface has coated layer of substance.The source Mg has been only introduced in the process in view of cladding, and necessarily MgO is calcined later in the source Mg, because This, nickelic positive electrode surface cladding has gone up MgO, and material still keeps good chondritic, clad after MgO is coated It is uniformly complete.
The XRD diagram of target product is shown in Fig. 3.As shown in Figure 3: products obtained therefrom occurs without dephasign peak, the ɑ-with hexagonal crystal system NaFeO2 structure.Do not have to show the diffraction maximum of MgO in XRD spectrum, be due to MgO amount very little, peak contrast it is too low caused by.In Fig. 3 It has been shown that, the main Qiang Fengwei (003) of sample, secondary Qiang Fengwei (104), (006) and (102) peak, (108) and (110) peak point of sample It splits obviously, illustrating sample all has good layer structure.
At room temperature, target product and electrically conductive graphite, acetylene black, PVDF is abundant in NMP by 90: 2: 2: 6 mass ratio It is uniformly mixed and is made into slurry, then slurry is coated in aluminum foil current collector.After 110 DEG C dry, being cut into diameter is The circle of 14mm, as anode pole piece.By anode pole piece in the glove box full of high-purity argon gas, lithium anode, diaphragm and Electrolyte is assembled into R2016 type button cell, and electrolyte is 1mol/LLiPF6/ (EC+DEC, volume ratio 1: 1).It is surveyed using battery It tries instrument and carries out electric performance test, voltage range is 2.75~4.25V, multiplying power 0.1C.Test result is as shown in Figure 4,5, and Fig. 4 is First charge-discharge curve, Fig. 5 are the discharge capacitance for recycling 50 weeks.It discharges for the first time ratio it can be seen from Fig. 4,5 in 0.1C Capacitance is about 191mAh/g, and under the conditions of 0.1C, after room temperature charge and discharge cycles 50 times, capacity retention ratio is about 94.6%.
Reference examples 1:
The difference from embodiment 1 is that: the dosage of acetic acid is according to MgO in step (1): the molar ratio of acetic acid is 1: 3 addition, It is other with embodiment 1.
The SEM figure of products obtained therefrom is as shown in Figure 6.As seen from Figure 6: the spherical structure that granular raw comes is destroyed, greatly Particle is fractured into little particle.This is because simultaneously the amount of acetic acid is excessive, acetic acid and oxide are had occurred instead during heat treatment It answers, spherical macro is made to be fractured into little particle.

Claims (2)

1. a kind of method of the nickelic positive electrode of magnesia coated lithium ion battery, it is characterised in that include the following steps:
(1), magnesia being dissolved in acetic acid solution, acetic acid and magnesia molar ratio are 2:1~2.1:1, colourless transparent solution is obtained, After magnesia is completely dissolved, it is dissolved in 250ml volumetric flask surely with dehydrated alcohol, concentration is calculated as 21.96mg/ml with magnesia；
(2), it weighs nickelic positive electrode 20g to be put into beaker, ethyl alcohol 20ml is added, and stir under blender；
(3), in the step (3), the mass percent that magnesia accounts for anode material for lithium-ion batteries is 0.01~1wt%, Evaporating to close to completely in beaker；
Covering amount according to magnesia is 0.2%, takes step (1) acquired solution 1.82ml, is added in the beaker of step (2), stirs It mixes；
(4), lasting stirring, until evaporating completely in beaker；
(5), product obtained in above-mentioned steps (4) is 1~4 hour, 80 DEG C~110 DEG C of temperature dry in drying box；
(6), product obtained in above-mentioned steps (5) is heat-treated, heat treatment time 2~6 hours, temperature 500 DEG C~800 ℃。
2. a kind of method of nickelic positive electrode of magnesia coated lithium ion battery according to claim 1, feature exist In: in the step (3), further comprising the steps of: according to the covering amount of magnesia is 0.2%, takes step (1) acquired solution 1.82ml is added in the beaker of step (2), stirring.
CN201811201866.3A 2018-10-16 2018-10-16 A kind of method of the nickelic positive electrode of magnesia coated lithium ion battery Pending CN109616620A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140141329A1 (en) * 2012-10-02 2014-05-22 Massachusetts Institute Of Technology Molybdenum oxides and uses thereof
CN105322176A (en) * 2015-09-23 2016-02-10 合肥国轩高科动力能源有限公司 Surface coating method of cathode material for lithium-ion battery
CN106602021A (en) * 2016-12-22 2017-04-26 金瑞新材料科技股份有限公司 Coated positive electrode material of lithium-ion battery and preparation method of positive electrode material
CN108336348A (en) * 2018-03-29 2018-07-27 新乡学院 A kind of method of alumina-coated anode material for lithium-ion batteries
CN108493415A (en) * 2018-03-21 2018-09-04 苏州林奈新能源有限公司 A kind of nickel cobalt aluminium ternary anode material for lithium-ion batteries, the Preparation method and use of MgO claddings

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140141329A1 (en) * 2012-10-02 2014-05-22 Massachusetts Institute Of Technology Molybdenum oxides and uses thereof
CN105322176A (en) * 2015-09-23 2016-02-10 合肥国轩高科动力能源有限公司 Surface coating method of cathode material for lithium-ion battery
CN106602021A (en) * 2016-12-22 2017-04-26 金瑞新材料科技股份有限公司 Coated positive electrode material of lithium-ion battery and preparation method of positive electrode material
CN108493415A (en) * 2018-03-21 2018-09-04 苏州林奈新能源有限公司 A kind of nickel cobalt aluminium ternary anode material for lithium-ion batteries, the Preparation method and use of MgO claddings
CN108336348A (en) * 2018-03-29 2018-07-27 新乡学院 A kind of method of alumina-coated anode material for lithium-ion batteries

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Application publication date: 20190412