CN107845802B - A kind of conducting polymer for lithium battery coats cobalt acid lithium and preparation method thereof - Google Patents
A kind of conducting polymer for lithium battery coats cobalt acid lithium and preparation method thereof Download PDFInfo
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- CN107845802B CN107845802B CN201711173861.XA CN201711173861A CN107845802B CN 107845802 B CN107845802 B CN 107845802B CN 201711173861 A CN201711173861 A CN 201711173861A CN 107845802 B CN107845802 B CN 107845802B
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- 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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Abstract
The present invention relates to the preparation methods that a kind of conducting polymer for lithium battery coats high voltage type cobalt acid lithium, mainly include the following steps that：(1) high temperature solid state reaction prepares doping cobalt acid lithium；(2) preparation (3) liquid-phase impregnation process cladding processing of conducting polymer dispersion liquid；At least one of wherein described cobalt acid lithium incorporation Al, Mg, Ti, Gr, for the concentration of each doped chemical in 500 5000ppm, the conductive polymer coating is one kind in polyaniline, polypyrrole, polythiophene；Material obtained by this method has sufficiently stable crystal structure, can be in 4.35V 4.60V (vs Li+/ Li) there is under voltage good capacity, while there is good cyclicity, and it is easy to implement industrialized production.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical fields, more particularly to a kind of conducting polymer for lithium battery
Object coats cobalt acid lithium and preparation method thereof.
Background technology
Lithium ion battery pollutes the features such as few with its memory-less effect, long lifespan, in our life extensively
Ground application is deep into mobile electronic device and hybrid vehicle every field.Ripe one of the lithium electric material of commercialization at present
Cobalt acid lithium is because its compacted density is big, and the features such as platform voltage is high, and capacity is big, is most widely used in 3C digital products
Lithium electric material.The theoretical capacity of cobalt acid lithium is up to 274mAh/g, and traditional cobalt acid lithium is in 3.0V-4.2V (vs Li+/ Li) under, hair
The capacity waved only has about 158mhA/g.With the increase of electronic equipment performance requirement, the requirement to battery capacity is also higher and higher,
Wish to more play the capacity of cobalt acid lithium.The way of mainstream is exactly to improve charging voltage, makes more lithiums embedding de-, but big
After amount loses Li, crystalline structure can become unstable, and irreversible transition occurs to make cycle life greatly reduce, and in high electricity
The side reactions such as Co dissolves, electrolyte is aoxidized can occur at pressure material and electrolyte interface, further decrease material lifetime.
In order to solve this problem, it is presently mainly carried out in terms of improving structural stability and reducing interface side reaction two
Design.By the doping of the elements such as magnesium, aluminium, zirconium, titanium, the lifetime stability of cobalt acid lithium, but doped chemical amount at present can be improved
Usual larger (27%-35% as described in 104538599 A of patent document CN), due to not having the active doping member of storage lithium
Element amount is big, often causes more capacitance loss.In terms of interface processing, using metal oxides such as aluminium oxide, magnesia
It is coated, but this kind of metal conductive oxide is poor, and same without storage lithium activity, inevitably reduces the appearance of material
The performance of amount and multiplying power.
And conducting polymer is a kind of covering material haveing excellent performance, outstanding chemical stability can play protection
The effect of material interface, good ductility can slow down the bulk effect in charge and discharge process as buffer matrix, good
Good electric conductivity can promote the migration of lithium ion.Domestic also someone coats lithium electric material using the substance, such as specially
Sharp 104600314 A of document CN carry out cladding processing using situ aggregation method to nickel ion doped, but such methods are more complicated,
Cost is higher, and industrialization difficulty is big.
Invention content
In view of the problems of the existing technology, the object of the present invention is to provide a kind of conducting polymer packets for lithium battery
Cover cobalt acid lithium and preparation method thereof.
To achieve the goals above, the present invention uses following technical scheme：
A kind of conducting polymer for lithium battery coats the preparation method of high voltage type cobalt acid lithium, includes the following steps：
1) it using lithium carbonate, cobaltosic oxide as primary raw material, using metal oxide as auxiliary material, is mixed in batch mixer equal
It is even, then carry out solid phase pyroreaction, reaction after the completion of through pulverizing and sieving processing obtain doping cobalt acid lithium；
2) micro/nano level conducting polymer powder is scattered in ethyl alcohol, uniform conducting polymer ethyl alcohol dispersion is made
Liquid；
3) step 1 doping cobalt acid lithium obtained is added into conducting polymer alcohol dispersion liquid made from step 2, is stirred
After reaction, then drying is heat-treated, is ground up, sieved the cobalt acid lithium coated to get conducting polymer.
Preferably, the metal oxide is selected from least one of magnesia, aluminium oxide, titanium dioxide, zirconium oxide.
Preferably, the one kind of the conducting polymer powder in polyaniline, polypyrrole, polythiophene, in charge and discharge
The effects that improving electric conductivity, reducing side reaction, be sustained volume change is acted in the process.
It is further preferred that the particle size range that the conducting polymer powder is is.
Preferably, primary raw material mass ratio Li by elements：Co=1.02-1.09.
Preferably, in the doping cobalt acid lithium, a concentration of 500-5000ppm of each doped chemical.
Preferably, a concentration of 0.005-0.05g/ml of conducting polymer alcohol dispersion liquid.
Preferably, in the cobalt acid lithium of conducting polymer cladding, the quality of the conducting polymer is conducting polymer
The 1%-8% of the cobalt acid lithium gross mass of object cladding.
Preferably, the temperature of solid phase pyroreaction is 850-1100 DEG C in step (1), time 6-12h.
Preferably, in step (3), mixing speed is 250~500r/min, mixing time 10-120min.It is preferred that
Ground, in step (3), the heat treatment is to be handled 1-4 hours in 100-200 DEG C of baking oven.
A kind of cobalt acid lithium of conducting polymer cladding, is prepared by above-mentioned preparation method.
Preferably, the grain size D50 of the cobalt acid lithium of the conducting polymer cladding is 6~21um, specific surface area 0.15m2/
G~0.55m2The charge cutoff voltage of/g, tap density >=2.5g/cm3, adaptation are 4.35~4.60V (vs Li+/Li)。
Beneficial effects of the present invention：
(1) amount of institute's doped chemical of the present invention is few, and under the premise of enhancing structure stability, the gram volume of cobalt acid lithium loses
It is few；
(2) clad of the present invention is conducting polymer, and outstanding chemical stability can play protected material
Expect that the effect at interface, good ductility can slow down the bulk effect in charge and discharge process as buffer matrix, it is good
Electric conductivity can promote the migration of lithium ion；
(3) present invention is by from design of both structural stability and interface stability, finally making the cycle of material
Service life significantly improves and possesses higher gram volume；
(4) present invention is coated using liquid phase wet method, and clad coats evenly, is thinner than mechanical mixture, technique ratio
Situ aggregation method is simpler, at low cost, is easy to implement industrialization.
Description of the drawings
Fig. 1 is the XRD spectra of the cobalt acid lithium of polyaniline-coated degree 2% prepared by embodiment 1；
Fig. 2 is before and after the cobalt acid lithium of polyaniline-coated degree 2% prepared by embodiment 1 is adulterated at 4.55V and before and after cladding
Cycle life performance compares under 1C electric currents；
Fig. 3 is before and after the cobalt acid lithium of polyaniline-coated degree 2% prepared by embodiment 1 is adulterated at 4.50V and before and after cladding
Cycle life performance compares under 1C electric currents.
Specific implementation mode
For a further understanding of the present invention, it is more comprehensively careful to be carried out below in conjunction with the accompanying drawings to the present invention with preferred embodiment
Illustrate, but protection scope of the present invention is not limited by the following examples.
Do not mentionlet alone bright except peculiar, the various reagents used, raw material are the electricity that can directly buy from the market in the present invention
Pond grade or technical grade commodity.
Embodiment 1
500g cobaltosic oxides, 240g lithium carbonates, 1.5g magnesia, 1g titanium oxide, 2.5g aluminium oxide are sufficiently stirred mixed
It closes, high temperature solid state reaction 12h is then carried out at 980 DEG C, obtains bulk product, finally obtain powder by pulverizing and sieving processing
State adulterates cobalt acid lithium.
2) it takes 5g micro/nano level powdered form polyanilines to be scattered in 500mL ethyl alcohol by being ultrasonically treated, is made a concentration of
The homogeneous conductive polymer alcohol dispersion liquid of 0.01g/ml.
3) 250g steps 1 gained cobalt acid lithium is added into above-mentioned 500ml conducting polymers alcohol dispersion liquid, continues fully to stir
Mix 25min, gained slurry be placed in baking oven at 60 DEG C and is dried, finally in an oven 120 DEG C carry out heat treatment 2 hours, grinding
Sieving is high voltage type cobalt acid lithium to get polyaniline-coated degree 2%.
Above-mentioned products obtained therefrom is taken to carry out powder diffraction XRD tests, the results are shown in Figure 1, it can be seen that new there is no generating
Phase or dephasign illustrate by the way that after cladding or doping, cobalt acid lithium can retain the crystal structure of original well.
Comparative example 1
500g cobaltosic oxides, 240g lithium carbonates, 1.5g magnesia, 1g titanium oxide, 2.5g aluminium oxide are sufficiently stirred mixed
It closes, high temperature solid state reaction 12h is then carried out at 980 DEG C, obtains bulk product, finally obtain powder by pulverizing and sieving processing
State adulterates cobalt acid lithium.
Comparative example 2
500g cobaltosic oxides, 240g lithium carbonates are thoroughly mixed, high temperature solid state reaction is then carried out at 980 DEG C
12h obtains bulk product, finally obtains the undoped cobalt acid lithium of powdered form by pulverizing and sieving to handle.
The cycle performance of material is tested according to following methods：By the cobalt acid lithium material of gained and conductive agent acetylene black
With binder PVDF according to 9:0.5:0.5 mass ratio is mixed in NMP in 15ml, is sufficiently stirred to form slurry, then passes through painting
It covers machine and is coated in aluminium foil surface, suitable size is cut into after drying, using lithium piece as cathode, lithium hexafluorophosphate solution is electrolyte,
It is assembled into button cell in the glove box that argon gas is protected using 2032 type button cell shells, is carried out at 45 DEG C, under 1C electric currents
High temperature circulation is tested.
According to above-mentioned test method, embodiment 1, comparative example 1 and comparative example 2 are carried out in 3.0V-4.55V voltage ranges
Test.The results are shown in Figure 2, and comparative example 2 is to undope not coat sample, in 40 weeks high temperature circulations, gram volume retention rate
It is 18%, is adulterated in comparative example 1 and do not coat sample, gram volume retention rate is 53%, and is mixed with sample in embodiment 1,
Gram volume retention rate is 81%.Illustrate that the cycle performance of material is greatly improved, and three exists by doping and cladding
The capacity that first lap plays under 1C electric currents is 180-190mAh/g.
Embodiment 2
500g cobaltosic oxides, 250g lithium carbonates, 1.0g magnesia, 1g titanium oxide, 1.5g aluminium oxide are sufficiently stirred mixed
It closes, high temperature solid state reaction 12h is then carried out at 1020 DEG C, obtains bulk product, finally obtain powder by pulverizing and sieving processing
Final states adulterates cobalt acid lithium.
2) it takes 4g micro/nano level powdered form polyanilines to be scattered in 500mL ethyl alcohol by being ultrasonically treated, is made a concentration of
The homogeneous conductive polymer alcohol dispersion liquid of 0.008g/ml.
3) 250g steps 1 gained cobalt acid lithium is added into above-mentioned 500ml conducting polymers alcohol dispersion liquid, continues fully to stir
Mix 30min, gained slurry be placed in baking oven at 60 DEG C and is dried, finally in an oven 120 DEG C carry out heat treatment 2 hours, grinding
Sieving is high voltage type cobalt acid lithium to get conducting polymer coverage degree 1.6%.
Comparative example 3
500g cobaltosic oxides, 250g lithium carbonates, 1.0g magnesia, 1g titanium oxide, 1.5g aluminium oxide are sufficiently stirred mixed
It closes, high temperature solid state reaction 12h is then carried out at 1020 DEG C, obtains bulk product, finally obtain powder by pulverizing and sieving processing
Final states adulterates cobalt acid lithium.
Comparative example 4
500g cobaltosic oxides, 250g lithium carbonates are thoroughly mixed, it is anti-that high temperature solid-state is then carried out at 1020 DEG C
Answer 12h, obtain bulk product, finally through pulverizing and sieving processing obtain powdered form doping cobalt acid lithium.
According to above-mentioned test method, embodiment 1, comparative example 1 and comparative example 2 are carried out in 3.0V-4.50V voltage ranges
Test.The results are shown in Figure 3, and comparative example 4 is to undope not coat sample, in 40 weeks high temperature circulations, gram volume retention rate
It is 49%, comparative example 3 is that doping does not coat sample, and gram volume retention rate is 74%, and is mixed with sample in embodiment 1,
Gram volume retention rate is 92%.Illustrate that, by doping and cladding, the cycle performance of material is greatly improved.And three exists
The capacity that first lap plays under 1C electric currents is 180-190mAh/g.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of conducting polymer for lithium battery coats the preparation method of high voltage type cobalt acid lithium, which is characterized in that including
Following steps：
1) it using lithium carbonate, cobaltosic oxide as primary raw material, using metal oxide as auxiliary material, is uniformly mixed in batch mixer, so
Afterwards carry out solid phase pyroreaction, reaction after the completion of through pulverizing and sieving processing obtain doping cobalt acid lithium；
2) conducting polymer powder is scattered in ethyl alcohol, uniform conducting polymer alcohol dispersion liquid is made；
3) step 1) doping cobalt acid lithium obtained is added into conducting polymer alcohol dispersion liquid made from step 2), stirring is anti-
Ying Hou, drying, is then heat-treated, is ground up, sieved the cobalt acid lithium coated to get conducting polymer；
Wherein, primary raw material mass ratio Li by elements：Co=1.02-1.09；In the doping cobalt acid lithium, respectively mix
A concentration of 500-5000ppm of miscellaneous element；The quality of the conducting polymer is the cobalt acid lithium gross mass of conducting polymer cladding
1%-8%；The heat treatment is to be handled 1-4 hours in 100-200 DEG C of baking oven；The cobalt acid of the conducting polymer cladding
The grain size D50 of lithium is 6~21um, specific surface area 0.15m2/ g~0.55m2/g。
2. the conducting polymer according to claim 1 for lithium battery coats the preparation method of high voltage type cobalt acid lithium,
It is characterized in that, the metal oxide is selected from least one of magnesia, aluminium oxide, titanium dioxide, zirconium oxide.
3. the conducting polymer according to claim 1 for lithium battery coats the preparation method of high voltage type cobalt acid lithium,
It is characterized in that, the one kind of the conducting polymer powder in polyaniline, polypyrrole, polythiophene.
4. the conducting polymer according to claim 1 or 3 for lithium battery coats the preparation side of high voltage type cobalt acid lithium
Method, which is characterized in that a concentration of 0.005-0.05g/ml of conducting polymer alcohol dispersion liquid.
5. the conducting polymer according to claim 1 for lithium battery coats the preparation method of high voltage type cobalt acid lithium,
It is characterized in that, in step 3), mixing speed is 250~500r/min, mixing time 10-120min.
6. a kind of cobalt acid lithium of conducting polymer cladding, which is characterized in that by the preparation method system of any one of claim 1-5
It is standby to obtain.
7. the cobalt acid lithium of conducting polymer cladding according to claim 6, which is characterized in that the conducting polymer cladding
Cobalt acid lithium tap density >=2.5g/cm3, the charge cutoff voltage of adaptation is 4.35~4.60V (vs Li+/Li)。
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| CN109037604A (en) * | 2018-06-13 | 2018-12-18 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of polyaniline-coated lithium titanate anode material |
| CN110391414A (en) * | 2019-06-19 | 2019-10-29 | 重庆市维都利新能源有限公司 | A kind of high energy density polymer lithium ion battery and preparation method thereof |
| CN111477856B (en) * | 2020-04-26 | 2023-05-05 | 河北省科学院能源研究所 | Nickel-based positive electrode material and preparation method thereof |
| CN111825124B (en) * | 2020-06-10 | 2022-02-15 | 昆明理工大学 | Method for preparing high-voltage anode material by surface modification and regeneration of waste lithium cobaltate material |
| CN112234203A (en) * | 2020-10-15 | 2021-01-15 | 光鼎铷业(广州)集团有限公司 | Conductive polymer coated rubidium-doped high-nickel ternary lithium battery positive electrode material and preparation method thereof |
| CN114937766B (en) * | 2022-05-31 | 2023-10-31 | 济宁学院 | Preparation method of transition metal doped poly (m-phenylenediamine) coated positive electrode material |
| CN115020672B (en) * | 2022-06-30 | 2024-03-12 | 广东邦普循环科技有限公司 | Lithium cobalt oxide positive electrode material and preparation method and application thereof |
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| CN102522563A (en) * | 2011-12-30 | 2012-06-27 | 中国科学院广州能源研究所 | Conducting-polymer dipped and coated lithium-ion battery composite-electrode material and preparation method thereof |
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| CN102522563A (en) * | 2011-12-30 | 2012-06-27 | 中国科学院广州能源研究所 | Conducting-polymer dipped and coated lithium-ion battery composite-electrode material and preparation method thereof |
| CN104659335A (en) * | 2014-12-09 | 2015-05-27 | 江波 | Preparation method for lithium ion battery positive electrode material |
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Application publication date: 20180327 Assignee: Zhongguancun Technology Leasing Co.,Ltd. Assignor: JIANGMEN KANHOO INDUSTRY Co.,Ltd. Contract record no.: X2022980016573 Denomination of invention: Conductive polymer coated lithium cobalate for lithium battery and its preparation method Granted publication date: 20181019 License type: Exclusive License Record date: 20220926 |
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Denomination of invention: Conductive polymer coated lithium cobalate for lithium battery and its preparation method Effective date of registration: 20220927 Granted publication date: 20181019 Pledgee: Zhongguancun Technology Leasing Co.,Ltd. Pledgor: JIANGMEN KANHOO INDUSTRY Co.,Ltd. Registration number: Y2022980016721 |