CN109786687A - A kind of preparation method to sacrifice template induced synthesis metal oxide cladding nickel-cobalt-manganese ternary anode material for lithium-ion batteries - Google Patents
A kind of preparation method to sacrifice template induced synthesis metal oxide cladding nickel-cobalt-manganese ternary anode material for lithium-ion batteries Download PDFInfo
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- CN109786687A CN109786687A CN201811545734.2A CN201811545734A CN109786687A CN 109786687 A CN109786687 A CN 109786687A CN 201811545734 A CN201811545734 A CN 201811545734A CN 109786687 A CN109786687 A CN 109786687A
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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
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Abstract
The present invention discloses a kind of preparation method to sacrifice template ZIF-67 induced synthesis metal oxide cladding nickel-cobalt-manganese ternary anode material for lithium-ion batteries, and step includes: liquid phase method synthesis ZIF-67 mould material；By presoma and the complete ternary material of lithium salts mixed sintering and ZIF-67 ultrasonic mixing in ethanol, drying composite later；By dried mixture, sintering obtains target product again in oxygen atmosphere.Generation metal oxide is calcined under oxygen atmosphere by sacrifice ZIF-67 can effectively stablize nickelic ternary material, prevent material from directly with air, contact with moisture, reducing material surface pH, hence it is evident that improve nickelic ternary material service life；Metal oxide carries out " deep layer cladding " along ternary material second particle gap simultaneously, and stable secondary structure prevents inside electrolyte permeability to second particle, is effectively improved the electrochemistry service performance of tertiary cathode material.There is the preparation method simple process, raw material to be easy to get, facilitate the advantage of large-scale production, there is good application prospect.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical fields, and in particular to a kind of to sacrifice template ZIF-67 induction
Form the preparation method of metal oxide cladding nickel-cobalt-manganese ternary anode material for lithium-ion batteries.
Background technique
Energy restructuring, new energy development is using promoting the lithium ion battery as a kind of New Green Energy product-derived quick
Development.Lithium ion battery has become the main force in the fields such as electronic apparatus, electric car, energy storage.With various fields spy
Be not the rapid development in electric car field, to lithium ion battery propose higher energy density, more long circulation life, preferably
The requirement such as security performance.And positive electrode be exactly lithium ion battery bottleneck where, determine lithium ion battery energy density,
Cycle performance and security performance, therefore the positive electrode for improving lithium ion battery is most important.Nickel-cobalt-manganese ternary material is especially
The it is proposed application of nickelic ternary material is so that the service performance of lithium ion battery reaches a new step.But pure nickel cobalt manganese
Ternary material is especially nickelic ternary material in practical there is also high-rate performance, high-temperature behavior are poor, and safety problem is relatively more prominent
Out the problem of.Specifically, nickelic ternary material surface residual alkali (LiOH, Li2CO3Deng) seriously, cause material pH to increase, to later
It sizes mixing and causes difficulty.Furthermore LiOH, Li2CO3And the arch-criminal of later period lithium ion battery flatulence is caused, not only result in electricity
Pond cyclicity is deteriorated, and influences storge quality and chemical property, more there is very big security risk.Therefore it needs to ternary material
Especially nickelic ternary material is modified.
Surface cladding be improve tertiary cathode material service performance research is relatively more and highly effective measure.Cladding
Main purpose is to maintain main body ternary material stable structure, while avoiding electrolyte directly and the contact of ternary material surface, reduces
Electrode/electrolyte interface side reaction, so as to improve ternary material service performance.Cladding type common at present has carbon material packet
It covers, metal fluoride cladding and metal oxide cladding etc., wherein metallic compound such as Al2O3、ZnO、LiXPO4Deng due to preparation
Simple process, this body structure are very stable to be able to perform well in coating tertiary cathode material.But most common method for coating
It is chemical vapor deposition (CVD) and atomic layer deposition (ALD), as the Chinese invention patent of Publication No. CN108258226A discloses
A kind of method of the method preparation carbon coating ternary material with chemical vapor deposition, this method want equipment, reaction condition etc.
It asks higher, is not suitable for large-scale application production.There is also similar problems for atomic layer deposition.It is contemplated that arriving both methods institute
The experiment condition and cost needed, is all unfavorable for large-scale application.
Summary of the invention
The purpose of the present invention is to provide a kind of suitable for large-scale production and application in view of the foregoing to sacrifice template
ZIF-67 induced synthesis metal oxide coats nickel-cobalt-manganese ternary anode material for lithium-ion batteries and preparation method thereof.Realizing benefit
While effectively cladding with ZIF-67 inducing metal oxide to tertiary cathode material, ternary material spy can be effectively reduced
It is not nickelic ternary material surface residual alkali, prevents ternary material second particle intercrystalline failure, hence it is evident that promotes tertiary cathode material electricity
Chemical property.
The present invention provides one kind with sacrifice template ZIF-67 induced synthesis metal oxide cladding nickel-cobalt-manganese ternary lithium from
The preparation method of sub- cell positive material, comprising the following steps:
(1) by nickel-cobalt-manganese ternary precursor material according to presoma: lithium salts=1:1~1.05 carry out mixed lithium, then in oxygen
It is calcined in atmosphere, obtains pure nickel-cobalt-manganternary ternary anode material NCM；
(2) prepare the ethyl alcohol of cabaltous nitrate hexahydrate, methanol mixed solution forms solution A, prepare 2-methylimidazole ethyl alcohol,
Methanol mixed solution forms B solution, and B solution is poured into solution A and is stood after mixing, is centrifuged to obtain sediment with ethyl alcohol,
It is freeze-dried to obtain metal-organic framework material ZIF-67；
(3) by the NCM that step (1) obtains and the ZIF-67 that step (2) obtains among ethyl alcohol ultrasonic mixing, dry mixed
Object；
(4) step (3) resulting mixture is calcined in oxygen atmosphere, calcining is completed to obtain metal oxide
The nickel-cobalt-manganese ternary anode material for lithium-ion batteries of cladding.
Optionally, the nickel-cobalt-manganese ternary precursor material is Ni0.8Co0.1Mn0.1(OH)2、Ni0.8Co0.1Mn0.1CO3、
Ni0.6Co0.2Mn0.2(OH)2、Ni0.6Co0.2Mn0.2CO3、Ni0.5Co0.2Mn0.3(OH)2、Ni0.5Co0.2Mn0.3CO3One of.
Optionally, the lithium salts is at least one of lithium hydroxide, lithium carbonate, lithium acetate.
Optionally, calcination process described in step (1) is 200~400min to be kept the temperature at 500~600 DEG C, then be warming up to
750~850 DEG C of 600~900min of heat preservation, whole heating rate are 1~3 DEG C/min.
Optionally, in step (2) solution A and B solution, the volume ratio of ethyl alcohol and methanol is respectively 1:1~2:1.
Optionally, step (2) B solution and solution A are according to the molar ratio of cabaltous nitrate hexahydrate and 2-methylimidazole
1:1~1:16 mixing.
Optionally, in step (2), the B solution is poured into solution A and stirs 2~10min, stand 22 later~
For 24 hours, it is then centrifuged.
Optionally, the weight ratio that ZIF-67 accounts for NCM in step (3) described mixture is 0.5%~5%.
Optionally, calcination temperature described in step (4) is 700~800 DEG C, and calcination time is 4~6h, heating rate 1
~3 DEG C/min.
The present invention also provides the nickel-cobalt-manganese ternary lithium-ion electrics of the metal oxide prepared by above-mentioned preparation method cladding
Pond positive electrode.
The invention has the benefit that
1) nickelic ternary material can effectively be stablized by generation metal oxide being calcined under oxygen atmosphere by sacrifice ZIF-67
Material, prevent material directly with air, contact with moisture；And can further be reacted with the residual alkali on nickle cobalt lithium manganate surface, reduce table
Face residual alkali concentration reduces material surface pH, is effectively improved nickelic ternary material service life.The metal oxygen in calcination process simultaneously
Compound effectively can carry out significantly more efficient " deep layer cladding " along ternary material second particle gap, this can effectively prevent
Since structure cell variation causes the rupture of second particle, stable secondary structure in circulating battery later, and prevent electrolyte permeability
Solid electrolyte (SEI) film is generated inside to second particle, is consumed the lithium in electrolyte, is effectively improved tertiary cathode material one
As electrochemistry service performance under voltage and high voltage, there is very strong application prospect.
2) preparation method that this method provides, process flow is simple, is applicable to be mass produced.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of 1 gained target product of embodiment.
Fig. 2 is that the SEM of 1 gained target product of embodiment schemes.
Fig. 3 is that 1 gained target product of embodiment is used as lithium electricity in the circulation survey of different voltages section (3-4.3,2.8-4.4)
Try comparison diagram.
Specific embodiment
In order to be more clear technical characterstic and beneficial effect of the invention, it is described in further detail below with reference to example
The present invention.But the invention is not limited to the embodiments provided in specification, it without departing from the principle of the present invention, can
More to be improved, these improvement are also considered as protection scope of the present invention.
Embodiment 1
Step 1: weighing 811 presoma Ni of 2g nickel cobalt manganese0.8Co0.1Mn0.1(OH)2With mono- hydronium(ion) lithia of 0.9356g
(LiOH·H2O) it is fully ground 30min；The mixture ground is placed in the tube furnace of oxygen atmosphere and calcines annealing, calcining
Condition is that 2 DEG C/min is warming up to 550 DEG C of heat preservation 300min, then 2 DEG C/min is warming up to 750 DEG C of heat preservation 10h, naturally cools to often
Temperature obtains 811 ternary material of nickel cobalt manganese.
Step 2: the cabaltous nitrate hexahydrate for weighing 0.3638g is dissolved in the in the mixed solvent of 20ml ethyl alcohol+20ml methanol (A is molten
Liquid), the 2-methylimidazole for weighing 1.642g is dissolved in the in the mixed solvent (B solution) of 20ml ethyl alcohol+20ml methanol.After completely dissolution
B solution is quickly adding into solution A, 5min, still aging 22h are quickly stirred.It is used ethyl alcohol eccentric cleaning 5 times after the completion of ageing
Sediment freeze-drying after centrifugation is obtained ZIF-67 material by obtained precipitating.
Step 3: weighing 811 ternary material of nickel cobalt manganese of 2g and the ZIF-67 material of 0.01g, the two is poured into and fills 10ml
Ultrasound 30min in the beaker of ethyl alcohol, is stirred for 30min later, dries ethyl alcohol at 80 DEG C to obtain mixture, in the mixture
The mass ratio of ZIF-67 and 811 ternary material of nickel cobalt manganese is 0.5%.
Step 4: mixture obtained in step 3 is placed in the tube furnace of oxygen atmosphere and is calcined, calcination condition be 2 DEG C/
Min is warming up to 750 DEG C of heat preservation 5h, this step is residual to sacrifice the ZIF-67 stabilizer to obtain consumption tertiary cathode material surface
Alkali forms metal oxide, obtains target product after naturally cool to room temperature.
Target product manufactured in the present embodiment is taken to carry out X-ray diffraction analysis, scanning electron microscope analysis.Fig. 1 can be seen that
The nickel-cobalt-manganese ternary anode material for lithium-ion batteries of the metal oxide cladding arrived has very high crystallinity, good stratiform knot
Structure.The nickel-cobalt-manganese ternary anode material for lithium-ion batteries for the metal oxide cladding that Fig. 2 can be seen that has very complete very well
Whole secondary structure.
Battery assembly and test: by the target product being prepared according to target product: acetylene black: PVDF=8:1:1 is dissolved in
It sizes mixing in NMP, is coated with later.With lithium metal be to electrode, Celgard-2400 polypropylene screen as diaphragm, 1mol/L's
The solution of the EC+DMC (volume ratio 1:1) of LiPF6 is electrolyte, is assembled into CR2032 button in the glove box full of argon gas
Battery, then will carry out cycle performance test in LAND test macro after the battery standing aging assembled, test voltage is
3-4.3V,2.8-4.4V.The cycle performance figure of battery is as shown in figure 3, the circulation of target product is steady under 2.8-4.4V at 0.5C
It is qualitative more excellent compared with 3-4.3V, and reversible capacity keeps stablizing in 195mAh/g or so, has good chemical property.
Embodiment 2
Step 1: weighing 811 presoma Ni of 2g nickel cobalt manganese0.8Co0.1Mn0.1(OH)2With mono- hydronium(ion) lithia of 0.9356g
(LiOH·H2O) it is fully ground 30min；The mixture ground is placed in the tube furnace of oxygen atmosphere and calcines annealing, calcining
Condition is that 2 DEG C/min is warming up to 550 DEG C of heat preservation 300min, then 2 DEG C/min is warming up to 750 DEG C of heat preservation 10h, naturally cools to often
Temperature obtains 811 ternary material of nickel cobalt manganese.
Step 2: the cabaltous nitrate hexahydrate for weighing 0.3638g is dissolved in the in the mixed solvent of 20ml ethyl alcohol+20ml methanol (A is molten
Liquid), the 2-methylimidazole for weighing 1.642g is dissolved in the in the mixed solvent (B solution) of 20ml ethyl alcohol+20ml methanol.After completely dissolution
B solution is quickly adding into solution A, 5min, still aging 22h are quickly stirred.It is used ethyl alcohol eccentric cleaning 5 times after the completion of ageing
Sediment freeze-drying after centrifugation is obtained ZIF-67 material by obtained precipitating.
Step 3: weighing 811 ternary material of nickel cobalt manganese of 2g and the ZIF-67 material of 0.1g, the two is poured into and fills 10ml
Ultrasound 30min in the beaker of ethyl alcohol, is stirred for 30min later, dries ethyl alcohol at 80 DEG C to obtain mixture, in the mixture
The mass ratio of ZIF-67 and 811 ternary material of nickel cobalt manganese is 5%.
Step 4: mixture obtained in step 3 is placed in the tube furnace of oxygen atmosphere and is calcined, calcination condition be 2 DEG C/
Min is warming up to 750 DEG C of heat preservation 5h, this step is residual to sacrifice the ZIF-67 stabilizer to obtain consumption tertiary cathode material surface
Alkali forms metal oxide, obtains target product after naturally cool to room temperature.
Above-described embodiment is only used to further illustrate one kind of the invention to sacrifice template ZIF-67 induced synthesis metal oxygen
Compound coats the preparation method of nickel-cobalt-manganese ternary anode material for lithium-ion batteries, but the invention is not limited to embodiments, all
Any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention, each fall within this hair
In the protection scope of bright technical solution.
Claims (10)
1. a kind of preparation to sacrifice template induced synthesis metal oxide cladding nickel-cobalt-manganese ternary anode material for lithium-ion batteries
Method, it is characterised in that the following steps are included:
(1) by nickel-cobalt-manganese ternary precursor material according to presoma: lithium salts=1:1~1.05 carry out mixed lithium, then in oxygen atmosphere
In calcined, obtain pure nickel-cobalt-manganternary ternary anode material NCM；
(2) ethyl alcohol, the methanol mixed solution formation solution A for preparing cabaltous nitrate hexahydrate, prepare ethyl alcohol, the methanol of 2-methylimidazole
Mixed solution forms B solution, and B solution is poured into solution A and is stood after mixing, is centrifuged to obtain sediment with ethyl alcohol, through cold
Jelly is dried to obtain metal-organic framework material ZIF-67；
(3) by the NCM that step (1) obtains and the ZIF-67 that step (2) obtains among ethyl alcohol ultrasonic mixing, drying composite；
(4) step (3) resulting mixture is calcined in oxygen atmosphere, calcining is completed to obtain metal oxide cladding
Nickel-cobalt-manganese ternary anode material for lithium-ion batteries.
2. preparation method according to claim 1, it is characterised in that: the nickel-cobalt-manganese ternary precursor material is
Ni0.8Co0.1Mn0.1(OH)2、Ni0.8Co0.1Mn0.1CO3、Ni0.6Co0.2Mn0.2(OH)2、Ni0.6Co0.2Mn0.2CO3、
Ni0.5Co0.2Mn0.3(OH)2、Ni0.5Co0.2Mn0.3CO3One of.
3. preparation method according to claim 1, it is characterised in that: the lithium salts is lithium hydroxide, lithium carbonate, lithium acetate
At least one of.
4. preparation method according to claim 1, it is characterised in that: calcination process described in step (1) be 500~
200~400min is kept the temperature at 600 DEG C, then is warming up to 750~850 DEG C of 600~900min of heat preservation, and whole heating rate is 1~3
℃/min。
5. preparation method according to claim 1, it is characterised in that: in step (2) solution A and B solution, ethyl alcohol and
The volume ratio of methanol is respectively 1:1~2:1.
6. preparation method according to claim 1, it is characterised in that: step (2) B solution and solution A are according to six water
The molar ratio of cobalt nitrate and 2-methylimidazole is closed as 1:1~1:16 mixing.
7. preparation method according to claim 1, it is characterised in that: in step (2), the B solution is poured into solution A
And stir 2~10min, later stand 22~for 24 hours, be then centrifuged.
8. preparation method according to claim 1, it is characterised in that: ZIF-67 accounts for NCM's in step (3) described mixture
Weight ratio is 0.5%~5%.
9. preparation method according to claim 1, it is characterised in that: calcination temperature described in step (4) is 700~800
DEG C, calcination time is 4~6h, and heating rate is 1~3 DEG C/min.
10. a kind of nickel-cobalt-manganese ternary lithium of the metal oxide cladding by the preparation method preparation of any one of claim 1~9
Ion battery positive electrode.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111924894A (en) * | 2020-07-03 | 2020-11-13 | 东莞东阳光科研发有限公司 | High-nickel ternary cathode material and preparation method thereof |
| WO2020258554A1 (en) * | 2019-06-24 | 2020-12-30 | 浙江天能能源科技股份有限公司 | Mof derivative-coated ncm ternary positive electrode material and preparation method therefor |
| CN112186167A (en) * | 2020-10-28 | 2021-01-05 | 陕西彩虹新材料有限公司 | Preparation method of template-method-coated high-nickel ternary cathode material for lithium ion battery |
| CN112661205A (en) * | 2020-12-31 | 2021-04-16 | 格林美股份有限公司 | Multi-oxide-coated ternary lithium ion battery positive electrode material and preparation method thereof |
| CN113428912A (en) * | 2021-08-26 | 2021-09-24 | 蜂巢能源科技有限公司 | Quaternary positive electrode material and preparation method and application thereof |
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| CN114744181A (en) * | 2022-05-17 | 2022-07-12 | 蜂巢能源科技股份有限公司 | Cobalt-free cathode material and preparation method and application thereof |
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| WO2020258554A1 (en) * | 2019-06-24 | 2020-12-30 | 浙江天能能源科技股份有限公司 | Mof derivative-coated ncm ternary positive electrode material and preparation method therefor |
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| CN113823794A (en) * | 2021-08-04 | 2021-12-21 | 北京泰和九思科技有限公司 | Method for modifying positive electrode material coated by organic metal framework based polymer electrolyte |
| CN113428912A (en) * | 2021-08-26 | 2021-09-24 | 蜂巢能源科技有限公司 | Quaternary positive electrode material and preparation method and application thereof |
| CN113428912B (en) * | 2021-08-26 | 2022-02-18 | 蜂巢能源科技有限公司 | Quaternary positive electrode material and preparation method and application thereof |
| CN113955809A (en) * | 2021-12-20 | 2022-01-21 | 河南科隆新能源股份有限公司 | Nickel-cobalt-manganese-lithium aluminate positive electrode material with shell-core structure and preparation method thereof |
| CN113955809B (en) * | 2021-12-20 | 2022-03-11 | 河南科隆新能源股份有限公司 | Nickel-cobalt-manganese-lithium aluminate positive electrode material with shell-core structure and preparation method thereof |
| CN114583120A (en) * | 2021-12-27 | 2022-06-03 | 武汉理工大学 | Method for designing and constructing gradient structure with metal ion component on surface of lithium-rich material |
| CN114744181A (en) * | 2022-05-17 | 2022-07-12 | 蜂巢能源科技股份有限公司 | Cobalt-free cathode material and preparation method and application thereof |
| CN114744181B (en) * | 2022-05-17 | 2024-01-30 | 蜂巢能源科技股份有限公司 | Cobalt-free positive electrode material and preparation method and application thereof |
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Application publication date: 20190521 |