CN104733714B - Modification method of lithium ion battery cathode material - Google Patents
Modification method of lithium ion battery cathode material Download PDFInfo
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- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a surface modification method of a lithium ion battery cathode material lithium manganate. The method comprises the steps of implanting a coating material into a surface layer of the lithium manganate body material by virtue of the bombardment of high-speed particle beams. The surface modification method is good in coating uniformity, and the coating thickness is controllable. The electrochemical performance test shows that the lithium manganate cathode material with the surface modified by adopting the high-speed particle injection method is high in cycling stability and obviously high in high-temperature performance.
Description
Technical field
The invention belongs to a kind of technical field of lithium ion battery positive pole material preparation, and in particular to a kind of lithium manganate cathode material
The method of modifying of material.
Background technology
LiMn2O4 (LiMn2O4) as anode material for lithium-ion batteries, platform voltage height (3.9- simple with synthesis
4.1V), material itself is nontoxic, safety, overcharge resistance performance can preferably the advantages of, raw material promoter manganese is abundant, cheap in addition, makes
Which becomes the ideal chose of power battery anode material.At present, manganate cathode material for lithium is primarily present under hot conditionss and stores, follows
The problems such as ring poor-performing and serious capacity attenuation.Cause capacitance loss factor mainly including John-teller distortion,
The oxygen defect of manganese loss by dissolution, the decomposition of electrolyte and presence in the electrolytic solution, these changes cause lattice unstability, granule point
Split and electrochemical dissolution, cause LiMn2O4 to be difficult to form industrialization.
It is main at present to be modified come the cycle performance for improving LiMn2O4 by doping and surface.Wherein, wrap on LiMn2O4 surface
The material (metal-oxide, compound containing Li, polymer, metal, fluoride etc.) that one layer of anti-electrolyte corrodes is covered, one layer is formed
Li is allowed only+Pass freely through, and H+With the impenetrable film of electrolyte, corrosion function of the electrolyte to its surface can be weakened, be suppressed
The dissolving of LiMn2O4 surface Mn, so as to improve its cyclical stability.
United States Patent (USP) US5705291 A is disclosed using boric acid H3BO3Or oxidation boron2O3Cladding LiMn2O4, significantly improves
High-temperature storage performance.
Chinese patent 200410027362.6 is disclosed in LiMn2O4 Surface coating LiCoO2, to improve LiMn2O4 body material
The cyclical stability and high-temperature behavior of material.
CN103746109A discloses a kind of method of liquid phase method coated lithium ion battery positive-material lithium manganate, by metal
The acid salt of oxide is made into liquid, carries out high-speed stirred and obtains colloidal sol, then by colloidal sol according to LiMn2O4 and metal-oxide acid
Be added in the dispersant and chelating agen of high-speed stirred after the mixing of formula salt, be sufficiently mixed the mixture that obtains be dried it is broken sieve,
Double sintering, sintering is divided to finish rear furnace cooling, crushed 400 mesh sieves in the air stream in the mixture after sieving.
CN103456942A is also the liquid-coating method for adopting.
CN104134793A discloses the preparation method of lithium cell anode material lithium manganate, carries out according to the following steps：
1. kernel LiMn2O4 is prepared, doping vario-property LiMn2O4 is 2. prepared, is 3. mixed, be 4. spray-dried, 5. sintered, the granule kernel for obtaining
For LiMn2O4, top layer coating-doping modified lithium manganate, coating thickness is 200-400nm.
CN103172120A discloses a kind of method for preparing anode material of lithium-ion battery of coated Si, by LiMn2O4 matrix
Surface passes through chemical precipitation coated Si O2.H2O, carries out precipitation, treats that silicon precipitation is fully washed to the slip that discharges after completion of the reaction
Wash, after solid-liquid separation, after being dried coated silica manganate cathode material for lithium.
In sum, the surface of LiMn2O4 is modified generally adopts liquid phase or wet chemical method (such as sol-gel process, coprecipitated
Shallow lake method, polymerization, electroless plating method), covering material is dispersed in into LiMn2O4 bulk material surface, is then passed through again at follow-up heat
Reason, realizes the cladding of LiMn2O4.In many surface modifying methods, concordance and the uniformity for coating how is controlled, and
Stability in commercial process, is to realize that lithium manganate material moves towards the key technology of industrialization production.
The content of the invention
Present invention aim to address the circulation that exists of existing manganate cathode material for lithium unstable, high-temperature behavior is poor asks
Topic, and overcome the deficiencies in the prior art, there is provided a kind of surface modifying method of LiMn2O4 and modified lithium manganate cathode material
Material.
The present invention provides a kind of preparation method of modified lithium ion battery mangaic acid lithium anode material, it is characterised in that include
Following step：Using particle injection method, covering material is implanted in by high velocity beam bombardment for the table of LiMn2O4 bulk material
In layer, the covering material is selected from metal-oxide or nitride.Correspondingly, a kind of modified lithium ion battery mangaic acid is also provided
Lithium anode material, which is made up of with metal-oxide or metal nitride LiMn2O4, wherein metal-oxide or nitride cladding
Or be implanted in the top layer of lithium manganate material.
The present invention adopts particle injection method, and covering material is implanted in LiMn2O4 bulk material by high velocity beam bombardment
Top layer in.
In described method of modifying, covering material includes metal, metallic compound, nonmetallic, nonmetallic compound.Gold
Category is selected from any one in aluminum, copper, zinc, nickel, platinum, gold, silver.Metallic compound is in metal-oxide, metal nitride
One kind.The one kind of metal-oxide in aluminium oxide, Zinc Oxide, magnesium oxide, titanium oxide, copper oxide.Metal nitride is selected
One kind from titanium nitride, nickel oxide.Nonmetallic one kind in carbon, conducting polymer.Nonmetallic compound is selected from dioxy
SiClx.
High-velocity particles is infused in be carried out under any one atmosphere or two kinds of atmosphere of argon, oxygen, nitrogen, ammonia,
It is preferred that the gaseous mixture of oxygen or ammonia, more preferred oxygen and ammonia, gas flow is 5-60sccm, air pressure 2 × 10-4～5 ×
10-4Pa.Temperature at 100-500 DEG C, preferred 150-200 DEG C.
Covering material thickness is 0.5-20nm, preferred 2-10nm.
Manganate cathode material for lithium may be selected from LiMn2O4 LiMn2O4, the LiMn2O4 LiM of cation dopingxMn2-xO4(wherein, M
Selected from Ge, Cr, Fe, Co, Ni, Zn, Al, Cu and Mg, 0 ＜ X≤0.5), anion doped LiMn2O4 LiMn2-xO4-yMy(its
In, the one kind of M in two kinds of elements of O and F, 0 ＜ X≤0.25,0 ＜ Y≤0.25), various cation dopings
LiM1xM2yMn2-x-yO4(wherein, M1, M2 any one in Ge, Cr, Fe, Co, Ni, Zn, Al, Cu, Mg, 0 ＜ X≤0.25,
0 ＜ Y≤0.25), and the LiMn2O4 of Anion-cation multiple dope.
The present invention also provides a kind of electrode containing the manganate cathode material for lithium.
The present invention also provides a kind of energy storage elements containing described electrode, the preferred lithium ion of the energy storage elements
Battery.
The present invention also provides a kind of portable electric appts containing the energy storage elements, the portable electric appts
It is preferred that mobile phone, photographing unit, video camera, MP3, MP4, notebook computer.
The present invention is had the advantage that compared with prior art：Being evenly coated property is preferable, and it is controllable to coat thickness.Obtain
Preferably, electrochemical property test shows manganate cathode material for lithium concordance, carries out what surface was modified using high-velocity particles injection method
Manganate cathode material for lithium, especially its cyclical stability, high-temperature behavior are significantly improved.
Description of the drawings
Fig. 1 is the SEM stereoscan photograph of lithium manganate material bulk material obtained in the present invention.
Fig. 2 is modified lithium manganate material SEM stereoscan photograph obtained in the embodiment of the present invention 1.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but the present invention is not limited to following examples.Under
Experimental technique described in embodiment is stated, if no special instructions, conventional method is；The reagent and material, if no special instructions,
Commercially obtain.
The chemical property of the manganate cathode material for lithium prepared using the method for the invention for test, has carried out manganese first
The preparation of sour lithium bulk material：According to Li：Mn mol ratios 0.55 weigh LiNO3And MnCl2, stirring is made into after being dissolved in water, obtains clear
Clear solution, adds HNO3PH value is adjusted in 2-2.5.Then it is spray-dried, obtains manganate precursor for lithium.By the presoma in Muffle
In stove, 750 DEG C of calcining 10h, obtain LiMn2O4 bulk material (as shown in Figure 1).Secondly, using high-velocity particles injection method, to LiMn2O4
Bulk material has carried out surface and has been modified, and concrete preparation process is as shown in embodiment 1-4.Finally, by the LiMn2O4 in the present invention just
Pole material and binding agent Kynoar (PVDF) and N-Methyl pyrrolidone (NMP) are according to 9:0.5:0.5 ratio stirring is mixed
Synthesis uniform sizing material, is coated in aluminium foil surface, after drying, section, obtains positive plate；Made to electrode, electricity using metal lithium sheet
Solution liquid is 1M LiFP6Ethylene carbonate (EC), (volume ratio is 1 to dimethyl carbonate (DMC):1) solution, is assembled into button electricity
Pond.By the button cell for assembling respectively under the conditions of 25 DEG C and 55 DEG C, performance is circulated using Arbin battery test systems
Test.Charging and discharging currents are 1C, and it is 3.0V～4.3V that charging/discharging voltage is interval.The lithium manganate cathode prepared in the present embodiment
The cell testing results of material are listed in table 1.
Embodiment 1
The lithium manganate material of titanium-oxide-coated：The LiMn2O4 bulk material of preparation is put into into vacuum chamber, vacuum is evacuated to
Spend for 3 × 10-4Pa, is heated to 100 DEG C, with high-velocity particles bombardment Titanium (purity 99.9%), argon is first passed through in vacuum room,
Flow is 50sccm, then is passed through oxygen with the flow of 5sccm, and whole process continues 5min, obtains nano-titanium oxide cladding
Lithium manganate material (as shown in Figure 2).Covering material thickness is in 1-3nm.
Embodiment 2
The whole process for being passed through oxygen continues 10min, to control covering material thickness as 8-10nm, the other the same as in Example 1.
Embodiment 3
The lithium manganate material of oxide coated by zinc：The LiMn2O4 bulk material of preparation is put into into vacuum chamber, vacuum is evacuated to
Spend for 2 × 10-4Pa, is heated to 150 DEG C, and with high-velocity particles bombardment metallic zinc (purity 99.9%), argon is first passed through in vacuum room
Gas, flow are 50sccm, then are passed through oxygen with the flow of 5sccm, and whole process continues 3min, control coating thickness for 3-
5nm, obtains the lithium manganate material of nano zine oxide cladding.
Embodiment 4
Other conditions are same as Example 3, and difference is to be evacuated to vacuum for 3 × 10-4Pa, is heated to 180
DEG C, so that coating thickness is 1-3nm.
Embodiment 5
The lithium manganate material of alumina-coated：The LiMn2O4 bulk material of preparation is put into into vacuum chamber, vacuum is evacuated to
Spend for 3 × 10-4Pa, is heated to 150 DEG C, with high-velocity particles bombardment metallic aluminium (purity 99.9%), argon is first passed through in vacuum room,
Flow is 50sccm, then is passed through oxygen with the flow of 5sccm, and whole process continues 5min, and it is 1-3nm to control coating thickness,
Obtain the lithium manganate material of nano aluminium oxide cladding.
Embodiment 6
The lithium manganate material of titanium nitride cladding：The LiMn2O4 bulk material of preparation is put into into vacuum chamber, vacuum is evacuated to
Spend for 3 × 10-4Pa, is heated to 200 DEG C, with high-velocity particles bombardment Titanium (purity 99.9%), argon is first passed through in vacuum room,
Flow is 50sccm, then is passed through nitrogen with the flow of 5sccm, and whole process continues 5min, obtains Nano titanium nitride cladding
Lithium manganate material, covering material thickness is in 1-3nm.
Embodiment 7
The preparation of mg-doped LiMn2O4
Other conditions are with the identical of LiMn2O4 bulk material, difference are prepared in specific embodiment is to be only that
According to Li：Mn mol ratios 0.55 weigh LiNO3And MnCl2When, weigh LiNO3、MnCl2While, weigh LiNO3And MnCl2Always
The MgNO of weight 5%3。
Embodiment 8
The lithium manganate material of titanium-oxide-coated mg-doped
Other conditions are same as Example 1, the difference is that only and use the mg-doped LiMn2O4 prepared using embodiment 7,
Obtain the mg-doped LiMn2O4 of titanium-oxide-coated.
Comparative example 1
LiMn2O4 bulk material is immersed in the ethanol solution of 5% butyl titanate of 100ml, is added after stirring 1h
1ml water, then solution is heated into 6h at 100 DEG C, it is dried after natural cooling, obtains the LiMn2O4 of titanium-oxide-coated.
The cycle performance of 1 manganate cathode material for lithium of table is compared
From table 1 it follows that when manganate cathode material for lithium is using high-velocity particles injection method cladding nano-titanium oxide, oxidation
After the materials such as zinc, aluminium oxide and titanium nitride, cycle performance has lifting, and wherein high temperature cyclic performance is lifted substantially, wherein, cladding
The effect of titanium nitride is best.
Claims (13)
1. a kind of preparation method of modified lithium ion battery mangaic acid lithium anode material, it is characterised in that comprise the steps：Adopt
Particle injection method is used, covering material is implanted in the top layer of LiMn2O4 bulk material by high velocity beam bombardment, the bag
Material selected from metal oxide or metal nitride are covered, the thus obtained manganate cathode material for lithium is by LiMn2O4 and metal oxygen
Compound or metal nitride composition, wherein metal-oxide or metal nitride coat or are implanted in the top layer of lithium manganate material
In.
2. the method described in claim 1, it is characterised in that：High-velocity particles is infused in selected from argon, oxygen, nitrogen, ammonia
Carry out under any one atmosphere or two kinds of atmosphere；Gas flow is 5-60sccm, air pressure 2 × 10-4～5 × 10-4Pa。
3. the method described in claim 2, it is characterised in that：High-velocity particles is infused in any one gas selected from oxygen or ammonia
Carry out under atmosphere or two kinds of atmosphere.
4. the method described in claim 1, it is characterised in that：High-velocity particles implantation temperature is at 100-500 DEG C；The cladding material of preparation
Material thickness is 1-10nm.
5. the method described in claim 1, it is characterised in that：The metal-oxide of covering material is selected from aluminium oxide, Zinc Oxide, oxygen
Change the one kind in magnesium, titanium oxide, copper oxide；The one kind of metal nitride in titanium nitride, nickel oxide.
6. the method described in claim 1, it is characterised in that：Manganate cathode material for lithium is selected from：
LiMn2O4 LiMn2O4；
The LiMn2O4 LiM of cation dopingxMn2-xO4, wherein, M be selected from Ge, Cr, Fe, Co, Ni, Zn, Al, Cu and Mg, 0 ＜ X≤
0.5；
Anion doped LiMn2O4 LiMn2-xO4-yMy, wherein, the one kind of M in two kinds of elements of O and F, 0 ＜ X≤0.25,0
＜ Y≤0.25；
The LiM1 of various cation dopingsxM2yMn2-x-yO4, wherein, M1, M2 are in Ge, Cr, Fe, Co, Ni, Zn, Al, Cu, Mg
Any one, 0 ＜ X≤0.25,0 ＜ Y≤0.25；
And the LiMn2O4 of above-mentioned Anion-cation multiple dope.
7. a kind of method of modifying of lithium ion battery mangaic acid lithium anode material, it is characterised in that comprise the steps：Using particle
Injection method, is implanted in covering material in the top layer of LiMn2O4 bulk material by high velocity beam bombardment.
8. the method for modifying described in claim 7, it is characterised in that：High-velocity particles is infused in selected from argon, oxygen, nitrogen, ammonia
Carry out under any one atmosphere of gas or two kinds of atmosphere；Gas flow is preferably 5-60sccm, air pressure 2 × 10-4～5 × 10- 4Pa。
9. the method for modifying described in claim 7, it is characterised in that：High-velocity particles implantation temperature is at 100-500 DEG C；The bag of preparation
Material thickness is covered for 1-10nm.
10. the method for modifying described in claim 7, it is characterised in that：The metal-oxide of covering material is selected from aluminium oxide, oxidation
One kind in zinc, magnesium oxide, titanium oxide, copper oxide；The one kind of metal nitride in titanium nitride, nickel oxide.
Method of modifying described in 11. claim 7, it is characterised in that：
Manganate cathode material for lithium is selected from LiMn2O4 LiMn2O4；
The LiMn2O4 LiM of cation dopingxMn2-xO4, wherein, M be selected from Ge, Cr, Fe, Co, Ni, Zn, Al, Cu and Mg, 0 ＜ X≤
0.5；
Anion doped LiMn2O4 LiMn2-xO4-yMy, wherein, the one kind of M in two kinds of elements of O and F, 0 ＜ X≤0.25,0
＜ Y≤0.25；
The LiM1 of various cation dopingsxM2yMn2-x-yO4, wherein, M1, M2 are in Ge, Cr, Fe, Co, Ni, Zn, Al, Cu, Mg
Any one, 0 ＜ X≤0.25,0 ＜ Y≤0.25；
And the LiMn2O4 of above-mentioned Anion-cation multiple dope.
12. a kind of manganate cathode material for lithium, it is characterised in that prepared by claim 1 methods described.
13. a kind of energy storage elements, it is characterised in that containing a kind of electrode, the electrode contains the manganese described in claim 12
Sour lithium anode material.
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| CN109428063A (en) * | 2017-08-28 | 2019-03-05 | 内蒙古欣源石墨烯科技有限公司 | A kind of particle injection method prepares Si-C composite material and preparation method thereof |
| CN107994214B (en) * | 2017-11-14 | 2021-04-06 | 山东丰元化学股份有限公司 | High-performance lithium iron phosphate composite material and preparation method thereof |
| CN107968198B (en) * | 2017-11-24 | 2021-03-12 | 中国科学院过程工程研究所 | Nickel-cobalt lithium manganate precursor with core-shell structure, preparation method thereof and application of precursor in lithium ion battery |
| CN108448076A (en) * | 2018-02-09 | 2018-08-24 | 山东丰元化学股份有限公司 | The method of modifying of nickle cobalt lithium manganate trielement composite material |
| CN111430710B (en) * | 2020-03-17 | 2021-06-11 | 桂林电子科技大学 | Modified nickel cobalt lithium manganate ternary cathode material and preparation method and application thereof |
| CN117117161B (en) * | 2023-10-25 | 2024-01-23 | 浙江帕瓦新能源股份有限公司 | Modified lithium ion battery positive electrode material, preparation method thereof and lithium ion battery |
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| CN101060173B (en) * | 2006-04-19 | 2011-09-14 | 深圳市比克电池有限公司 | Complex Li-Mn-oxide, manufacture method and battery made of this material |
| CN100418256C (en) * | 2006-07-28 | 2008-09-10 | 中国科学院成都有机化学有限公司 | ZnO coated surface spinel type LiMnO positive electrode material and its preparation method |
| CN100503894C (en) * | 2006-12-21 | 2009-06-24 | 武汉科技大学 | Preparation method of high silicon orientation silicon steel thin plate |
| CN101475221A (en) * | 2008-11-26 | 2009-07-08 | 万向电动汽车有限公司 | Spinelle lithium manganate material for lithium ionic cell and preparation thereof |
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| CN103107337A (en) * | 2012-04-01 | 2013-05-15 | 湖南大学 | Method for improving cycling stability of lithium ion battery anode material |
| CN102723487A (en) * | 2012-06-20 | 2012-10-10 | 天津大学 | LiFePO4 cathode material of lithium ion battery compositely coated by TiN and C and preparation method thereof |
| CN102738454B (en) * | 2012-07-19 | 2015-04-29 | 北大先行科技产业有限公司 | Surface coating material for cathode material of lithium ion battery and preparation method |
| CN103107330A (en) * | 2013-02-18 | 2013-05-15 | 奇瑞汽车股份有限公司 | Preparation method of nitride coated lithium-rich cathode material |
| CN103811765B (en) * | 2014-02-27 | 2015-12-09 | 广西师范大学 | A kind of two-dimensional nano metal oxide composite coating manganate cathode material for lithium and preparation method thereof |
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