CN110492061A - A kind of method for coating of water-soluble additives auxiliary positive material interface growth boron aluminum oxide thin layer - Google Patents
A kind of method for coating of water-soluble additives auxiliary positive material interface growth boron aluminum oxide thin layer Download PDFInfo
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- CN110492061A CN110492061A CN201810462453.4A CN201810462453A CN110492061A CN 110492061 A CN110492061 A CN 110492061A CN 201810462453 A CN201810462453 A CN 201810462453A CN 110492061 A CN110492061 A CN 110492061A
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Abstract
The present invention discloses a kind of method for coating using a kind of water-soluble additives auxiliary positive material interface growth boron aluminum oxide thin layer, specifically: press boron raw material, aluminum feedstock, organic additive, the mass ratio of inorganic additive and positive electrode is that (0.001 ~ 1:0 ~ 1:0.0001 ~ 1:0.0001 ~ 1:1 ~ 50) weighs boron raw material, aluminum feedstock, organic additive, this three kinds of solids of inorganic additive coat raw material, weighed solid cladding raw material is mixed with liquid dispersant, it is completely dissolved, again plus positive electrode is configured to slurry, it is stirred for, filter (or centrifugation), it is dried to obtain the presoma of cladding, then in the case where handling atmosphere, annealing obtains the good positive electrode of boron aluminide covering property.The present invention effectively can carry out coated with uniform to positive electrode, improve the cyclical stability of positive electrode, which stablizes, and operating procedure is easy, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to field of lithium ion battery anode, are related specifically to a kind of water-soluble additives auxiliary positive material
Expect the method for interface Boron Coated aluminum oxide thin layer.
Background technique
Popularizing for power vehicle develops with the portability of 3C electronic product so as to high-energy, high power, long-life
The demand of lithium ion battery is increasingly urgent to.And layer structure class anode (such as LiCoO2, ternary material LiNixCoyMnzO2、
LiNixCoyAlzO2, rich lithium materialxLi2MnO3·(1-x)LiMO2Deng), spinel-type anode (LiMn2O4、LiNixMn2-xO4) and
Olivine-type anode (LiFePO4) with voltage, the raising of multiplying power, operating temperature, interface is easier to that irreversible side reaction occurs, and leads
Cause performance degradation.
In the technological invention for improving positive electrode interface stability, a kind of thinking is that the boron member of body phase is carried out to positive electrode
Element doping.For example, patent CN103296249A, in synthesis of ternary material, raw material adds B2O3, burn boron doped in 900 oC
Ternary material；For patent CN103413931B when synthesizing rich lithium material, raw material addition contains boron oxide compound, burns in 800-900 oC
Boron doped richness lithium material.Body phase boron doping is both advantageous and disadvantageous for the battery performance influence of positive electrode, is more common in academic exploration,
It is not used for actual production.The new approaches that another kind improves positive electrode interface performance are to carry out subsequent interface packet to positive electrode
It covers containing boron oxide compound.(Electrochim. Acta, 2015,174,1225) is in LiOHH for example, document2O and H3BO31:
LiNi is added in 2 mixed aqueous solutions0.5Co0.2Mn0.3O2Product, 80 oC are evaporated, then are calcined 500oC and obtained Li2O·2B2O3Cladding
LiNi0.5Co0.2Mn0.3O2Material；Document (J. Power Sources, 2017,362,131) is by LiCoO2Boric acid water
90 oC of solution is evaporated, then 500 oC burn to obtain B2O3The LiCoO of cladding2.Above-mentioned two reports, there is coating thicknesses not
, interfacial phase change caused by positive electrode heats too long in water phase, the high voltage capability of material are simultaneously not up to best.Patent
CN101359736 is directly LiOH, H3BO3It calcines to obtain mLi with ternary material ball milling, then 600-1000 oC2O·nB2O3Packet
The product covered.It is uneven with the mutually boron doped problem of body that the material faces clad simultaneously.Patent CN103236521A is by boracic
Neutral organic solution mixed with ternary material and ultrasound, then subsequent addition organic dispersing agent, be evaporated organic solvent through 70 oC,
Last 600-850 oC air calcination obtains the ternary material of Li-B-O cladding.In this method, additive helps to improve clad
Uniformity, but additive type selection and charging opportunity it is non-optimal, especially cladding operation is in neutral organic solvent
Middle long-time heating is completed, and interface is easily undergone phase transition, and process costs are high, and practical value is not high.
Around the above problem, the present invention passes through a kind of water-soluble additives auxiliary positive material interface boron aluminum oxide thin layer
Method for coating, on the basis of not damaging positive electrode interfacial structure and battery performance, water phase realizes that positive electrode interface is raw
Long thickness is controllable, is evenly coated, the adjustable boron aluminum oxide of doping component.
Summary of the invention
For the above goal of the invention, it is a kind of water-soluble additives auxiliary positive material that the present invention solves technical solution accordingly
Expect the method for coating of interface growth boron aluminum oxide thin layer, which comprises the following steps:
1. press boron raw material: aluminum feedstock: organic additive: inorganic additive: positive electrode mass ratio (0.001 ~ 1:0 ~ 1:
0.0001 ~ 1:0.0001 ~ 1:1 ~ 50) weigh this four kinds of solid bags of boron raw material, aluminum feedstock, organic additive, inorganic additive
Raw material is covered, weighed solid cladding raw material is mixed with liquid dispersant by the solid-to-liquid ratio of (0.00001 ~ 1) g/mL, it is completely molten
Solution obtains solution A, and the temperature of constant solution A is 0 ~ 80 oC；
2. by step, 1. middle mass ratio weighs positive electrode, and constant temperature (0 ~ 80 oC) stirs 0.5 ~ 12h after being added to solution A, then passes through
Filter (or centrifugation), 50 ~ 180 oC dry (vacuum drying or forced air drying) obtain cladding presoma；Presoma will be coated in heat
It handles in atmosphere and calcines 1 ~ 10h in 300 ~ 900 oC to get ultra-thin boron oxide compound cladded type positive electrode is arrived.
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer,
Be characterized in: boron raw material is boric acid, metaboric acid, diboron trioxide, one or more of mixing of Boratex in the 1. step.
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer,
Be characterized in: aluminum feedstock is aluminum nitrate, aluminium chloride, aluminum sulfate, one or more of mixing of aluminium acetate in the 1. step.
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer,
Be characterized in: organic additive is glucose, cassava ative starch, soluble starch, wheat ative starch, corn original in the 1. step
Starch, carboxymethyl starch, polyvinyl alcohol, citric acid, fructose, cetyl trimethylammonium bromide (CTAB), polyacrylamide
(PAM), polyvinylpyrrolidone (PVP), lauryl sodium sulfate (SDS), stearic acid, neopelex (SDBS)
One or more of mixing.
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer,
Be characterized in: inorganic additive is copper chloride, copper sulphate, zinc sulfate, zinc nitrate, lanthanum chloride, lanthanum sulfate, chlorination in the 1. step
Cerium, cerous nitrate, yttrium nitrate, ammonium metavanadate, lithium hydroxide, lithium carbonate, lithium chloride, lithium nitrate, sodium chloride, sodium sulphate, potassium chloride,
The mixing of one or more of potassium sulfate, sodium acetate, potassium acetate.
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer,
Be characterized in: dispersing agent is pure water and one or more of ethyl alcohol, methanol, ethylene glycol, isopropanol, glycerine in the 1. step
Mixing (volume ratio of the pure water in dispersing agent is not less than 50%).
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer,
Be characterized in: positive electrode is LiCoO in the 1. step2、LiNixCo1-x-yMnyO2 (0 ﹤ x ﹤ 1,0 ﹤ y ﹤ 1),
LiNixCoyAl1-x-yO2 (0.7 ﹤ x ﹤ 1,0 ﹤ y ﹤ 0.3),xLi2MnO3·(1-x)LiMO2、LiMn2O4 (0 ﹤ x ﹤ 1, M=Ni, Co,
Mn)。
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer,
Be characterized in: heat-treating atmosphere is air, oxygen (99.6% ~ 99.9%), one in high purity oxygen gas (99.99%) in the 2. step
Kind or several mixed gas.
Detailed description of the invention
Fig. 1 is the ultra-thin boron oxide compound cladding LiNi prepared in the embodiment of the present invention one0.5Co0.2Mn0.3O2Material
XRD figure.
Fig. 2 is the ultra-thin boron aluminum oxide cladding LiNi prepared in the embodiment of the present invention two0.5Co0.2Mn0.3O2Material
XRD figure；
Fig. 3 is the ultra-thin boron oxide compound cladding LiNi prepared in the embodiment of the present invention one0.5Co0.2Mn0.3O2The scanning electricity of material
Mirror low power figure:
Fig. 4 is the ultra-thin boron oxide compound cladding LiNi prepared in the embodiment of the present invention one0.5Co0.2Mn0.3O2The scanning electricity of material
Mirror high power figure:
Fig. 5 is the ultra-thin boron aluminum oxide cladding LiNi prepared in the embodiment of the present invention two0.5Co0.2Mn0.3O2The scanning of material
Electronic Speculum low power figure:
Fig. 6 is the ultra-thin boron aluminum oxide cladding LiNi prepared in the embodiment of the present invention two0.5Co0.2Mn0.3O2The scanning of material
Electronic Speculum high power figure:
Fig. 7 is the ultra-thin boron oxide compound cladding LiNi prepared in the embodiment of the present invention one0.5Co0.2Mn0.3O2The button electricity of material
Pond is in 0.1 C, 0.5 C, 1 C, 5 C, 10 C, the high rate performance figure under 0.1 C；
Fig. 8 is the ultra-thin boron oxide compound cladding LiNi prepared in the embodiment of the present invention one0.5Co0.2Mn0.3O2The button electricity of material
Cycle life figure of the pond at 1 C；
Fig. 9 is the ultra-thin boron aluminum oxide cladding LiNi prepared in the embodiment of the present invention four0.5Co0.2Mn0.3O2The button of material
Battery is in 0.1 C, 0.5 C, 1 C, 5 C, 10 C, the high rate performance figure under 0.1 C；
Figure 10 is the ultra-thin boron aluminum oxide cladding LiNi prepared in the embodiment of the present invention two0.5Co0.2Mn0.3O2The button of material
Battery cycle life figure at 1 C.
Specific embodiment
Embodiment 1
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
Be, comprising the following steps: weigh 0.9275g boric acid, 1g polyvinylpyrrolidone (PVP), by weighed solid cladding raw material with
The pure water of 100mL mixes, and is completely dissolved to obtain solution A, the temperature of constant solution A is 0 oC；10g is weighed again
LiNi0.5Co0.2Mn0.3O20 oC of constant temperature stirs 2h after being added to solution A, then is dried in vacuo before obtaining cladding through suction filtration, 120 oC
Drive body；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 500 oC of oxygen to get ultra-thin boron oxide compound cladded type is arrived just
Pole material.
Embodiment 2
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
It is, comprising the following steps: weigh 0.9275g boric acid, nine water aluminum nitrate of 0.0759g, 1g polyvinylpyrrolidone (PVP), will claim
The solid cladding raw material taken is mixed with the ethyl alcohol of 100mL, is completely dissolved to obtain solution A, the temperature of constant solution A is 25 oC；Again
Weigh 10g LiNi0.5Co0.2Mn0.3O20 oC of constant temperature stirs 2h after being added to solution A, then is dried in vacuo through suction filtration, 120 oC
To cladding presoma；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 500 oC of oxygen to get ultra-thin boron alumina is arrived
Object cladded type positive electrode.
Embodiment 3
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
It is, comprising the following steps: 0.9275g boric acid, nine water aluminum nitrate of 0.0918g, 1g soluble starch and 0.1g lanthanum chloride are weighed, it will
Weighed solid cladding raw material is mixed with the ethyl alcohol of 100mL, is completely dissolved to obtain solution A, the temperature of constant solution A is 0 oC；
10g LiNi is weighed again0.6Co0.2Mn0.2O20 oC of constant temperature stirs 2h after being added to solution A, then is filtered, 120 oC vacuum drying
Obtain cladding presoma；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 700 oC of oxygen to get ultra-thin boron alumina is arrived
Compound cladded type positive electrode.
Embodiment 4
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
It is, comprising the following steps: weigh 0.9275g boric acid, nine water aluminum nitrate of 0.0759g, 1g glucose and 0.1g yttrium nitrate, will weigh
Solid cladding raw material mix with the pure water of 100mL, be completely dissolved to obtain solution A, the temperature of constant solution A is 25 oC；Claim again
Take 10g LiNi0.8Co0.1Mn0.1O225 oC of constant temperature stirs 2h after being added to solution A, then is dried in vacuo through suction filtration, 120 oC
To cladding presoma；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 500 oC of oxygen to get ultra-thin boron alumina is arrived
Object cladded type positive electrode.
Embodiment 5
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
It is, comprising the following steps: weigh 0.9275g boric acid, 0.8g carboxymethyl starch and 0.08g sodium acetate, weighed solid is coated
Raw material is mixed with the pure water of 100mL, is completely dissolved to obtain solution A, the temperature of constant solution A is 25 oC；10g is weighed again
LiNi0.8Co0.1Mn0.1O225 oC of constant temperature stirs 2h after being added to solution A, then is dried in vacuo and is coated through suction filtration, 120 oC
Presoma；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 800 oC of oxygen to get ultra-thin boron oxide compound cladded type is arrived
Positive electrode.
Embodiment 6
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
It is, comprising the following steps: 0.9275g boric acid, nine water aluminum nitrate of 0.0607g, 1g cassava ative starch and 0.1g lanthanum sulfate are weighed, it will
Weighed solid cladding raw material is mixed with the pure water of 100mL, is completely dissolved to obtain solution A, the temperature of constant solution A is 0 oC；
10g LiNi is weighed again0.8Co0.15Al0.05O20 oC of constant temperature stirs 2h after being added to solution A, then dry through suction filtration, 120 oC vacuum
It is dry to obtain cladding presoma；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 450 oC of oxygen to get ultra-thin boron aluminium is arrived
Oxide cladded type positive electrode.
Embodiment 7
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
It is, comprising the following steps: weigh 0.9275g boric acid, nine water aluminum nitrate 0.0380g, 1g fructose and 0.1g ammonium metavanadate, will weigh
Solid cladding raw material mix with the ethyl alcohol of 100mL, be completely dissolved to obtain solution A, the temperature of constant solution A is 0 oC；Claim again
Take 10g LiNi0.8Co0.15Al0.05O20 oC of constant temperature stirs 2h after being added to solution A, then is dried in vacuo through suction filtration, 120 oC
To cladding presoma；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 500 oC of oxygen to get ultra-thin boron alumina is arrived
Object cladded type positive electrode.
Embodiment 8
According to a kind of method of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer, feature
It is, comprising the following steps: weigh 0.9275g boric acid, nine water aluminum nitrate of 0.0759g, 1g glucose and 0.1g yttrium nitrate, will claim
The solid cladding raw material taken is mixed with the pure water of 100mL, is completely dissolved to obtain solution A, the temperature of constant solution A is 0 oC；Again
Weigh 10g 0.5Li2MnO3·0.5Li0.44Co0.25Mn0.31O20 oC of constant temperature stirs 2h after being added to solution A, then filtered,
120 oC are dried in vacuo to obtain cladding presoma；Cladding presoma is homogeneously disposed in magnetic boat and calcines 2h in 500 oC of oxygen, i.e.,
Obtain ultra-thin boron aluminum oxide cladded type positive electrode.
The pioneering side reaction that the generation of positive electrode surface is reduced by preparing ultra-thin and uniform clad of the present invention, changes
Chemical stability of the material in charge and discharge process has been apt to it, the cyclical stability at 4.5 V of high voltage further increases.In view of
Operation of the present invention is simple, and covered effect is excellent, asepsis environment-protecting, it is easy to accomplish industrialized production.
Claims (5)
1. a kind of method for coating of water-soluble additives auxiliary positive material interface growth boron aluminum oxide thin layer, feature exist
In, comprising the following steps:
1. press boron raw material: aluminum feedstock: organic additive: inorganic additive: positive electrode mass ratio (0.001 ~ 1:0 ~ 1:
0.0001 ~ 1:0.0001 ~ 1:1 ~ 50) weigh this four kinds of solid bags of boron raw material, aluminum feedstock, organic additive, inorganic additive
Raw material is covered, weighed solid cladding raw material is mixed with liquid dispersant by the solid-to-liquid ratio of (0.00001 ~ 1) g/mL, it is completely molten
Solution obtains solution A, and the temperature of constant solution A is 0 ~ 80 oC；
2. by step, 1. middle mass ratio weighs positive electrode, and constant temperature (0 ~ 80 oC) stirs 0.5 ~ 12h after being added to solution A, then passes through
Filter (or centrifugation), 50 ~ 180 oC dry (vacuum drying or forced air drying) obtain cladding presoma；Presoma will be coated in heat
It handles in atmosphere and calcines 1 ~ 10h in 300 ~ 900 oC to get ultra-thin boron oxide compound cladded type positive electrode is arrived.
2. a kind of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer according to claim 1
Method, it is characterized in that: in the 1. step boron raw material be boric acid, metaboric acid, diboron trioxide, the one or more of Boratex
Mixing.
3. a kind of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer according to claim 1
Method, it is characterized in that: aluminum feedstock is aluminum nitrate, aluminium chloride, aluminum sulfate in the 1. step, the one or more of aluminium acetate are mixed
It closes.
4. a kind of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer according to claim 1
Method, it is characterized in that: in the 1. step organic additive be glucose, cassava ative starch, soluble starch, wheat original form sediment
Powder, native cornstarch, carboxymethyl starch, polyvinyl alcohol, citric acid, fructose, cetyl trimethylammonium bromide (CTAB), poly- third
Acrylamide (PAM), polyvinylpyrrolidone (PVP), lauryl sodium sulfate (SDS), stearic acid, neopelex
(SDBS) one or more of mixing.
5. a kind of water-soluble additives auxiliary positive material interface Boron Coated aluminum oxide thin layer according to claim 1
Method, it is characterized in that: in the 1. step inorganic additive be copper chloride, copper sulphate, zinc sulfate, zinc nitrate, lanthanum chloride, sulphur
Sour lanthanum, cerium chloride, cerous nitrate, yttrium nitrate, ammonium metavanadate, lithium hydroxide, lithium carbonate, lithium chloride, lithium nitrate, sodium chloride, sulfuric acid
The mixing of one or more of sodium, potassium chloride, potassium sulfate, sodium acetate, potassium acetate.
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| CN112599779A (en) * | 2020-12-15 | 2021-04-02 | 上海华谊（集团）公司 | Double-layer coated lithium ion battery anode material and preparation method thereof |
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