CN108682795A - A kind of ternary cathode material of lithium ion battery surface acid-washing cladding TiO2Method - Google Patents

A kind of ternary cathode material of lithium ion battery surface acid-washing cladding TiO2Method Download PDF

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CN108682795A
CN108682795A CN201810266455.6A CN201810266455A CN108682795A CN 108682795 A CN108682795 A CN 108682795A CN 201810266455 A CN201810266455 A CN 201810266455A CN 108682795 A CN108682795 A CN 108682795A
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cathode material
tio
lithium ion
titanium sulfate
saturation
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CN108682795B (en
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王庆莉
李道聪
楚雄
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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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
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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

Abstract

The invention discloses a kind of ternary cathode material of lithium ion battery surface acid-washings to coat TiO2Method, be related to technical field of lithium ion, include the following steps：Titanium sulfate acyl and sulfuric acid are dissolved in deionized water, saturation titanium sulfate acyl solution is prepared；Tertiary cathode material is added in saturation titanium sulfate acyl solution, ultrasonic mixing forms suspension, suspension is continued to stir, until suspension lighter, obtains tan precipitate, filters, and with ethanol wash, vacuum drying obtains dried material；Dried material is placed in Muffle furnace and is heat-treated, then furnace cooling, obtains TiO2The tertiary cathode material of cladding.The present invention carries out surface modification by controllable pickling cladding process to tertiary cathode material, and while reducing ternary material surface residual alkali, uniform TiO is formed on surface2Clad, the water absorption character that can be effectively improved in first charge discharge efficiency, discharge capacity, cyclical stability and the storing process of ternary material have huge application value.

Description

A kind of ternary cathode material of lithium ion battery surface acid-washing cladding TiO2Method
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of ternary cathode material of lithium ion battery surface acids Wash bags cover TiO2Method.
Background technology
Ternary layered oxide material is because of its height ratio capacity, low cost and advantages of environment protection, by as lithium ion Cell positive material is largely used to portable equipment, electric vehicle and energy storage field.But its poor thermal stability, stable circulation Property and storge quality significantly limit its large-scale application in practical applications there is some potential safety problems.
Thermal stability, cyclical stability and the storge quality of commercial nickel-cobalt-manganese ternary material difference are largely due to now Batch production technique cause ternary material surface to there are largely free lithiums, be easy to and H in air2O and CO2Reaction, in material table Face generates LiOH and Li2CO3, lead to material pH value and surface residual alkali too high levels.LiOH can be with the LiPF in electrolyte6Reaction Generate HF, Li2CO3High-temperature storage can be caused to generate serious inflatable, seriously affect the chemical property of material, while causing to pacify Full hidden danger.
It is a large amount of real although the residual alkali of material surface can be efficiently reduced to tertiary cathode material washing in the prior art The material tested after showing washing resists H in air2O/CO2Ability decline.Simultaneously processed to material progress wet method cladding Cheng Zhong, the exposed region that material surface is not wrapped by are similar to the material after washing, these regions are excessive, the cycle performance of material It will deteriorate.In addition, existing washing or cladding process are uncontrollable due to washing and coating process, lattice defect, packet are easily caused It covers uneven, the discharge capacity of tertiary cathode material is caused to reduce, micro-crack is more also easy to produce in storage and discharge process, material Stability and storge quality are not improved.
Invention content
Technical problems based on background technology, the present invention propose a kind of ternary cathode material of lithium ion battery surface Pickling coats TiO2Method, solve existing batch production technique and cause the pH value on tertiary cathode material surface excessively high, surface residual alkali Content is high and washes caused lattice defect in cladding process, the non-uniform problem of cladding.
A kind of ternary cathode material of lithium ion battery surface acid-washing proposed by the present invention coats TiO2Method, including it is following Step：
S1, titanium sulfate acyl and sulfuric acid are dissolved in deionized water, prepare saturation titanium sulfate acyl solution；
S2, tertiary cathode material is added in saturation titanium sulfate acyl solution, ultrasonic mixing forms suspension, by suspension Lasting stirring filters until suspension lighter, obtains tan precipitate, and with ethanol wash, vacuum drying obtains dried material；
S3, it dried material is placed in Muffle furnace is heat-treated, then furnace cooling obtains TiO2The ternary of cladding is just Pole material.
Preferably, in the S1,1-1.2 parts of titanium sulfate acyls and 60-100 parts of 1mol/L sulfuric acid are dissolved in 2000 parts of deionizations The titanium sulfate acyl solution of saturation is equipped in water.
Preferably, in the S2, tertiary cathode material is added in saturation titanium sulfate acyl solution, ultrasonic mixing 25- 40min forms suspension, and suspension is continued to stir 0.5-5h, until suspension lighter, obtains tan precipitate, is filtered, With ethanol wash, it is dried in vacuo 6-10h at 65-75 DEG C, obtains dried material.
Preferably, in the S2, tertiary cathode material is nickle cobalt lithium manganate LiNixCoyMn1-x-yO2, wherein 0.6≤x<1,0 <y≤0.2。
Preferably, in the S2, the addition of tertiary cathode material ensures the TiO that reaction generates2Quality accounting for ternary just The 0.1-10% of pole quality of materials.
Preferably, in the S3, heat treatment operation is as follows：In air atmosphere, it is warming up to 150-200 DEG C with 2 DEG C/min, 1.5-2h is kept the temperature, then 450-500 DEG C is warming up to 5 DEG C/min, keeps the temperature 5-8h, furnace cooling obtains TiO2The ternary of cladding is just Pole material.
Preferably, the saturation titanium sulfate acyl solution can also be saturation titanyl nitrate solution, the saturation titanyl nitrate Titanyl nitrate and nitric acid are dissolved in deionized water by solution to be formulated.
Advantageous effect：The present invention is reacted using titanium sulfate acyl (or titanyl nitrate) reversible hydrolysis,Saturation titanium sulfate acyl (or titanyl nitrate) solution is prepared, and is led to The amount that sulfuric acid (nitric acid) is added in control is crossed, while reducing nickel-cobalt-manganese ternary material surface residual alkali, hydrolysis is promoted to send out to the right It is raw, in its Surface Creation metatitanic acid, then again by the processing such as being filtered, washed, drying, be sintered after, formation coated with uniform TiO2Ternary material, avoid and side reaction and the non-uniform situation of cladding occur during wet method cladding.In addition, passing through control Pickling time processed can achieve the purpose that regulate and control coating thickness.The present invention by controllable pickling cladding process to ternary just Pole material carries out surface modification, and while reducing ternary material surface residual alkali, uniform TiO is formed on surface2Clad can have Effect improves the first charge discharge efficiency, discharge capacity, cyclical stability of ternary material, promotes ternary material and resists CO in air2And H2O Ability, in the actual production process, have huge application value.
Description of the drawings
Fig. 1 is the principle schematic that present invention saturation titanium sulfate acyl solution acid wash bags cover process；
Fig. 2 is that tertiary cathode material surface acid-washing coats TiO in the embodiment of the present invention 22Preceding and cladding TiO2SEM figures afterwards.
Specific implementation mode
Fig. 1 is the principle schematic that present invention saturation titanium sulfate acyl solution acid wash bags cover process.It can be seen from the figure that three There is largely free lithium in first positive electrode surface, it is easy to H in air2O and CO2Reaction, material surface generate LiOH and Li2CO3, lead to material pH value and surface residual alkali too high levels.Pickling, a side are carried out using the sulfuric acid solution of saturation titanium sulfate acyl Sulfuric acid in the solution of face and LiOH and Li2CO3Neutralization reaction occurs, reduces material surface residual alkali content, meanwhile, promote titanium sulfate The reaction of acyl reversible hydrolysis occurs to the right, and uniform cladding is formed in material surface in its Surface Creation metatitanic acid, then through subsequent processing TiO2Ternary material, avoid and side reaction and the non-uniform situation of cladding occur during wet method cladding.
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of ternary cathode material of lithium ion battery surface acid-washing proposed by the present invention coats TiO2Method, including it is following Step：
S1,1 part of titanium sulfate acyl and 60 parts of 1mol/L sulfuric acid are dissolved in the titanium sulfate that saturation is equipped in 2000 parts of deionized waters Acyl solution；
S2, by 5 parts of tertiary cathode material LiNi0.85Co0.1Mn0.05O2It is added in saturation titanium sulfate acyl solution, ultrasonic mixing 30min is uniformly mixed, and forms suspension, and suspension is continued to stir 0.5-1h, until suspension lighter, it is heavy to obtain brown It forms sediment, filters, with ethanol wash 3 times, be dried in vacuo 6h at 65 DEG C, obtain dried material；
S3, dried material is placed on porcelain boat, is put into Muffle furnace and is heat-treated, in air atmosphere, with 2 DEG C/min 150 DEG C are warming up to, 1.5h is kept the temperature, then 450 DEG C are warming up to 5 DEG C/min, keeps the temperature 5h, furnace cooling obtains TiO2The three of cladding First positive electrode.
To TiO obtained in the present embodiment2The tertiary cathode material of cladding is detected.After testing, surface Ti elements Content is few, and Ti constituent contents are about 0.2wt% or so, and ternary electrode material surface pH is greatly reduced, volume change unobvious, But cyclical stability is improved, and 1C recycles 100 capacity and reaches 190mAh/g.This explanation, at TiO (OH)2Have under colloidal sol protection While effect reduces surface residual alkali, avoids wet method cladding process and side reaction occurs.Since pickling time is short, final TiO2Selection Property cladding, it can be seen that particle surface has apparent thin spot under scanning electron microscope.
Embodiment 2
A kind of ternary cathode material of lithium ion battery surface acid-washing proposed by the present invention coats TiO2Method, including it is following Step：
S1,1 part of titanium sulfate acyl and 60 parts of 1mol/L sulfuric acid are dissolved in the titanium sulfate that saturation is equipped in 2000 parts of deionized waters Acyl solution；
S2, by 5 parts of tertiary cathode material LiNi0.85Co0.1Mn0.05O2It is added in saturation titanium sulfate acyl solution, ultrasonic mixing 30min is uniformly mixed, and forms suspension, and suspension is continued to stir 4h, until suspension lighter, obtains tan precipitate, It filters, with ethanol wash 3 times, is dried in vacuo 6h at 70 DEG C, obtains dried material；
S3, dried material is placed on porcelain boat, is put into Muffle furnace and is heat-treated, in air atmosphere, with 2 DEG C/min 150 DEG C are warming up to, 1.5h is kept the temperature, then 500 DEG C are warming up to 5 DEG C/min, keeps the temperature 5h, furnace cooling obtains TiO2The three of cladding First positive electrode.
To TiO obtained in the present embodiment2The tertiary cathode material of cladding is detected.After testing, surface Ti elements Content is about 2wt%, and ternary electrode material surface pH is greatly reduced, and capacity and cyclical stability are improved, and Fig. 2 is ternary The front and back SEM of positive electrode cladding compares photo, it is as can be seen from the figure coated after material granule surface is more compact, surface becomes It obtains smoothly, can detect that Ti elements are uniformly distributed from EDS Elemental redistributions.
Embodiment 3
A kind of ternary cathode material of lithium ion battery surface acid-washing proposed by the present invention coats TiO2Method, including it is following Step：
S1,1 part of titanyl nitrate and 100 parts of 1mol/L nitric acid are dissolved in the Nitric Acid Oxidation that saturation is equipped in 2000 parts of deionized waters Titanium solution；
S2, by 10 parts of tertiary cathode material LiNi0.85Co0.1Mn0.05O2It is added in saturation titanyl nitrate solution, ultrasonic mixing 30min is uniformly mixed, and forms suspension, and suspension is continued to stir 2h, until suspension lighter, obtains tan precipitate, It filters, with ethanol wash 3 times, is dried in vacuo 6h at 75 DEG C, obtains dried material；
S3, dried material is placed on porcelain boat, is put into Muffle furnace and is heat-treated, in air atmosphere, with 2 DEG C/min 150 DEG C are warming up to, 1.5h is kept the temperature, then 500 DEG C are warming up to 5 DEG C/min, keeps the temperature 5h, furnace cooling obtains TiO2The three of cladding First positive electrode.
To TiO obtained in the present embodiment2The tertiary cathode material of cladding is detected.After testing, surface Ti elements Content is about 0.2wt%, and pH is greatly reduced, and capacity and cyclical stability are improved, 0.1C, 1C, 2C discharge capacity up to 215, 198 and 192mAh/g, 0.1C head effects recycle 100 capacity retention ratios up to 98.5% up to 92.1%.From the SEM photograph after cladding In it can be seen that particle surface is more compact, surface is smoothened, can detect that Ti elements are uniformly distributed from EDS Elemental redistributions. Compare Examples 1 and 2, and the pickling covered effect of the embodiment is more preferable, this oxidisability for being possible as dust technology is compared Dilute sulfuric acid is weaker, influences smaller to ternary material particle surface.
Embodiment 4
A kind of ternary cathode material of lithium ion battery surface acid-washing proposed by the present invention coats TiO2Method, including it is following Step：
S1,1.2 parts of titanium sulfate acyls and 100 parts of 1mol/L sulfuric acid are dissolved in the sulfuric acid that saturation is equipped in 2000 parts of deionized waters Titanium acyl solution；
S2, by 6 parts of tertiary cathode material LiNi0.85Co0.1Mn0.05O2It is added in saturation titanium sulfate acyl solution, ultrasonic mixing 25min is uniformly mixed, and forms suspension, and suspension is continued to stir 3.5h, until suspension lighter, it is heavy to obtain brown It forms sediment, filters, with ethanol wash 3 times, be dried in vacuo 8h at 65 DEG C, obtain dried material；
S3, dried material is placed on porcelain boat, is put into Muffle furnace and is heat-treated, in air atmosphere, with 2 DEG C/min 180 DEG C are warming up to, 1.5h is kept the temperature, then 480 DEG C are warming up to 5 DEG C/min, keeps the temperature 7h, furnace cooling obtains TiO2The three of cladding First positive electrode.
Embodiment 5
A kind of ternary cathode material of lithium ion battery surface acid-washing proposed by the present invention coats TiO2Method, including it is following Step：
S1,1 part of titanium sulfate acyl and 60 parts of 1mol/L sulfuric acid are dissolved in the titanium sulfate that saturation is equipped in 2000 parts of deionized waters Acyl solution；
S2, by 5 parts of tertiary cathode material LiNi0.85Co0.1Mn0.05O2It is added in saturation titanium sulfate acyl solution, ultrasonic mixing 40min is uniformly mixed, and forms suspension, and suspension is continued to stir 5h, until suspension lighter, obtains tan precipitate, It filters, with ethanol wash 3 times, is dried in vacuo 10h at 70 DEG C, obtains dried material；
S3, dried material is placed on porcelain boat, is put into Muffle furnace and is heat-treated, in air atmosphere, with 2 DEG C/min 200 DEG C are warming up to, 2h is kept the temperature, then 490 DEG C are warming up to 5 DEG C/min, keeps the temperature 8h, furnace cooling obtains TiO2The ternary of cladding Positive electrode.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (7)

1. a kind of ternary cathode material of lithium ion battery surface acid-washing coats TiO2Method, which is characterized in that including following step Suddenly：
S1, titanium sulfate acyl and sulfuric acid are dissolved in deionized water, prepare saturation titanium sulfate acyl solution；
S2, tertiary cathode material is added in saturation titanium sulfate acyl solution, ultrasonic mixing forms suspension, suspension is continued Stirring filters until suspension lighter, obtains tan precipitate, and with ethanol wash, vacuum drying obtains dried material；
S3, it dried material is placed in Muffle furnace is heat-treated, then furnace cooling obtains TiO2The tertiary cathode material of cladding Material.
2. ternary cathode material of lithium ion battery surface acid-washing according to claim 1 coats TiO2Method, feature exists In, in the S1, by 1-1.2 parts of titanium sulfate acyls and 60-100 parts of 1mol/L sulfuric acid be dissolved in 2000 parts of deionized waters be equipped be saturated Titanium sulfate acyl solution.
3. ternary cathode material of lithium ion battery surface acid-washing according to claim 1 coats TiO2Method, feature exists In, in the S2, tertiary cathode material is added in saturation titanium sulfate acyl solution, ultrasonic mixing 25-40min forms suspension, Suspension is continued to stir 0.5-5h, until suspension lighter, tan precipitate is obtained, filters, with ethanol wash, in 65- It is dried in vacuo 6-10h at 75 DEG C, obtains dried material.
4. ternary cathode material of lithium ion battery surface acid-washing according to claim 1 coats TiO2Method, feature exists In in the S2, tertiary cathode material is nickle cobalt lithium manganate LiNixCoyMn1-x-yO2, wherein 0.6≤x<1,0<y≤0.2.
5. ternary cathode material of lithium ion battery surface acid-washing according to claim 1 coats TiO2Method, feature exists In in the S2, the addition of tertiary cathode material ensures the TiO that reaction generates2Quality account for tertiary cathode material quality 0.1-10%.
6. ternary cathode material of lithium ion battery surface acid-washing according to claim 1 coats TiO2Method, feature exists In in the S3, heat treatment operation is as follows：In air atmosphere, it is warming up to 150-200 DEG C with 2 DEG C/min, keeps the temperature 1.5-2h, It is warming up to 450-500 DEG C with 5 DEG C/min again, keeps the temperature 5-8h, furnace cooling obtains TiO2The tertiary cathode material of cladding.
7. coating TiO according to any ternary cathode material of lithium ion battery surface acid-washings of claim 1-62Method, It is characterized in that, the saturation titanium sulfate acyl solution can also be saturation titanyl nitrate solution, and the saturation titanyl nitrate solution is Titanyl nitrate and nitric acid be dissolved in and is formulated in deionized water.
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CN112993258A (en) * 2021-05-12 2021-06-18 蜂巢能源科技有限公司 Doping and coating method of ternary cathode material, ternary cathode material and lithium ion battery
CN113461072A (en) * 2021-06-29 2021-10-01 贝特瑞（江苏）新材料科技有限公司 Method and device for processing anode material and lithium ion battery
CN113522868A (en) * 2021-06-29 2021-10-22 格林美（无锡）能源材料有限公司 Washing method for removing residual alkali on surface of positive electrode material
CN113461072B (en) * 2021-06-29 2023-10-24 贝特瑞（江苏）新材料科技有限公司 Method and device for processing positive electrode material and lithium ion battery

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