CN108199037A - A kind of nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping and preparation method thereof - Google Patents

A kind of nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping and preparation method thereof Download PDF

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Publication number
CN108199037A
CN108199037A CN201711421348.8A CN201711421348A CN108199037A CN 108199037 A CN108199037 A CN 108199037A CN 201711421348 A CN201711421348 A CN 201711421348A CN 108199037 A CN108199037 A CN 108199037A
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solution
doping
nickel cobalt
mixing
lithium aluminate
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CN108199037B (en
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许开华
李伟
徐世国
许国干
张玉军
刘钰
王星宁
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Greenmei (Hubei) new energy materials Co.,Ltd.
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Grammy (wuxi) Energy Materials Co Ltd
GEM Co Ltd China
Jingmen GEM New Material 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
    • H01M4/48—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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention is suitable for technical field of lithium batteries, a kind of nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping and preparation method thereof is provided, the method of the present invention is first using the burn in process for spraying saleratus solution and F solution, by the spherical pre-burning presoma of nickel cobalt lithium aluminate NCA presoma pre-fired porous honeycombs, then by Mg, Nb sources are configured to solution in proportion, after being mixed under the conditions of water system with pre-burning presoma, Mg, Nb solution is effectively imported by cellular hole in positive electrode base material inside, when high mixer batch mixing is used to mend lithium, sprinkling F ion adjusts agent solution again, so that material is sufficiently mixed uniformly, final high temperature is sintered, so that finished product crystallization, obtain zwitterion mixing and doping type nickel cobalt lithium aluminate cathode material；In the positive electrode, Nb4+ it can reduce cationic mixing, Mg3+ polarization can be reduced, enhance chemical property, therefore Mg3+/Nb4+ in charging process electrochemical reaction does not occur, variation of valence does not occur, stable crystal form structure can be played the role of, and oxygen can be consolidated by this anion doping of F, reducing oxygen is precipitated, stabilizing material structure, improves circulation ability.

Description

A kind of nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping and preparation method thereof
Technical field
The invention belongs to technical field of lithium batteries more particularly to a kind of nickel cobalt lithium aluminate anodes of zwitterion mixing and doping Material and preparation method thereof.
Background technology
Nickel cobalt lithium aluminate tertiary cathode material due to having higher energy density, widely applied to IT product and New-energy automobile field.But simple nickel cobalt lithium aluminate (LNCA) is since structural stability is poor, and nickel cobalt lithium aluminate has Cationic mixing, Ni easily occur for higher nickel content2+, the mutual occupy-places of Li+, hinder Li+ transmission and destroy material crystals knot Structure, and the reception and registration ability that Li+ is passed between crystal boundary is poor, and the cycle life and capacity for leading to material cause great harm.
Invention content
In view of the above problems, the purpose of the present invention is to provide a kind of nickel cobalt lithium aluminate anodes of zwitterion mixing and doping Material and preparation method thereof, it is intended to solve the cycle life of existing nickel cobalt lithium aluminate tertiary cathode material and the technology that capacity is poor Problem.
On the one hand, the preparation method of the nickel cobalt lithium aluminate cathode material of the zwitterion mixing and doping includes following steps Suddenly：
S1, pre-sintering step：
Nickel cobalt lithium aluminate presoma is weighed, and sprays a certain amount of saleratus solution and F solution, is then uniformly mixed, is turned Enter sintering furnace and first carry out low temperature presintering knot, be then rapidly heated, carry out a period of time high temperature pre-sintering, obtain the pre-burning of hole shape Presoma；
S2, cation doping step：
Certain density Nb solution and Mg solution is configured and mixes, weighs the pre-burning presoma of described hole shape, is stirred on side In the case of mixing side heating a period of time, pre-burning presoma is poured into Nb, Mg mixed solution, is uniformly mixed, obtains spare Sample；
S3, drying steps：
Processing is dried in the ready sample, obtains Nb, Mg doping precursor material；
S4, mixing material and anion doped step：
Nb, Mg doping precursor material is weighed, adds in lithium source according to certain lithium proportioning, together high merging high mixer In mixed, mixing sprays into a certain amount of F ion and adjusts agent solution simultaneously；
S5, sintering step：
The sample mixed is put into sintering oven, sintering temperature and sintering time are set, is passed through gas, sintering is completed Sample afterwards obtains the nickel cobalt lithium aluminate cathode material of the zwitterion mixing and doping after crossing and screening out iron.
On the other hand, the nickel cobalt lithium aluminate cathode material of the zwitterion mixing and doping is prepared by the above method, Components Chemical formula LixNi1-a-b-c-dCoaAlbMgcNbdO2-yFyIt represents, wherein 0.85≤x≤1.2,0≤a≤0.15,0≤b≤ 0.03,0.001≤c≤0.003,0.001≤d≤0.0003,0.001≤y≤0.005。
The beneficial effects of the invention are as follows：In preparation method of the present invention, use spraying saleratus solution and F solution is pre- first Firing method, by the spherical pre-burning presoma of nickel cobalt lithium aluminate NCA presoma pre-fired porous honeycombs, then by Mg, Nb Source is configured to solution in proportion, and after being mixed under the conditions of water system with pre-burning presoma, Mg, Nb solution have by cellular hole Effect is imported into positive electrode base material inside, then sprinkling F ion adjusts agent solution when high mixer batch mixing is used to mend lithium so that Material is sufficiently mixed uniformly, final high temperature sintering so that finished product crystallizes, and is obtaining zwitterion mixing and doping type nickel cobalt lithium aluminate just Pole material；In the positive electrode, Nb4+ it can reduce cationic mixing, Mg3+ polarization can be reduced, enhance chemical property, because This Mg3+/Nb4+ in charging process electrochemical reaction does not occur, variation of valence does not occur, the work of stable crystal form structure can be played With, and oxygen can be consolidated by this anion doping of F, reducing oxygen is precipitated, stabilizing material structure, improves circulation ability.
Description of the drawings
Fig. 1 is the preparation method flow chart of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping of the present invention；
Fig. 2 is that the embodiment of the present invention is pre-sintered presoma electron microscope；
Fig. 3 be the embodiment of the present invention obtain Mg, Nb, F ion mixing and doping type nickel cobalt lithium aluminate cathode material Electronic Speculum Figure；
Fig. 4 is the electrical property comparison diagram of lithium battery prepared by the embodiment of the present invention and comparative example.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.
As shown in Figure 1, the preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping provided by the invention Include the following steps：
S1, pre-sintering step：Nickel cobalt lithium aluminate presoma is weighed, and sprays a certain amount of saleratus solution and F solution, so After be uniformly mixed, be transferred to sintering furnace and first carry out low temperature presintering knot, be then rapidly heated, carry out a period of time high temperature pre-sintering, obtain To the pre-burning presoma of hole shape.
The mass percent concentration of the saleratus solution is 5%-10%, and fountain height accounts for the total matter of nickel cobalt lithium aluminate presoma The 1%-10% of amount, the mass percent concentration of the F solution is 0.2%-1.5%, and it is total that F solution accounts for nickel cobalt lithium aluminate presoma The 1%-5% of quality, the F solution are NH4F, NaF, MgF2In one kind；Sintering furnace low temperature presintering junction temperature is 300 DEG C, when Between for 2-5h, be then rapidly heated by 5-10 DEG C/min, high temperature pre-sintering carried out after being warming up to 600-800 DEG C, the time is 5-10h。
S2, cation doping step：Certain density Nb solution and Mg solution is configured and mixes, weighs described hole shape In the case where heating a period of time while stirring, pre-burning presoma is poured into Nb, Mg mixed solution for pre-burning presoma, It is uniformly mixed, obtains ready sample.
The mass percent concentration of the Nb solution and Mg solution is 0.05-3%, and pre-burning presoma is mixed with Nb, Mg The mass ratio of solution is 1：(5-20), whipping temp are 40-80 DEG C, mixing time 1-4h, and the Nb solution is nitric acid niobium, niobium One or more of acid, lithium niobate, fluorination niobium, sulfuric acid niobium, the Mg solution is magnesium nitrate, magnesium oxalate, magnesium chloride, magnesium sulfate Middle one or more.
S3, drying steps：Processing is dried in the ready sample, obtains Nb, Mg doping precursor material.
This step uses rotary evaporation drying process, and the ready sample is placed into Rotary Evaporators, is rotated Vacuum distillation, the temperature of Rotary Evaporators are set in 60-90 DEG C, rotational time 2-6h, by the completely rear gains of moisture evaporation Material is Nb, Mg doping precursor material.
S4, mixing material and anion doped step：Nb, Mg doping precursor material is weighed, is matched according to certain lithium Than adding in lithium source, mixed in high merging high mixer together, mixing sprays into a certain amount of F ion and adjusts agent solution simultaneously.
The mass percent concentration that the F ion adjusts agent solution is more than F solution in step S1, and F described here from Son adjusts the mass percent concentration 1-10% of agent solution, and it is NH that F ion, which adjusts agent solution,4F、NaF、MgF2In one kind, use Lithium source be Lithium hydroxide monohydrate, lithium carbonate, one or more of lithium chloride, lithium proportioning Li/Me is 1.0-1.2, here Me For the integral molar quantity of nickel cobalt aluminium manganese niobium, incorporation time 2-10min, rotating speed 500-1400rpm.
S5, sintering step：The sample mixed is put into sintering oven, sintering temperature and sintering time are set, are passed through Gas, the sample after the completion of being sintered obtain the nickel cobalt lithium aluminate anode of the zwitterion mixing and doping after crossing and screening out iron Material.Here sintering temperature is 500-800 DEG C, sintering time 10-25h, is passed through gas as air or oxygen.
The nickel cobalt lithium aluminate cathode material ingredient of the zwitterion mixing and doping finally obtained is nickel cobalt lithium aluminate；Its pattern For spherical shape.Its Components Chemical formula can use LixNi1-a-b-c-dCoaAlbMgcNbdO2-yFyIt represents, 0.85≤x≤1.2,0≤a ≤0.15,0≤b≤0.03,0.001≤c≤0.003,0.001≤d≤0.0003,0.001≤y≤0.005。
The present invention crosses the cation doping of Mg+Nb by mixing the appropriate mixing cation of Mg3+, Nb4+ and F anion Cationic mixing can be effectively reduced, and oxygen can be consolidated by this anion doping of F, reducing oxygen is precipitated, stabilizing material structure, Improve circulation ability.It is incorporated by the hole for carrying out cation to presoma in advance, then anionic surface half wet process adulterates, and mends The means that pyroreaction is adulterated after Li can cause the more uniform of element doping, more complete, the improvement effect of cycle of distribution Fruit can be better.The production method of this material is simple, raw material is easy to get, and can be easier to be transferred to industrialized production.
This product effect is verified below by specific embodiment and comparative example：
Embodiment：
1) 100g nickel cobalt lithium aluminate presomas are weighed, and spray 5% saleratus solution and 0.2% NH4F solution mixes It closes uniformly, is then transferred to sintering furnace and is pre-sintered.The mass ratio of fountain height and nickel cobalt lithium aluminate presoma on saleratus solution The 2% first sintering temperature that nickel cobalt lithium aluminate presoma gross mass is accounted for for 5%, F spray solution amounts is 300 DEG C, time 2h, then It is rapidly heated by 5 DEG C/min, is warming up to 600 DEG C, time 10h, obtain the pre-burning presoma of hole shape.
2) 100g is weighed into the pre-burning presoma of hole shape, by pre-burning presoma in the case where heating while stirring It is added to 1% NbCl5Solution and 2% MgCl2Then solution is uniformly mixed, obtain ready sample.Pre-burning presoma and Mg, The mass ratio of Nb mixed solutions is 1:10, whipping temp is 40 DEG C, mixing time 1h.
3) ready sample that will have been adulterated is placed into Rotary Evaporators, and the temperature for setting Rotary Evaporators is 80 DEG C, rotation Turn the time as 2h, carry out rotating pressure-decreasing distillation, be Nb, Mg doping precursor material by the completely rear resulting material of moisture evaporation.
4) weigh 100g has Nb, Mg to adulterate precursor material, is 1.03 according to Li/Me, lithium hydroxide is added in, by two kinds Raw material is put into high mixer, while sprays into a concentration of 4% NH again4F solution, then according in rotating speed to mix under 1000rpm 10min。
5) sample mixed is put into sintering oven, is sintered 20h at a temperature of 750 DEG C, is passed through oxygen, be sintered Into sample, through mistake screen out iron after be zwitterion mixing and doping nickel cobalt lithium aluminate cathode material.
Comparative example：
100g nickel cobalt lithium aluminate presomas are weighed, is 1.03 according to Li/Me, adds in lithium hydroxide, two kinds of raw materials are put into In high mixer.The sample mixed is put into sintering oven, 12h is sintered at a temperature of 600 DEG C, is passed through oxygen, be sintered Into sample, through mistake screen out iron after be common lithium aluminate cathode material.
For the positive electrode prepared respectively using embodiment and comparative example as positive active material, lithium piece is cathode, is assembled into button Formula battery.The composition of positive plate is m (active material)：M (acetylene black)：M (PVDF)=80:12:8, using blue electrical measurement test system It is tested, charging/discharging voltage is 2.75~4.3V, and cycle performance test is carried out under normal temperature environment.Charge and discharge cycles number with The relationship of capacity retention ratio is as shown in Figure 4.After 50 circle cycles, lithium battery conservation rate prepared by embodiment positive electrode is 97.2%, lithium battery capacity conservation rate prepared by comparative example positive electrode is 95.3%.It can be seen that zwitterion of the present invention mixes The nickel cobalt lithium aluminate cathode material electric property for closing doping is better than common nickel cobalt lithium aluminate cathode material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.

Claims (9)

  1. A kind of 1. preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping, which is characterized in that the preparation Method includes the following steps：
    S1, pre-sintering step：
    Nickel cobalt lithium aluminate presoma is weighed, and sprays a certain amount of saleratus solution and F solution, is then uniformly mixed, is transferred to burning Freezing of a furnace first carries out low temperature presintering knot, is then rapidly heated, and carries out a period of time high temperature pre-sintering, obtains the pre-burning forerunner of hole shape Body；
    S2, cation doping step：
    Certain density Nb solution and Mg solution is configured and mixes, the pre-burning presoma of described hole shape is weighed, while stirring In the case of heating a period of time, pre-burning presoma is poured into Nb, Mg mixed solution, is uniformly mixed, obtains ready sample；
    S3, drying steps：
    Processing is dried in the ready sample, obtains Nb, Mg doping precursor material；
    S4, mixing material and anion doped step：
    Weigh described Nb, Mg doping precursor material, lithium source added according to certain lithium proportioning, together in high merging high mixer into Row mixing, mixing spray into a certain amount of F ion and adjust agent solution simultaneously；
    S5, sintering step：
    The sample mixed is put into sintering oven, sintering temperature and sintering time are set, gas is passed through, after the completion of being sintered Sample obtains the nickel cobalt lithium aluminate cathode material of the zwitterion mixing and doping after crossing and screening out iron.
  2. 2. the preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping as described in claim 1, feature exist In in step S1, the mass percent concentration of the saleratus solution is 5%-10%, and saleratus solution fountain height accounts for nickel cobalt aluminium The 1%-10% of sour lithium presoma gross mass, the mass percent concentration of the F solution is 0.2%-1.5%, and F solution accounts for nickel cobalt The 1%-5% of lithium aluminate presoma gross mass, the F solution are NH4F、NaF、MgF2In one kind；Sintering furnace low temperature presintering knot Temperature is 300 DEG C, and then time 2-5h is rapidly heated by 5-10 DEG C/min, high temperature is carried out after being warming up to 600-800 DEG C It is pre-sintered, time 5-10h.
  3. 3. the preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping as described in claim 1, feature exist In in step S2, Nb solution and the mass percent concentration of Mg solution are 0.05-3%, and pre-burning presoma is mixed with Nb, Mg The mass ratio of solution is 1：(5-20), whipping temp are 40-80 DEG C, mixing time 1-4h, and the Nb solution is nitric acid niobium, niobium One or more of acid, lithium niobate, fluorination niobium, sulfuric acid niobium, the Mg solution is magnesium nitrate, magnesium oxalate, magnesium chloride, magnesium sulfate Middle one or more.
  4. 4. the preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping as described in claim 1, feature exist In step S3 uses rotary evaporation drying process, and the ready sample is placed into Rotary Evaporators, carries out rotating pressure-decreasing steaming It evaporates, is Nb, Mg doping precursor material by the completely rear resulting material of moisture evaporation.
  5. 5. the preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping as claimed in claim 4, feature exist In the temperature of Rotary Evaporators is set in 60-90 DEG C, rotational time 2-6h.
  6. 6. the preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping as described in claim 1, feature exist The mass percent concentration that agent solution is adjusted in, F ion in step S4 is more than F solution in step S1, and F described here from Son adjusts the mass percent concentration 1-10% of agent solution, and it is NH that F ion, which adjusts agent solution,4F、NaF、MgF2In one kind, use Lithium source be Lithium hydroxide monohydrate, lithium carbonate, one or more of lithium chloride, lithium proportioning Li/Me is 1.0-1.2, during mixing Between be 2-10min, rotating speed 500-1400rpm.
  7. 7. the preparation method of the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping as described in claim 1, feature exist In sintering temperature is 500-800 DEG C, sintering time 10-25h in step S5, is passed through gas as air or oxygen.
  8. 8. a kind of nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping, which is characterized in that the zwitterion mixing is mixed Miscellaneous nickel cobalt lithium aluminate cathode material is prepared by any one of such as described claim 1-7 the methods.
  9. 9. the nickel cobalt lithium aluminate cathode material of zwitterion mixing and doping as claimed in claim 8, which is characterized in that the negative and positive The Components Chemical formula Li of the nickel cobalt lithium aluminate cathode material of Ar ion mixing dopingxNi1-a-b-c-dCoaAlbMgcNbdO2-yFyIt represents, Wherein 0.85≤x≤1.2,0≤a≤0.15,0≤b≤0.03,0.001≤c≤0.003,0.001≤d≤0.0003,0.001 ≤y≤0.005。
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CN110289415A (en) * 2019-07-05 2019-09-27 福州大学 A kind of class monocrystalline tertiary cathode material and preparation method thereof that cation-anion co-doping is miscellaneous
CN111233042A (en) * 2020-01-16 2020-06-05 阜阳师范大学 Lithium manganate positive electrode material precursor, lithium manganate positive electrode material and preparation method thereof
CN112701271A (en) * 2020-12-28 2021-04-23 格林美（无锡）能源材料有限公司 Element doping method based on ternary precursor positive electrode material
WO2022206065A1 (en) * 2021-03-29 2022-10-06 广东邦普循环科技有限公司 Material mixing process for preparing high-nickel positive electrode material and use thereof
GB2618690A (en) * 2021-03-29 2023-11-15 Guangdong Brunp Recycling Technology Co Ltd Material mixing process for preparing high-nickel positive electrode material and use thereof
ES2956824R1 (en) * 2021-03-29 2024-04-01 Guangdong Brunp Recycling Technology Co Ltd Mixing process to prepare cathode material with high nickel content and application thereof
CN114914436A (en) * 2022-02-10 2022-08-16 中国第一汽车股份有限公司 High-nickel ternary cathode material and preparation method thereof
CN114914436B (en) * 2022-02-10 2024-06-04 中国第一汽车股份有限公司 High-nickel ternary positive electrode material and preparation method thereof
CN116169280A (en) * 2023-03-07 2023-05-26 北京工业大学 High-entropy compound for positive electrode of aluminum ion battery and preparation method thereof

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