CN104701520A - A preparing method of a LiMn<1.5>Ni<0.5>O<4-a> cathode material - Google Patents

A preparing method of a LiMn<1.5>Ni<0.5>O<4-a> cathode material Download PDF

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CN104701520A
CN104701520A CN201310656753.3A CN201310656753A CN104701520A CN 104701520 A CN104701520 A CN 104701520A CN 201310656753 A CN201310656753 A CN 201310656753A CN 104701520 A CN104701520 A CN 104701520A
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limn
presoma
hour
positive electrode
temperature
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许寒
刘兴江
刘浩杰
彭庆文
卢志威
任丽彬
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CETC 18 Research Institute
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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
    • 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
    • H01M4/52—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)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a preparing method of a LiMn<1.5>Ni<0.5>O<4-a> cathode material. The method includes a step of preparing lithium carbonate, nickel monoxide and manganese dioxide into a LiMn<1.5>Ni<0.5>O4 precursor. The method is characterized in that: the LiMn<1.5>Ni<0.5>O4 precursor is sintered at different temperature stages to complete preparation of the LiMn<1.5>Ni<0.5>O<4-a> cathode material. By adoption of the different temperature stages, the LiNi<0.5> Mn<1.5>O4 is subjected to heat processing. The degree of oxygen vacancies in a product is controlled without doping other elements so as to obtain the LiMn<1.5>Ni<0.5>O<4-a> material. The oxygen content in the molecular is reduced, thus achieving adjustment on material rate capacity, improving material conductivity and avoiding system homogeneity unbalance caused by doping other elements, allowing batch uniformity of the prepared material to be good, and facilitating industrial technology popularization of the product.

Description

LiMn 1.5ni 0.5o 4-athe preparation method of positive electrode
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, particularly relate to a kind of LiMn 1.5ni 0.5o 4-athe preparation method of positive electrode.
Background technology
Enter 21st century, the global energy crisis brought along with automobile and environmental pollution, national governments all successively drop into the development that huge fund strengthens new-energy automobile, and New-energy electric vehicle and hybrid vehicle become the favorite in epoch.Current power battery of electric motor car mainly contains three kinds: lead-acid battery, Ni-MH battery and lithium dynamical battery.From development trend in the future, lithium-ion-power cell will become main flow, have broad application prospects, and accordingly, the positive pole of lithium-ion-power cell critical material researches and develops requirement of must keeping pace with the times.
First lithium-ion-power cell has good security performance to the requirement of positive electrode, can normally work in more wide in range temperature range, there is higher energy density simultaneously, the requirement of lithium ion battery to positive electrode high power performance can be adapted to, and energy density depends primarily on electrochemistry and the physical properties such as the tap density of the operating voltage of material itself, capacity and material, in current industry, the focus of anode material for lithium-ion batteries research mainly concentrates on olivine transition metal phosphate system positive electrode (LiMPO 4) and spinelle manganese cathode material on.
The olivine transition metal phosphate system positive electrode being representative with LiFePO 4 and lithium manganese phosphate has and has extended cycle life, fail safe is good, extensively and lower-price characteristic, but it is lower meanwhile also to there is material electric conductivity for raw material sources, and high rate performance difference waits the deficiency of practical application.
For spinel manganese based material, that use is more usually is LiMn2O4 (LiMn 2o 4) material, but to there is inherent problem in this material be exactly charge-discharge performance difference, and capacity attenuation is very fast.It has been generally acknowledged that main cause is wherein Mn 3+existence create Jahn-Teller effect, there is distortion of lattice in material, cause volume contraction or expansion in charge and discharge process.
Find that application number is 201110428113.8 through retrieval, publication number is CN102683668A, name is called: the patent of invention of spinel nickel manganese-base oxide positive electrode and preparation method thereof, disclose a kind of spinel nickel manganese-base oxide positive electrode in its specification, there is the atomic ratio composition shown in formula (I): Li am x+ yNi 0.5-ymn 1.5-xo 4; (I); Wherein, 0.9≤a≤1.1,0≤x≤0.2,0≤y≤0.1; M is one or more in Mg, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zr, Nb, Ag, Sn, Ce, Nd, Ta, W, Pt and Au.The patent application be found to have employed the method for doped with metal elements, less volume contraction or expansion, improve the power-performance of spinel anode material, but owing to introducing new metallic element in doping process, add raw material type, thus make batch consistency existing problems of material, be unfavorable for that the industrialization technology of product is promoted.
Summary of the invention
The present invention for solve in known technology the technical problem that exists and provide a kind of multiplying power and cycle performance good, batches of materials consistency is good, and the industrialization technology being conducive to product is promoted, and has the LiMn of environment protecting 1.5ni 0.5o 4-athe preparation method of positive electrode.
The present invention includes following technical scheme:
LiMn 1.5ni 0.5o 4-athe preparation method of positive electrode, preparation process comprises: make presoma: (1) according to the ratio of mol ratio Li:Ni:Mn=1.1-2:0.5-1:1.5-2, by lithium carbonate, nickel protoxide, manganese dioxide, be that ball-milling medium carries out wet ball grinding mixing 3-15 hour with ethanol, form LiMn 1.5ni 0.5o 4slurry presoma; (2) by LiMn 1.5ni 0.5o 4the taking-up of slurry presoma is placed on 60 DEG C of-80 DEG C of drying boxes and carries out drying in 3-6 hour, completes LiMn 1.5ni 0.5o 4the manufacturing process of presoma, is characterized in: preparation process also comprises and is divided into different temperatures section sintering LiMn 1.5ni 0.5o 4presoma, completes LiMn 1.5ni 0.5o 4-athe manufacturing process of (0 < a≤0.05) positive electrode.
The present invention can also adopt following technical measures:
The described different temperatures section that is divided into sinters LiMn 1.5ni 0.5o 4the process of presoma comprises: by the LiMn made 1.5ni 0.5o 4presoma is placed in high temperature Muffle furnace and heat-treats, and the temperature arranged in high temperature Muffle furnace is successively: 850 DEG C-950 DEG C sintering 14-22 hour, then in 1.5-15 hour, the temperature in high temperature Muffle furnace is down to 610 DEG C-625 DEG C; At 610 DEG C of-625 DEG C of temperature, continue sintering after 2-32 hour, material is Temperature fall to 25 DEG C in stove, and the material of taking-up is LiMn 1.5ni 0.5o 4-a.
The advantage that the present invention has and good effect:
1, the present invention is by taking the different temperatures stage, to the LiNi of preparation 0.5mn 1.5o 4positive electrode is heat-treated, and by controlling merely high temperature sintering condition, other yuan any that do not adulterate usually control the degree of oxygen defect in product, obtains LiMn 1.5ni 0.5o 4-amaterial, because oxygen element content in molecule reduces, realizes, to the adjustment of material high rate performance, improving material conductivity; Avoid because the system system consistency that other element brings of adulterating is unbalance, the batches of materials consistency made is good, and the industrialization technology being conducive to product is promoted.
2, the present invention is not owing to increasing other element any, do not increase poisonous and harmful emission in production process yet, meets the requirement of environmental protection.
3, the LiMn for preparing of the present invention 1.5ni 0.5o 4-apositive electrode, cycle performance is compared to LiNi 0.5mn 1.5o 4, not only effectively improve the cycle life of material, and material multiplying power electric conductivity there has also been obvious lifting, simultaneously from preparation technology's angle, oxygen-starved positive electrode LiMn 1.5ni 0.5o 4-a, compare LiNi 0.5mn 1.5o 4annealing time is shorter, and chemical property plays more excellent.
Embodiment
For summary of the invention of the present invention, Characteristic can be disclosed further, be described in detail as follows especially exemplified by following instance.
LiMn 1.5ni 0.5o 4-athe preparation method of positive electrode, preparation process comprises: make presoma: (1) according to the ratio of mol ratio Li:Ni:Mn=1.1-2:0.5-1:1.5-2, by lithium carbonate, nickel protoxide, manganese dioxide, be that ball-milling medium carries out wet ball grinding mixing 3-15 hour with ethanol, form LiMn 1.5ni 0.5o 4slurry presoma; (2) by LiMn 1.5ni 0.5o 4the taking-up of slurry presoma is placed on 60 DEG C of-80 DEG C of drying boxes and carries out drying in 3-6 hour, completes LiMn 1.5ni 0.5o 4the manufacturing process of presoma, is characterized in: preparation process also comprises and is divided into different temperatures section sintering LiMn 1.5ni 0.5o 4presoma, completes LiMn 1.5ni 0.5o 4-athe manufacturing process of (0 < a≤0.05) positive electrode.
The described different temperatures section that is divided into sinters LiMn 1.5ni 0.5o 4the process of presoma comprises: by the LiMn made 1.5ni 0.5o 4presoma is placed in high temperature Muffle furnace and heat-treats, and the temperature arranged in high temperature Muffle furnace is successively: 850 DEG C-950 DEG C sintering 14-22 hour, then in 1.5-15 hour, the temperature in high temperature Muffle furnace is down to 610 DEG C-625 DEG C; At 610 DEG C of-625 DEG C of temperature, continue sintering after 2-32 hour, material is Temperature fall to 25 DEG C in stove, and the material of taking-up is LiMn 1.5ni 0.5o 4-a.
Embodiment 1
By lithium carbonate (Li 2cO 3), nickel protoxide (NiO), manganese dioxide (MnO 2) according to the ratio of mol ratio Li:Ni:Mn=1.5:0.5:1.5, lithium carbonate, nickel protoxide, manganese dioxide are inserted ball mill, be that ball-milling medium carries out wet ball grinding and mixes 4 hours with ethanol, form LiMn 1.5ni 0.5o 4slurry presoma; By LiMn 1.5ni 0.5o 4the taking-up of slurry presoma is placed on 60 DEG C of drying boxes and carries out drying in 3 hours, completes LiMn 1.5ni 0.5o 4the manufacturing process of presoma; By obtained LiMn 1.5ni 0.5o 4presoma is placed in high temperature Muffle furnace, first at 850 DEG C of temperature, sinter 14 hours, then in 2 hours, the temperature in high temperature Muffle furnace is cooled to 610 DEG C from 850 DEG C, at 610 DEG C of temperature, sinter 6 hours, take out after naturally cooling to 25 DEG C of room temperatures, namely form LiMn of the present invention 1.5ni 0.5o 4-apositive electrode.
Embodiment 2
By lithium carbonate, nickel protoxide, manganese dioxide according to the ratio of mol ratio Li:Ni:Mn=1.2:0.5:1.5, lithium carbonate, nickel protoxide, manganese dioxide are inserted ball mill, be that ball-milling medium carries out wet ball grinding and mixes 6 hours with ethanol, form LiMn 1.5ni 0.5o 4slurry presoma; By LiMn 1.5ni 0.5o 4the taking-up of slurry presoma is placed on 60 DEG C of drying boxes and carries out drying in 3 hours, completes LiMn 1.5ni 0.5o 4the manufacturing process of presoma; By obtained LiMn 1.5ni 0.5o 4presoma is placed in high temperature Muffle furnace, first at 850 DEG C of temperature, sinter 16 hours, then in 5 hours, the temperature in high temperature Muffle furnace is cooled to 620 DEG C from 850 DEG C, at 620 DEG C of temperature, sinter 8 hours, take out after naturally cooling to 25 DEG C of room temperatures, namely form LiMn of the present invention 1.5ni 0.5o 4-apositive electrode.
Embodiment 3
By lithium carbonate, nickel protoxide, manganese dioxide according to the ratio of mol ratio Li:Ni:Mn=1.2:0.5:1.5, lithium carbonate, nickel protoxide, manganese dioxide are inserted ball mill, be that ball-milling medium carries out wet ball grinding and mixes 10 hours with ethanol, form LiMn 1.5ni 0.5o 4slurry presoma; By LiMn 1.5ni 0.5o 4the taking-up of slurry presoma is placed on 60 DEG C of drying boxes and carries out drying in 3 hours, completes LiMn 1.5ni 0.5o 4the manufacturing process of presoma; By obtained LiMn 1.5ni 0.5o 4presoma is placed in high temperature Muffle furnace, first at 850 DEG C of temperature, sinter 20 hours, then in 10 hours, the temperature in high temperature Muffle furnace is cooled to 625 DEG C from 850 DEG C, at 625 DEG C of temperature, sinter 10 hours, take out after naturally cooling to 25 DEG C of room temperatures, namely complete LiMn of the present invention 1.5ni 0.5o 4-athe manufacturing process of positive electrode.
Comparative example 1
By lithium carbonate, nickel protoxide, manganese dioxide according to the ratio of Li:Ni:Mn=1.5:0.5:1.5, be that ball-milling medium carries out wet ball grinding and mixes 4 hours with ethanol, formed slurry presoma; Slurry presoma is placed in 60 DEG C of drying boxes 3 after dry hour, is placed in 850 DEG C of high temperature Muffle furnace heat treatments 14 hours, completes LiMn 1.5ni 0.5o 4the manufacturing process of positive electrode.
Comparative example 2
By lithium carbonate, nickel protoxide, manganese dioxide according to the ratio of Li:Ni:Mn=1.5:0.5:1.5, be that ball-milling medium carries out wet ball grinding and mixes 6 hours with ethanol, formed slurry presoma; Slurry presoma is placed in 60 DEG C of drying boxes 3 after dry hour, is placed in 625 DEG C of high temperature Muffle furnace heat treatments 14 hours, completes LiMn 1.5ni 0.5o 4the manufacturing process of positive electrode.
The test result contrast table of table 1 embodiment of the present invention and comparative example
Capacity (0.2C) mAh/g 50 circulation conservation rate % Multiplying power ratio (5C/0.2C) %
Embodiment 1 139 100 95
Embodiment 2 142 100 94
Embodiment 3 137 100 96
Comparative example 1 128 85 92
Comparative example 2 125 100 74
Test result as can be seen from table: adopt LiMn prepared by the present invention 1.5ni 0.5o 4positive electrode, is ensureing that under the prerequisite that cycle performance does not lose, the high rate performance improving material further (specifically can as can be seen from table 1 multiplying power ratio (5C/0.2C) %.
Operation principle of the present invention:
The present invention takes the different temperatures stage, to the LiNi of preparation 0.5mn 1.5o 4positive electrode is heat-treated, and by controlling merely high temperature sintering condition, other yuan any that do not adulterate usually control the degree of oxygen defect in product, obtains LiMn 1.5ni 0.5o 4-amaterial, make the 4V platform namely occurring certain capacity in material containing appropriate manganic in discharge curve, the capacity of 4V platform accounts for the 7%-9% of total capacity in addition because oxygen element content in molecule reduces, so make the total chemical valence of anion in molecule reduce, again because Li, Ni element presents stable+1 valency and+3 valencys in the molecule, therefore in order to realize valent balance, the manganese element chemical valence of+4 valencys can only be made to reduce a part, namely generate small part+3 valency manganese, maintain chemical valence balance; Realize the adjustment to material high rate performance, improve material conductivity; Avoid because the system system consistency that other element brings of adulterating is unbalance, the batches of materials consistency made is good, and the industrialization technology being conducive to product is promoted.
Although be described the preferred embodiments of the present invention above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing under the ambit that present inventive concept and claim protect, a lot of form can also be made.These all belong within protection scope of the present invention.

Claims (2)

1.LiMn 1.5ni 0.5o 4-athe preparation method of positive electrode, preparation process comprises: make presoma: (1) according to the ratio of mol ratio Li:Ni:Mn=1.1-2:0.5-1:1.5-2, by lithium carbonate, nickel protoxide, manganese dioxide, be that ball-milling medium carries out wet ball grinding mixing 3-15 hour with ethanol, form LiMn 1.5ni 0.5o 4slurry presoma; (2) by LiMn 1.5ni 0.5o 4the taking-up of slurry presoma is placed on 60 DEG C of-80 DEG C of drying boxes and carries out drying in 3-6 hour, completes LiMn 1.5ni 0.5o 4the manufacturing process of presoma, is characterized in that: preparation process also comprises and is divided into different temperatures section sintering LiMn 1.5ni 0.5o 4presoma, completes LiMn 1.5ni 0.5o 4-athe manufacturing process of positive electrode.
2. LiMn according to claim 1 1.5ni 0.5o 4-athe preparation method of positive electrode, is characterized in that: described in be divided into different temperatures section sintering LiMn 1.5ni 0.5o 4the process of presoma comprises: by the LiMn made 1.5ni 0.5o 4presoma is placed in high temperature Muffle furnace and heat-treats, and the temperature arranged in high temperature Muffle furnace is successively: 850 DEG C-950 DEG C sintering 14-22 hour, then in 1.5-15 hour, the temperature in high temperature Muffle furnace is down to 610 DEG C-625 DEG C; At 610 DEG C of-625 DEG C of temperature, continue sintering after 2-32 hour, material is Temperature fall to 25 DEG C in stove, and the material of taking-up is LiMn 1.5ni 0.5o 4-a, wherein: 0 < a≤0.05.
CN201310656753.3A 2013-12-05 2013-12-05 A preparing method of a LiMn<1.5>Ni<0.5>O<4-a> cathode material Pending CN104701520A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101243564A (en) * 2005-08-25 2008-08-13 原子能委员会 High-voltage positive electrode material having a spinel structure based on nickel and manganese for lithium cell batteries
CN102299310A (en) * 2011-07-13 2011-12-28 奇瑞汽车股份有限公司 Preparation method for LiNi0.5Mn1.5O4 material and lithium ion battery prepared by materials
CN102623691A (en) * 2012-04-27 2012-08-01 常熟理工学院 Method for preparing lithium nickel manganese oxide serving as cathode material of lithium battery
CN103227323A (en) * 2013-05-22 2013-07-31 哈尔滨工业大学 Preparation method of positive pole material (spinel type lithium nickel manganese oxide) of high-voltage lithium ion battery

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101243564A (en) * 2005-08-25 2008-08-13 原子能委员会 High-voltage positive electrode material having a spinel structure based on nickel and manganese for lithium cell batteries
CN102299310A (en) * 2011-07-13 2011-12-28 奇瑞汽车股份有限公司 Preparation method for LiNi0.5Mn1.5O4 material and lithium ion battery prepared by materials
CN102623691A (en) * 2012-04-27 2012-08-01 常熟理工学院 Method for preparing lithium nickel manganese oxide serving as cathode material of lithium battery
CN103227323A (en) * 2013-05-22 2013-07-31 哈尔滨工业大学 Preparation method of positive pole material (spinel type lithium nickel manganese oxide) of high-voltage lithium ion battery

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
J.-H. KIM, ET AL.: "Comparative Study of LiNi0.5Mn1.5O4-δ and LiNi0.5Mn1.5O4 Cathodes Having Two Crystallographic Structures：Fd3m and P4332", 《CHEM. MATER.》 *

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