CN103700840A - Cathode material of high-voltage lithium battery and preparation method for cathode material - Google Patents

Cathode material of high-voltage lithium battery and preparation method for cathode material Download PDF

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Publication number
CN103700840A
CN103700840A CN201410006909.8A CN201410006909A CN103700840A CN 103700840 A CN103700840 A CN 103700840A CN 201410006909 A CN201410006909 A CN 201410006909A CN 103700840 A CN103700840 A CN 103700840A
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coo
mixture
cathode material
grind
preparation
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关成善
宗继月
李涛
贾传龙
单传省
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Shandong Goldencell Electronics Technology Co Ltd
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Shandong Goldencell Electronics Technology 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
    • 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
    • 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 cathode material of a high-voltage lithium battery. The general formula of the cathode material is LiNi(0.5-x)Mn(1.5)MxO4. The invention also discloses a preparation method for the cathode material of the high-voltage lithium battery. The preparation method comprises the steps of putting LiCH3COO, Ni(CH3COO)2, Mn(CH3COO)2 and M(CH3COO)y into a ball grinding machine according to the ratio of 2:(1-x):3:x, then adding alcohol to prepare uniform paste, and grinding the paste for 30-60min; adding ammonia water into the paste mixture to generate full reaction by reactants, then screening the mixture, putting the screened mixture into an air blowing drying box with the temperature of 100-130 DEG C for drying, putting a precursor into a muffle furnace for pretreatment at the temperature of 300-400 DEG C for 3-5 hours, then heating to 850-950 DEG C, burning for 10-11 hours, annealing at the temperature of 400-500 DEG C for 6-7 hours, and finally naturally cooling to room temperature to obtain the LiNi(0.5-x)Mn(1.5)MxO4.

Description

A kind of high-voltage lithium-battery cathode material and preparation method thereof
Technical field
The present invention relates to a kind of high-voltage lithium, relate in particular to a kind of high-voltage lithium-battery cathode material and preparation method thereof.
Background technology
Lithium rechargeable battery occupies rapidly consumption market with superior performance, and the main energy sources that is considered to electric motor car of future generation and hybrid electric vehicle thereof, in recent years, improved anode material of lithium battery and improved security performance, improve battery charge capacity and reduce production costs and become the major axes orientation of lithium rechargeable battery development.Be accompanied by very big demand and high-tension electrolyte and the electrolytical successfully development of electric automobile, high-tension LiNi xmn 2-xo 4(0<x<2) receive great concern.Research in recent years shows, LiNi in above-mentioned various spinel-types 0.5mn 1.5o 4(theoretical gram volume is 147mAh/g) not only has the high voltage platform of 4.7V, and has good safety and cycle performance.
The synthetic method of high voltage material nickel LiMn2O4 of spinel-type has: solid phase method, sol-gal process, coprecipitation, fuse salt method, spray pyrolysis etc.Solid phase method is that lithium source, He Meng source, nickel source ball milling is even, and presoma is at high temperature calcined.This method is simple to operate, but easily occurs batch mixing uneven phenomenon in manufacturing process, thereby makes difficult control of performance of product; Molten salt method is when calcining heat is 1000 ℃ of left and right, and Spinel starts to decompose along with the lowering one's standard or status of crystal structure, and it is very poor that chemical property becomes; Spray pyrolysis complex manufacturing process and yielding poorly, discharges and recharges reversibility poor.
Summary of the invention
The object of this invention is to provide a kind of high-voltage lithium-battery cathode material that a kind of cycle performance is high, security performance is good.
Another object of the present invention is to provide a kind of preparation method of high-voltage lithium-battery cathode material.
For achieving the above object, the technical solution used in the present invention is: a kind of high-voltage lithium-battery cathode material, is characterized in that: this positive electrode general formula is LiNi 0.5-xmn 1.5m xo 4, wherein: M is one or more of mixing in metal Cu, Co, Al and Cr, 0.07≤x≤0.1.
A preparation method for high-voltage lithium-battery cathode material, is characterized in that: the method for employing Rheological Phase Method is prepared the high-voltage anode material of spinel structure.
In the method, comprise the following steps:
(1) preparation of presoma
Step 1: the ammoniacal liquor that compound concentration is 1-20mol/L;
Step 2: by LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2, M (CH 3cOO) yby 2:(1-x): 3:x puts into ball mill, its LiCH 3the excessive 3%-5% of COO, fully grinds raw material evenly, then adds distilled water, continues to grind evenly, then adds alcohol, and mixture is made into uniform pasty state, grinds the 30-60min time;
Step 3: drip the ammoniacal liquor that step 1 is prepared in pasty mixture, regulating pH value is 8-9, continues to grind the 30-60min time, reactant is fully reacted, then sieve, the mixture after sieving is placed in 100-130 ℃ of air dry oven dry, obtains presoma;
(2) high-temperature process
Presoma is put into Muffle furnace 300-400 ℃ of preliminary treatment 3-5h, be then warming up to 850-950 ℃ and burn 10-11h, then 400-500 ℃ of annealing 6-7h, the last naturally cooling room temperature of being down to obtains LiNi 0.5-xmn 1.5m xo 4.
Advantageous effect of the present invention is: 1, Rheological Phase Method is prepared organic use amount in material than solvent gel method, has realized nickel, manganese and has mixed mixing of ion.2, the condition that Rheological Phase Method synthesis technique can react by change, easily controls the surface area of presoma, the size of particle and crystal grain distribute.3, this method is passed through at high-voltage anode material LiNi 0.5mn 1.5in O4, mix the LiNi that part ion obtains 0.5-xmn 1.5m xo 4(0.07≤x≤0.1), has improved positive electrode LiNi 0.5mn 1.5the stability of O4.4, the present invention has optimized the physical and chemical performance of material, and material granule size evenly, has improved the stable circulation performance of material.
Accompanying drawing explanation
Fig. 1 is the SEM figure of embodiment 2 high-voltage anode material samples;
Fig. 2 is the cyclic curve figure of embodiment 3 high-voltage anode material samples.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
As shown in Figure 1, 2, a kind of high-voltage lithium-battery cathode material, is characterized in that in the present invention: this positive electrode general formula is LiNi 0.5-xmn 1.5m xo 4, wherein: M is one or more of mixing in metal Cu, Co, Al and Cr, 0.07≤x≤0.1.A preparation method for high-voltage lithium-battery cathode material, is characterized in that: the method for employing Rheological Phase Method is prepared the high-voltage anode material of spinel structure, comprises the following steps:
(1) preparation of presoma
Step 1: the ammoniacal liquor that compound concentration is 1-20mol/L;
Step 2: by LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2, M (CH 3cOO) yby 2:(1-x): 3:x puts into ball mill, its LiCH 3the excessive 3%-5% of COO, fully grinds raw material evenly, then adds distilled water, continues to grind evenly, then adds alcohol, and mixture is made into uniform pasty state, grinds the 30-60min time;
Step 3: drip the ammoniacal liquor that step 1 is prepared in pasty mixture, regulating pH value is 8-9, continues to grind the 30-60min time, reactant is fully reacted, then sieve, the mixture after sieving is placed in 100-130 ℃ of air dry oven dry, obtains presoma;
(2) high-temperature process
Presoma is put into Muffle furnace 300-400 ℃ of preliminary treatment 3-5h, be then warming up to 850-950 ℃ and burn 10-11h, then 400-500 ℃ of annealing 6-7h, the last naturally cooling room temperature of being down to obtains LiNi 0.5-xmn 1.5m xo 4.In the present embodiment, described M (CH 3cOO) yfor Cu (CH 3cOO) 2, Co (CH 3cOO) 2, Al 2(CH 3cOO) 3, Cr2 (CH 3cOO) 3in one or more.In the present embodiment, described alcohol is one or more in methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol.
Embodiment 1:
By LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2by 2.03:1:3, put into ball mill, raw material is fully ground evenly, then add a certain amount of distilled water, continue to grind evenly, then add a small amount of methyl alcohol, mixture is made into uniform pasty state, grind the 30min time; Toward the ammoniacal liquor that drips a small amount of preparation in pasty mixture, regulating pH value be 8-9, continues the grinding 30min time, and reactant is fully reacted, and then sieves, and the mixture after sieving is placed in 100 ℃ of air dry ovens and is dried, and obtains presoma.Presoma is put into 300 ℃ of preliminary treatment 5h of Muffle furnace, be then warming up to 850 ℃ and burn 11h, then 400 ℃ of annealing 6h, the last naturally cooling room temperature of being down to obtains positive electrode.
Embodiment 2:
By LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2, Mg (CH 3cOO) 2by putting into ball mill in 2.04:0.86:3:0.14, raw material is fully ground evenly, then add a certain amount of distilled water, continue to grind evenly, then add a small amount of ethanol, mixture is made into even pasty state, grind the 50min time; Toward the ammoniacal liquor that drips a small amount of preparation in pasty mixture, regulating pH value be 8-9, continues the grinding 50min time, and reactant is fully reacted, and then sieves, and the mixture after sieving is placed in 110 ℃ of air dry ovens and is dried, and obtains presoma.Presoma is put into 350 ℃ of preliminary treatment 4h of Muffle furnace, be then warming up to 900 ℃ and burn 10h, then 450 ℃ of annealing 6.5h, the last naturally cooling room temperature of being down to obtains positive electrode.
Embodiment 3:
By LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2, Cu (CH 3cOO) 2by putting into ball mill in 2.05:0.8:3:0.2, raw material is fully ground evenly, then add a certain amount of distilled water, continue to grind evenly, then add a small amount of propyl alcohol, mixture is made into pasty state, grind the 60min time; Toward the ammoniacal liquor that drips a small amount of preparation in pasty mixture, regulate pH value 8-9, continue to grind the 60min time, reactant is fully reacted, then sieve, the mixture after sieving is placed in 130 ℃ of air dry ovens and is dried, and obtains presoma.Presoma is put into 400 ℃ of preliminary treatment 3h of Muffle furnace, be then warming up to 950 ℃ and burn 11h, then 500 ℃ of annealing 7h, the last naturally cooling room temperature of being down to obtains positive electrode.
The charging voltage of spinel-type nickel manganate cathode material for lithium of the present invention approaches 5V.
In building-up process of the present invention, can prepare by controlling the parameter of course of reaction the comparatively pure LiNi of different physicochemical characteristics 0.5-xmn 1.5m xo 4positive electrode.

Claims (8)

1. a high-voltage lithium-battery cathode material, is characterized in that: this positive electrode general formula is LiNi 0.5-xmn 1.5m xo 4, wherein: M is one or more of mixing in metal Cu, Co, Al and Cr, 0.07≤x≤0.1.
2. a preparation method for high-voltage lithium-battery cathode material, is characterized in that: the method for employing Rheological Phase Method is prepared the high-voltage anode material of spinel structure.
3. the preparation method of a kind of high-voltage lithium-battery cathode material according to claim 2, is characterized in that: comprise the following steps:
(1) preparation of presoma
Step 1: the ammoniacal liquor that compound concentration is 1-20mol/L;
Step 2: by LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2, M (CH 3cOO) yby 2:(1-x): 3:x puts into ball mill, its LiCH 3the excessive 3%-5% of COO, fully grinds raw material evenly, then adds distilled water, continues to grind evenly, then adds alcohol, and mixture is made into uniform pasty state, grinds the 30-60min time;
Step 3: drip the ammoniacal liquor that step 1 is prepared in pasty mixture, regulating pH value is 8-9, continues to grind the 30-60min time, reactant is fully reacted, then sieve, the mixture after sieving is placed in 100-130 ℃ of air dry oven dry, obtains presoma;
(2) high-temperature process
Presoma is put into Muffle furnace 300-400 ℃ of preliminary treatment 3-5h, be then warming up to 850-950 ℃ and burn 10-11h, then 400-500 ℃ of annealing 6-7h, the last naturally cooling room temperature of being down to obtains LiNi 0.5-xmn 1.5m xo 4.
4. the preparation method of a kind of high-voltage lithium-battery cathode material according to claim 3, is characterized in that: described M (CH 3cOO) yfor Cu (CH 3cOO) 2, Co (CH 3cOO) 2, Al 2(CH 3cOO) 3, Cr2 (CH 3cOO) 3in one or more.
5. the preparation method of a kind of high-voltage lithium-battery cathode material according to claim 4, is characterized in that: by LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2by 2.03:1:3, put into ball mill, raw material is fully ground evenly, then add distilled water, continue to grind evenly, then add methyl alcohol, mixture is made into uniform pasty state, grind the 30min time, in pasty mixture, drip the ammoniacal liquor of preparing, regulating pH value is 8-9, continues to grind the 30min time, reactant is fully reacted, then sieve, the mixture after sieving is placed in 100 ℃ of air dry ovens dry, obtains presoma; Presoma is put into 300 ℃ of preliminary treatment 5h of Muffle furnace, be then warming up to 850 ℃ and burn 11h, then 400 ℃ of annealing 6h, the last naturally cooling room temperature of being down to obtains positive electrode.
6. the preparation method of a kind of high-voltage lithium-battery cathode material according to claim 4, is characterized in that: by LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2, Mg (CH 3cOO) 2by 2.04:0.86:3:0.14, put into ball mill, raw material is fully ground evenly, then add distilled water, continue to grind evenly, add again ethanol, mixture is made into even pasty state, grind the 50min time, in pasty mixture, drip the ammoniacal liquor of preparing, regulating pH value is 8-9, continue to grind the 50min time, reactant is fully reacted, then sieve, mixture after sieving is placed in 110 ℃ of air dry ovens dry, obtain presoma, presoma is put into 350 ℃ of preliminary treatment 4h of Muffle furnace, then be warming up to 900 ℃ and burn 10h, again 450 ℃ annealing 6.5h, the last naturally cooling room temperature of being down to obtains positive electrode.
7. the preparation method of a kind of high-voltage lithium-battery cathode material according to claim 4, is characterized in that: by LiCH 3cOO, Ni (CH 3cOO) 2, Mn (CH 3cOO) 2, Cu (CH 3cOO) 2by 2.05:0.8:3:0.2, put into ball mill, raw material is fully ground evenly, then add distilled water, continue to grind evenly, then add propyl alcohol, mixture is made into pasty state, grind the 60min time, in pasty mixture, drip the ammoniacal liquor of preparing, regulate pH value 8-9, continue to grind the 60min time, reactant is fully reacted, then sieve, the mixture after sieving is placed in 130 ℃ of air dry ovens dry, obtains presoma; Presoma is put into 400 ℃ of preliminary treatment 3h of Muffle furnace, be then warming up to 950 ℃ and burn 11h, then 500 ℃ of annealing 7h, the last naturally cooling room temperature of being down to obtains positive electrode.
8. according to the preparation method of a kind of high-voltage lithium-battery cathode material described in claim 6 or 7, it is characterized in that: described alcohol is one or more in methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol.
CN201410006909.8A 2014-01-08 2014-01-08 Cathode material of high-voltage lithium battery and preparation method for cathode material Pending CN103700840A (en)

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CN103928675A (en) * 2014-04-18 2014-07-16 东莞市迈科科技有限公司 Lithium nickel manganese oxide anode material and preparation method thereof
CN104466159A (en) * 2014-10-15 2015-03-25 惠州龙为科技有限公司 Preparation method of high-performance lamellar lithium-enriched high-manganese positive material
CN105655572A (en) * 2014-11-12 2016-06-08 中国电子科技集团公司第十八研究所 Spherical lithium nickel manganese positive electrode material preparation method
CN108807891A (en) * 2018-05-31 2018-11-13 电子科技大学 High potential anode material for lithium-ion batteries LiNi0.5-xMxMn1.5-ySiyO4And preparation method
CN110931770A (en) * 2019-12-03 2020-03-27 江南大学 Cr-doped modified high-voltage spinel cathode material and preparation method thereof
CN110921720A (en) * 2019-12-03 2020-03-27 江南大学 High-voltage lithium ion battery positive electrode material and preparation method thereof
CN113745472A (en) * 2020-05-29 2021-12-03 山东海科创新研究院有限公司 Preparation method of single crystal ternary cathode material and ternary lithium ion battery

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Cited By (11)

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Publication number Priority date Publication date Assignee Title
CN103915617A (en) * 2014-04-18 2014-07-09 东莞市迈科科技有限公司 Lithium-rich positive material and preparation method thereof
CN103928675A (en) * 2014-04-18 2014-07-16 东莞市迈科科技有限公司 Lithium nickel manganese oxide anode material and preparation method thereof
CN104466159A (en) * 2014-10-15 2015-03-25 惠州龙为科技有限公司 Preparation method of high-performance lamellar lithium-enriched high-manganese positive material
CN104466159B (en) * 2014-10-15 2017-11-14 惠州龙为科技有限公司 A kind of preparation method of the high manganese anode material of high-performance stratiform richness lithium
CN105655572A (en) * 2014-11-12 2016-06-08 中国电子科技集团公司第十八研究所 Spherical lithium nickel manganese positive electrode material preparation method
CN108807891A (en) * 2018-05-31 2018-11-13 电子科技大学 High potential anode material for lithium-ion batteries LiNi0.5-xMxMn1.5-ySiyO4And preparation method
CN108807891B (en) * 2018-05-31 2021-07-06 电子科技大学 High-potential lithium ion battery anode material LiNi0.5-xMxMn1.5-ySiyO4And preparation method
CN110931770A (en) * 2019-12-03 2020-03-27 江南大学 Cr-doped modified high-voltage spinel cathode material and preparation method thereof
CN110921720A (en) * 2019-12-03 2020-03-27 江南大学 High-voltage lithium ion battery positive electrode material and preparation method thereof
CN110921720B (en) * 2019-12-03 2022-02-15 江南大学 High-voltage lithium ion battery positive electrode material and preparation method thereof
CN113745472A (en) * 2020-05-29 2021-12-03 山东海科创新研究院有限公司 Preparation method of single crystal ternary cathode material and ternary lithium ion battery

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Application publication date: 20140402