CN103840151A - Ternary positive electrode material with special single-crystal structure, and preparation method thereof - Google Patents

Ternary positive electrode material with special single-crystal structure, and preparation method thereof Download PDF

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CN103840151A
CN103840151A CN201310675280.1A CN201310675280A CN103840151A CN 103840151 A CN103840151 A CN 103840151A CN 201310675280 A CN201310675280 A CN 201310675280A CN 103840151 A CN103840151 A CN 103840151A
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cobalt
nickel
sintering
manganese
crystalline structures
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CN103840151B (en
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关成善
宗继月
李涛
杜丽丽
贾传龙
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Shandong Goldencell Electronics Technology Co Ltd
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SHANDONG HETER ELECTRONIC 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 invention relates to a preparation method for a ternary positive electrode material with a special single-crystal structure. A general formula of the positive electrode material is LiNixCoyMnzMvO2, wherein a sum of x, y and z is 1, x is equal to or larger than 0.2 but smaller than or equal to 0.6; y is equal to or larger than 0.1 but smaller than or equal to 0.4; z is equal to or larger than 0.2 but smaller than or equal to 0.5; v is equal to or larger than 0.01 but smaller than or equal to 0.03; and M is one of Ti, Zn, Cr and F. The preparation method for the ternary positive electrode material with the special single-crystal structure comprises two steps of 1. preparing a precursor-cobalt nickel manganese oxide with the single-crystal structure; and 2. preparing a cobalt nickel manganese ternary material with the single-crystal structure.

Description

Tertiary cathode material of a kind of special mono-crystalline structures and preparation method thereof
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries and preparation method thereof, relate in particular to tertiary cathode material of a kind of special mono-crystalline structures and preparation method thereof.
Background technology
Lithium rechargeable battery becomes more and more important in people's life, is widely used in the source of portable power by people.Than other power source, it has lot of advantages, such as longer useful life, lighter weight, cost are low and environmental friendliness etc.Thereby, lithium battery market trend sustainable growth at home and abroad.
Early stage business-like anode material for lithium-ion batteries mainly concentrates on LiCoO 2, its capacity is lower only a 140mAh/g, this be mainly because material under high voltage condition chemical property and structure all unstable, and cobalt price is higher, poisonous.Except cobalt acid lithium, commercial positive electrode also comprises ternary material, LiMn2O4, LiFePO4 at present.From whole positive electrode product proportion general layout, although cobalt acid lithium at current dominate, from global shipment amount, tertiary cathode material rapid growth just significantly compresses the market ratio of lithium cobaltate cathode material.2012 and the predictable coming years, Chinese Enterprise, Japan and Korea S etc. can be increasing to the use amount of ternary.Ternary is mainly the ternary material of secondary spherical particle in the market, and this material compaction is low, and in production process, secondary ball is easily broken.
Summary of the invention
The object of this invention is to provide the tertiary cathode material of a kind of special mono-crystalline structures of a kind of high power capacity, high-energy-density, excellent cycle performance.
Another object of the present invention is to provide a kind of preparation method of tertiary cathode material of special mono-crystalline structures.
For achieving the above object, the technical solution used in the present invention is: a kind of tertiary cathode material of special mono-crystalline structures, the general formula of this positive electrode is: LiNi xco ymn zm vo 2, wherein x+y+z=1,0.2≤x≤0.6,0.1≤y≤0.4,0.2≤z≤0.5,0.01≤v≤0.03, M is a kind of element in Ti, Zn, Cr, F.
A preparation method for the tertiary cathode material of special mono-crystalline structures, comprises following two steps:
Step 1: prepare presoma, i.e. mono-crystalline structures nickel, cobalt and manganese oxide;
Take in nickel, cobalt, manganese compound water-soluble solution according to mol ratio x:y:z, under the condition constantly stirring, add ammoniacal liquor regulator solution pH, it is between 8 ~ 10 that the value range of pH is controlled at, again this solution is poured in reactor, reactor is put into Muffle furnace sintering, the temperature range of sintering is 300 ~ 500 ℃, and the time of sintering is between 12 ~ 15h, then cooling, clean, grind and obtain presoma;
Step 2: prepare mono-crystalline structures nickel-cobalt-manganese ternary material;
Take the compound of lithium salts, presoma, M according to mol ratio 1:1.0 ~ 1.09:v; lithium salts, presoma are evenly mixed with M compound; carry out again multi-steps sintering; in sintering process, there is atmosphere protection; the temperature curve of sintering is 500 ~ 550 ℃ of sintering 2 ~ 3 hours; 820 ~ 1020 ℃ of sintering 8 ~ 10 hours, cooling, grind, obtain mono-crystalline structures nickel-cobalt-manganese ternary material LiNi xco ymn zm vo 2.
In this preparation method, nickel, cobalt, manganese compound are nickel, cobalt, the manganese of nitrose, the nickel of chloride-based, cobalt, manganese, the nickel of sulfuric acid based, cobalt, manganese, or the nickel of acetic acid class, cobalt, manganese.
In this preparation method, lithium salts is a kind of or its salt-mixture in lithium hydroxide, lithium acetate, lithium carbonate.
In this preparation method, M is the element one in Ti, Zn, Cr, F.
Advantageous effect of the present invention is: due to this preparation method of the present invention, so the ternary material of the mono-crystalline structures of preparation has the following advantages: 1) single crystal grain surface is comparatively smooth, can contact preferably with conductive agent, is beneficial to the transmission of lithium ion; 2) compacting of monocrystalline ternary material is large, and the ternary material compacting of secondary spherical particle is generally 3.6g/cm 3, the compacting of monocrystalline ternary material can reach 3.8 ~ 3.9g/cm 3, its higher compacting can reduce internal resistance, reduces polarization loss, extends battery cycle life, improves the energy content of battery; 3) this material is a special monocrystal particle structure, and specific surface is low, and its representative value is 0.25m 2/ g, in the course of processing, material is difficult for water suction, and is not easy fragmentation in the ternary material electrode compacting process of mono-crystalline structures, has good processing characteristics.
Accompanying drawing explanation
Fig. 1 is the SEM figure of embodiment 1 positive electrode presoma;
Fig. 2 is the cyclic curve figure of embodiment 1 positive electrode sample.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
As described in Fig. 1,2, below by case study on implementation, the present invention is further described, but this is not limitation of the present invention, those skilled in the art can be according to basic ideas of the present invention, make corresponding improvement, only otherwise depart from thinking of the present invention, all in scope of the present invention.
Embodiment 1
Prepare mono-crystalline structures tertiary cathode material LiNi according to the following step 0.25co 0.25mn 0.5f 0.01o 2
1) accurately taking 200 grams of nickelous sulfates, cobaltous sulfate, manganese sulfates according to the mol ratio of Ni:Co:Mn=1:1:2 is dissolved in a certain amount of water, configuration solution, then ammoniacal liquor is slowly dropped in solution, to pH be 9, solution is poured in reactor, reactor is put into 385 ℃ of sintering 17h of Muffle furnace, cooling, clean, dry, grind, obtain mono-crystalline structures presoma, i.e. nickel, cobalt and manganese oxide.
2) according to the mol ratio 1.01:1 of Li and nickel, cobalt, manganese three plain summations, take lithium carbonate, F and nickel, cobalt, the plain summation of manganese three are than taking lithium fluoride for 0.01:1, lithium carbonate, nickel, cobalt and manganese oxide and lithium fluoride are evenly mixed, carry out again multi-steps sintering, nitrogen atmosphere protection in sintering process, 500 ℃ of sintering 3 hours, cooling, grind; 920 ℃ of sintering 11 hours again, cooling, grind, obtain mono-crystalline structures ternary material.
The ternary material of the mono-crystalline structures preparing, as shown in Figure 1.Its first capacitance be 152mAh/g, as shown in Figure 2, efficiency is 82% first, compacting is 3.8g/cm 3.
Embodiment 2
Prepare mono-crystalline structures tertiary cathode material LiNi according to the following step 0.25co 0.25mn 0.5cr 0.02o 2
1) accurately taking 200 grams of nickel nitrates, cobalt nitrate, manganese nitrates according to the mol ratio of Ni:Co:Mn=1:1:2 is dissolved in a certain amount of water, configuration solution, then ammoniacal liquor is slowly dropped in solution, to pH be 9, solution is poured in reactor, reactor is put into 420 ℃ of sintering 15h of Muffle furnace, cooling, clean, dry, grind, obtain mono-crystalline structures presoma, i.e. nickel, cobalt and manganese oxide.
2) according to the mol ratio 1.02:1 of Li and nickel, cobalt, manganese three plain summations, take lithium carbonate, Cr and nickel, cobalt, the plain summation of manganese three are than taking lithium fluoride for 0.02:1, lithium carbonate, nickel, cobalt and manganese oxide and chromic nitrate are evenly mixed, carry out again multi-steps sintering, nitrogen atmosphere protection in sintering process, 500 ℃ of sintering 3 hours, cooling, grind; 920 ℃ of sintering 11 hours again, cooling, grind, obtain mono-crystalline structures ternary material.
The ternary material of the mono-crystalline structures preparing, its first capacitance be 153mAh/g, efficiency is 82.4% first, compacting is 3.8g/cm 3.
Embodiment 3
Prepare mono-crystalline structures tertiary cathode material LiNi according to the following step 0.25co 0.25mn 0.5ti 0.02o 2
1) accurately taking 200 grams of nickel chlorides, cobalt chloride, manganese chlorides according to the mol ratio of Ni:Co:Mn=1:1:2 is dissolved in a certain amount of water, configuration solution, then ammoniacal liquor is slowly dropped in solution, to pH be 9, solution is poured in reactor, reactor is put into 350 ℃ of sintering 17h of Muffle furnace, cooling, clean, dry, grind, obtain mono-crystalline structures presoma, i.e. nickel, cobalt and manganese oxide.
2) according to the mol ratio 1.02:1 of Li and nickel, cobalt, manganese three plain summations, take lithium hydroxide, Cr and nickel, cobalt, the plain summation of manganese three are than taking lithium fluoride for 0.02:1, lithium carbonate, nickel, cobalt and manganese oxide and chromic nitrate are evenly mixed, carry out again multi-steps sintering, nitrogen atmosphere protection in sintering process, 480 ℃ of sintering 3 hours, cooling, grind; 870 ℃ of sintering 11 hours again, cooling, grind, obtain mono-crystalline structures ternary material.
The ternary material of the mono-crystalline structures preparing, its first capacitance be 152mAh/g, efficiency is 84% first, compacting is 3.85g/cm 3.
The preparation method who the invention discloses a kind of monocrystalline ternary anode material for lithium-ion batteries with special construction, by special reaction condition, high temperature, high pressure, alkaline environment first prepare the presoma with mono-crystalline structures; Lithium salts is evenly being mixed with the monocrystalline presoma of special construction, and a small amount of inorganic substances that simultaneously adulterate, improve the degree of crystallinity of material when improving the performance of material; Mixed material is carried out to multi-steps sintering, in the process of sintering, carry out atmosphere protection.

Claims (8)

1. a tertiary cathode material for special mono-crystalline structures, the general formula of this positive electrode is: LiNi xco ymn zm vo 2, wherein x+y+z=1,0.2≤x≤0.6,0.1≤y≤0.4,0.2≤z≤0.5,0.01≤v≤0.03, M is a kind of element in Ti, Zn, Cr, F.
2. a preparation method for the tertiary cathode material of special mono-crystalline structures, comprises following two steps:
Step 1: prepare presoma, i.e. mono-crystalline structures nickel, cobalt and manganese oxide;
Take in nickel, cobalt, manganese compound water-soluble solution according to mol ratio x:y:z, under the condition constantly stirring, add ammoniacal liquor regulator solution pH, it is between 8 ~ 10 that the value range of pH is controlled at, again this solution is poured in reactor, reactor is put into Muffle furnace sintering, the temperature range of sintering is 300 ~ 500 ℃, and the time of sintering is between 12 ~ 15h, then cooling, clean, grind and obtain presoma;
Step 2: prepare mono-crystalline structures nickel-cobalt-manganese ternary material;
Take the compound of lithium salts, presoma, M according to mol ratio 1:1.0 ~ 1.09:v; lithium salts, presoma are evenly mixed with M compound; carry out again multi-steps sintering; in sintering process, there is atmosphere protection; the temperature curve of sintering is 500 ~ 550 ℃ of sintering 2 ~ 3 hours; 820 ~ 1020 ℃ of sintering 8 ~ 10 hours, cooling, grind, obtain mono-crystalline structures nickel-cobalt-manganese ternary material LiNi xco ymn zm vo 2.
3. the preparation method of the tertiary cathode material of a kind of special mono-crystalline structures according to claim 2, comprises following two steps:
Step 1: accurately take 200 grams of nickelous sulfates, cobaltous sulfate, manganese sulfates according to the mol ratio of Ni:Co:Mn=1:1:2 and be dissolved in a certain amount of water, configuration solution, then ammoniacal liquor is slowly dropped in solution to pH be 9, solution is poured in reactor, reactor is put into 385 ℃ of sintering 17h of Muffle furnace, cooling, clean, dry, grind, obtain mono-crystalline structures presoma, i.e. nickel, cobalt and manganese oxide;
Step 2: according to the mol ratio 1.01:1 of Li and nickel, cobalt, manganese three plain summations, take lithium carbonate, F and nickel, cobalt, the plain summation of manganese three are than taking lithium fluoride for 0.01:1, lithium carbonate, nickel, cobalt and manganese oxide and lithium fluoride are evenly mixed, carry out again multi-steps sintering, atmosphere protection in sintering process, 500 ℃ of sintering 3 hours, cooling, grind; 920 ℃ of sintering 11 hours again, cooling, grind, obtain mono-crystalline structures ternary material LiNi 0.25co 0.25mn 0.5f 0.01o 2.
4. the preparation method of the tertiary cathode material of a kind of special mono-crystalline structures according to claim 2, comprises following two steps:
Step 1: accurately take 200 grams of nickel nitrates, cobalt nitrate, manganese nitrates according to the mol ratio of Ni:Co:Mn=1:1:2 and be dissolved in a certain amount of water, configuration solution, then ammoniacal liquor is slowly dropped in solution to pH be 9, solution is poured in reactor, reactor is put into 420 ℃ of sintering 15h of Muffle furnace, cooling, clean, dry, grind, obtain mono-crystalline structures presoma, i.e. nickel, cobalt and manganese oxide;
Step 2: according to the mol ratio 1.02:1 of Li and nickel, cobalt, manganese three plain summations, take lithium carbonate, Cr and nickel, cobalt, the plain summation of manganese three are than taking lithium fluoride for 0.02:1, lithium carbonate, nickel, cobalt and manganese oxide and chromic nitrate are evenly mixed, carry out again multi-steps sintering, atmosphere protection in sintering process, 500 ℃ of sintering 3 hours, cooling, grind; 920 ℃ of sintering 11 hours again, cooling, grind, obtain mono-crystalline structures ternary material LiNi 0.25co 0.25mn 0.5cr 0.02o 2.
5. the preparation method of the tertiary cathode material of a kind of special mono-crystalline structures according to claim 2, comprises following two steps:
Step 1: accurately take 200 grams of nickel chlorides, cobalt chloride, manganese chlorides according to the mol ratio of Ni:Co:Mn=1:1:2 and be dissolved in a certain amount of water, configuration solution, then ammoniacal liquor is slowly dropped in solution to pH be 9, solution is poured in reactor, reactor is put into 350 ℃ of sintering 17h of Muffle furnace, cooling, clean, dry, grind, obtain mono-crystalline structures presoma, i.e. nickel, cobalt and manganese oxide;
Step 2: according to the mol ratio 1.02:1 of Li and nickel, cobalt, manganese three plain summations, take lithium hydroxide, Cr and nickel, cobalt, the plain summation of manganese three are than taking lithium fluoride for 0.02:1, lithium carbonate, nickel, cobalt and manganese oxide and chromic nitrate are evenly mixed, carry out again multi-steps sintering, atmosphere protection in sintering process, 480 ℃ of sintering 3 hours, cooling, grind; 870 ℃ of sintering 11 hours again, cooling, grind, obtain mono-crystalline structures ternary material LiNi 0.25co 0.25mn 0.5ti 0.02o 2.
6. the preparation method of the tertiary cathode material of a kind of special mono-crystalline structures according to claim 5, it is characterized in that: nickel, cobalt, manganese compound are nickel, cobalt, the manganese of nitrose, the nickel of chloride-based, cobalt, manganese, the nickel of sulfuric acid based, cobalt, manganese, or the nickel of acetic acid class, cobalt, manganese.
7. the preparation method of the tertiary cathode material of a kind of special mono-crystalline structures according to claim 6, is characterized in that: lithium salts is a kind of or its salt-mixture in lithium hydroxide, lithium acetate, lithium carbonate.
8. the preparation method of the tertiary cathode material of a kind of special mono-crystalline structures according to claim 7, is characterized in that: M is the element one in Ti, Zn, Cr, F.
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