CN104852043A - High voltage anode material for lithium ion battery and preparation method thereof - Google Patents
High voltage anode material for lithium ion battery and preparation method thereof Download PDFInfo
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- CN104852043A CN104852043A CN201410854801.4A CN201410854801A CN104852043A CN 104852043 A CN104852043 A CN 104852043A CN 201410854801 A CN201410854801 A CN 201410854801A CN 104852043 A CN104852043 A CN 104852043A
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- ion battery
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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
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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
- 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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/52—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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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 high voltage anode material for a lithium ion battery. The chemical formula of a single crystal morphous particle is LiNimConMn(1-m-n)O2, wherein m is greater than or equal to 0.1 and is less than 1, n is greater than or equal to 0 and is less than or equal to 0.5, and m+n is greater than 0 and is less than 1. The anode material is an anode material for the lithium ion battery of single crystal morphous and layered structure. Through accurate control of the particle size of a precursor and a manner of motion roasting, a single crystal morphous ni-co lithium manganite anode material is obtained. Through adoption of a preparation method of the invention, compared with common anode materials, the ni-co lithium manganite anode material maintains the capacity and also effectively improves the high voltage cycling stability and heat stability, and has the advantage of higher cost performance, so that the high voltage anode material of the lithium ion battery is likely to be used extensively.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, specifically a kind of high-voltage lithium-battery cathode material of monocrystalline pattern, and the preparation method of this positive electrode.
Background technology
Lithium ion battery is as a kind of novel green high-energy battery, because having, operating voltage is high, specific capacity is large, have extended cycle life, self-discharge rate is low, memory-less effect and the advantage such as environmentally friendly and be widely used, positive electrode is then the key of lithium ion battery technology, the positive electrode of lithium ion battery, must meet following requirement: (1) high-energy-density; (2) during electric discharge, change in voltage is little, namely should have stable discharge platform; (3) high power density; (4) remarkable cycle performance; (5) environmental friendliness; (6) low price.Along with lithium ion battery is in electric automobile, cordless power tool and military application, the energy density of positive electrode has been suggested higher requirement.Because energy density is the comprehensive embodiment of voltage and capacity, so there is high voltage and jumbo cell positive material seems particularly important simultaneously.
The discharge and recharge interval of business-like lithium ion battery is substantially all between 3.0V ~ 4.2V, seldom there is business-like lithium ion battery can use the charging voltage of 4.4V, use cobalt acid lithium or ternary material can carry out the charging of 4.4V as the lithium ion battery of positive electrode, and improve the discharge capacity that the charging voltage of lithium ion battery also obviously can increase battery, cobalt acid lithium as the lithium ion lithium cell charging of positive pole to the capacity that can increase about 14.0% during 4.4V.But from current application result, mainly there is the problem of thermal stability and security performance decline in the lithium ion battery of cobalt acid lithium, and the lithium ion battery of common nickel-cobalt lithium manganate material mainly exists the problem that cycle performance obviously worsens under the voltage charging of 4.4V under 4.4V high voltage.Charging voltage is brought up to 4.4V, LiNi
0.5co
0.2mn
0.3o
2capacity can reach 190mAh/g, but cycle performance will significantly be decayed, and there will be serious flatulence phenomenon.
For improving the comprehensive electrochemical problem that lithium ion battery exists under above-mentioned high voltage, there are some material suppliers to adopt at present and modification is carried out to improve this stability under higher charging voltage of material to its material.The method of modification mainly contains Surface coating, bulk phase-doped and pattern control.Pattern controls side reaction and the dissolving that can reduce material and electrolyte, increases the stability of material.
Summary of the invention
Technical problem to be solved by this invention is, provide a kind of energy density large, high rate performance is good, and cost is low, and fail safe is good, long service life under high voltage, the anode material of lithium battery that the powder granule of the lamellar single crystal structure that compacted density is high is formed.Wherein the chemical formula of monocrystalline pattern particle is LiNi
mco
nmn
1-m-no
2, wherein: 0.1≤m<1; 0≤n≤0.5,0<m+n<1, the pattern of this material is the little single crystal grain of even particle size distribution.The particle size distribution of particle is 3.0≤D
10≤ 6.0; 6.0≤D
50≤ 13.0; 10.0≤D
90≤ 20.0; 1.0≤(D
90-D
10)/D
50≤ 2.0.
The preparation method of a kind of high-voltage lithium ion battery cathode material that the present invention proposes, step is as follows:
Step one, stratiform (Ni
mco
nmn
1-m-n) (OH)
2the preparation of presoma, comprising:
1-1, with the nickel cobalt manganese material salting liquid 1-100L of the proportions 0.5-2.5M of mol ratio Ni:Co:Mn=m:n:1-m-n, wherein, 0.1≤m<1; 0≤n≤0.5; 0<m+n<1;
1-2, in reactor, at the uniform velocity add this salting liquid prepared with the speed of 0.01-1L/min, under the condition of pH value at 10-12, carry out coprecipitation reaction by the sodium hydroxide solution of 2-10M and obtain presoma solidliquid mixture, precipitated solid molecular formula is (Ni
mco
nmn
1-m-n) (OH)
2wherein, 0.1≤m<1; 0≤n≤0.5; 0<m+n<1;
1-3, stopping reaction after all salting liquids inject reactor completely, solidliquid mixture is separated by centrifugal filtration, washs and at 80-200 DEG C, dry 4-10h to neutrality, obtains molecular formula for (Ni
mco
nmn
1-m-n) (OH)
2(wherein, 0.1≤m<1; 0≤n≤0.5; Presoma 0<m+n<1);
Step 2, prepare granule ternary precursor, comprising:
Above-mentioned presoma is broken for the particle that particle diameter is 0.5-3 μm by 2-1, use pulverizer, uses dispersant to reunite to avoid fine particle in shattering process;
Presoma after 2-2, fragmentation is 120 DEG C of oven dry;
Step 3, prepare monocrystalline oxide particle, comprising:
The granule presoma that step 2 is obtained is placed in Muffle furnace and carries out presintering process by 3-1, and its treatment temperature is 700-1200 DEG C;
The further fragmentation of granule presoma after presintering process is sieved and is obtained monocrystalline oxide particle by 3-2, and its molecular formula is (Ni
mco
nmn
1-m-n)
2o
3, wherein, 0.1≤m<1; 0≤n≤0.5; 0<m+n<1;
Step 4, prepare monocrystalline LiNi
mco
nmn
1-m-no
2particle;
4-1, take the obtained monocrystalline oxide particle of step 3, and take lithium salts according to the mol ratio of Li:M=1.05-1.20, wherein, M is transition metal;
4-2, be 1:(1 ~ 2 according to the mass ratio of monocrystalline oxide particle and lithium salts gross mass and batch mixing ball) ratio take batch mixing ball;
4-3, the monocrystalline oxide particle weighed up is put into batch mixer with lithium salts together with batch mixing ball, batch mixing 2-8 hour, until monocrystalline oxide particle and lithium salts mix;
4-4, the above-mentioned monocrystalline oxide particle that mixes and lithium salts be placed in Muffle furnace carry out multistage roasting, its sintering temperature 300-1200 DEG C, roasting time 8-30h, after multistage roasting through cooling, broken, sieving obtains the powder granule LiNi of monocrystalline pattern
mco
nmn
1-m-no
2.
Further, the nickel cobalt manganese material salting liquid in step 1-1, comprises nickel salt, cobalt salt and manganese salt and is sulfate soluble in water, chlorate, nitrate, acetate.
In step 2, described dispersant is copolymer containing acidic-group or solution, selects the one in BYK-W995, BYK-W996, BYK-W972, BYK-9010 of German Bi Ke company.
In step 4, described lithium salts easily decomposes the lithium salts reacted with presoma under adopting high temperature, select the one in lithium carbonate, lithium hydroxide, lithium nitrate and lithium acetate, described monocrystalline oxide with adopt hard medium to impel in the mixed process of lithium source to mix, described hard medium comprises zirconium ball and corundum ball.
Step 2 is in step 4, and shattering process all uses hard medium, and described hard medium comprises zirconium ball and corundum ball.
Positive electrode of the present invention has following advantage compared with traditional anode material of lithium battery: 1, monocrystalline pattern makes this material have more outstanding high voltage stability than common material; 2, the material compacted density of monocrystalline pattern is compared common ternary material and is improve 0.1-0.2g/ml.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the embodiment of the present invention 1 and comparative example 1;
Fig. 2 is that the embodiment of the present invention 1 is schemed with the XRD of comparative example 1;
Fig. 3 is the first charge-discharge curve chart of the embodiment of the present invention 1 and comparative example 1;
Fig. 4 is 150 1C cyclic curve figure of the embodiment of the present invention 1 and comparative example 1;
Fig. 5 is that the embodiment of the present invention 1 charges to the DSC curve chart after 4.5V with comparative example 1.
Embodiment
Tell about detailed process of the present invention by the following examples, provide embodiment to be convenience in order to understand, is never restriction the present invention.
Comparative example 1:
With the salting liquid 30L that 7967g nickelous sulfate, 3450g cobaltous sulfate, 3043g manganese sulfate compound concentration are 2M.The solution prepared is injected with the speed of 1L/h the reactor that rotating speed is 500rps, injects the NaOH solution of 10M simultaneously, note regulating aqueous slkali flow velocity, keep pH value between 11-12, salting liquid injects reactor completely, and precursor power has reacted.By the solidliquid mixture after having reacted by centrifugation, wash and at 120 DEG C, dry 6h to neutrality.After presoma after drying is mixed by Li and transition metal mole ratio 1:1.05 with lithium carbonate in Muffle furnace 950 DEG C of roasting 16h, material after roasting sieves through fragmentation and obtains homogeneous spherical granular material LiNi
0.5co
0.2mn
0.3o
2.
Embodiment 1:
Presoma high speed ball mill obtained in comparative example 1 is ground 4 hours, BYK-W995 auxiliary agent is adopted when grinding, presoma after grinding is put into Muffle furnace 800 DEG C sintering 5 hours, presoma after process is mixed with lithium carbonate, puts into Muffle furnace 980 DEG C after mixing according to the ratio of lithium and transition metal mole ratio 1.08:1 and sinter 10 hours.Material after roasting obtains the LiNi of homogeneous monocrystalline pattern through broken sieving
0.5co
0.2mn
0.3o
2.
As shown in Figure 1, from SEM, the pattern of visual contrast example 1 is good secondary ball particle, particle diameter about 9 μm, tap density is 2.5g/ml, the monocrystalline that embodiment 1 primary particle is larger is closely reunited together, primary particle particle diameter is about 4 μm, and the aggregate particle size after reunion is about 9 μm, and tap density is 2.7g/ml; Can find out that comparative example 1 and embodiment 1 all do not find assorted peak from the XRD curve comparison figure of Fig. 2, crystal structure is complete; As shown in Figure 3, after 2032 button cells made by embodiment 1 and comparative example 1 material, in the voltage range of 3.0-4.4V, under 0.1C multiplying power electric current, first discharge specific capacity is respectively 188.3mAh/g and 188.7mAh/g; Fig. 4 display be the circulation comparison diagram of comparative example 1 and embodiment 1, comparative example 1 capacity only surplus 93mAg/g after 1C multiplying power current charge-discharge electricity circulation 150 circle, and the specific discharge capacity of embodiment 1 can remain to 147.3mAh/g; The DSC curve chart be charged to after 4.5V of Fig. 5 display, as shown in the figure, embodiment 1 thermal decomposition initial temperature in DSC test is 240 DEG C, and improve obviously than 180 DEG C of comparative example 1, thermal discharge significantly reduces simultaneously.
Comparative example 2:
With the salting liquid 30L that 5311g nickelous sulfate, 5749g cobaltous sulfate, 3381g manganese sulfate compound concentration are 2M.The solution prepared is injected with the speed of 1L/h the reactor that rotating speed is 500rps, injects the NaOH solution of 10M simultaneously, note regulating aqueous slkali flow velocity, keep pH value between 11-12, inject reactor completely to salting liquid, precursor power has reacted.By the solidliquid mixture after having reacted by centrifugation, wash and at 120 DEG C, dry 6h to neutrality.After presoma after drying is mixed by Li and transition metal mole ratio 1:1.05 with lithium carbonate in Muffle furnace 950 DEG C of roasting 16h, material after roasting sieves through fragmentation and obtains homogeneous spherical granular material LiNi
1/3co
1/3mn
1/3o
2.
Embodiment 2:
Presoma high speed ball mill obtained in comparative example 1 is ground 4 hours, BYK-W995 auxiliary agent is adopted when grinding, presoma after grinding is put into Muffle furnace 800 DEG C sintering 5 hours, presoma after process is mixed with lithium carbonate, puts into Muffle furnace 1000 DEG C after mixing according to the ratio of lithium and transition metal mole ratio 1.08:1 and sinter 10 hours.Material after roasting obtains the LiNi of homogeneous monocrystalline pattern through broken sieving
1/3co
1/3mn
1/3o
2.
Embodiment 2 and comparative example 2 material to be made after 2032 button cells within the scope of 3.0-4.4V, and the capability retention after 100 times that circulates under 1C multiplying power electric current is respectively 88% and 75%.
In sum, the nickle cobalt lithium manganate synthesis process of monocrystalline pattern prepared by the method using the present invention to state is simple, lower to equipment requirement, is applicable to suitability for industrialized production.The nickel-cobalt lithium manganate material normal temperature circulation of preparing and high temperature circulation, stability can all be better than common spherical nickel-cobalt lithium manganate material.
Although invention has been described for composition graphs above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; when not departing from present inventive concept, can also make a lot of distortion, these all belong within protection of the present invention.
Claims (9)
1. a high-voltage lithium ion battery cathode material, is characterized in that: its chemical formula is LiNi
mco
nmn
1-m-no
2, wherein, 0.1≤m<1; 0≤n≤0.5; 0<m+n<1.
2. high-voltage lithium ion battery cathode material according to claim 1, is characterized in that, the pattern of this material is the little single crystal grain of even particle size distribution.
3. high-voltage lithium ion battery cathode material according to claim 2, is characterized in that: the particle size distribution of particle is 3.0≤D
10≤ 6.0; 6.0≤D
50≤ 13.0; 10.0≤D
90≤ 20.0; 1.0≤(D
90-D
10)/D
50≤ 2.0.
4. the preparation method of high-voltage lithium ion battery cathode material as described in claims 1 to 3, is characterized in that: concrete steps are as follows:
Step one, stratiform (Ni
mco
nmn
1-m-n) (OH)
2the preparation of presoma, comprising:
1-1, with the nickel cobalt manganese material salting liquid 1-100L of the proportions 0.5-2.5M of mol ratio Ni:Co:Mn=m:n:1-m-n, wherein, 0.1≤m<1; 0≤n≤0.5; 0<m+n<1;
1-2, in reactor, at the uniform velocity add this salting liquid prepared with the speed of 0.01-1L/min, under the condition of pH value at 10-12, carry out coprecipitation reaction by the sodium hydroxide solution of 2-10M and obtain presoma solidliquid mixture, precipitated solid molecular formula is (Ni
mco
nmn
1-m-n) (OH)
2wherein, 0.1≤m<1; 0≤n≤0.5; 0<m+n<1;
1-3, stopping reaction after all salting liquids inject reactor completely, solidliquid mixture is separated by centrifugal filtration, washs and at 80-200 DEG C, dry 4-10h to neutrality, obtains molecular formula for (Ni
mco
nmn
1-m-n) (OH)
2(wherein, 0.1≤m<1; 0≤n≤0.5; Presoma 0<m+n<1);
Step 2, prepare granule ternary precursor, comprising:
Above-mentioned presoma is broken for the particle that particle diameter is 0.5-3 μm by 2-1, use pulverizer, uses dispersant to reunite to avoid fine particle in shattering process;
Presoma after 2-2, fragmentation is 120 DEG C of oven dry;
Step 3, prepare monocrystalline oxide particle, comprising:
The granule presoma that step 2 is obtained is placed in Muffle furnace and carries out presintering process by 3-1, and its treatment temperature is 700-1200 DEG C;
The further fragmentation of granule presoma after presintering process is sieved and is obtained monocrystalline oxide particle by 3-2, and its molecular formula is (Ni
mco
nmn
1-m-n)
2o
3, wherein, 0.1≤m<1; 0≤n≤0.5; 0<m+n<1;
Step 4, prepare monocrystalline LiNi
mco
nmn
1-m-no
2particle;
4-1, take the obtained monocrystalline oxide particle of step 3, and take lithium salts according to the mol ratio of Li:M=1.05-1.20, wherein, M is transition metal;
4-2, be 1:(1 ~ 2 according to the mass ratio of monocrystalline oxide particle and lithium salts gross mass and batch mixing ball) ratio take batch mixing ball;
4-3, the monocrystalline oxide particle weighed up is put into batch mixer with lithium salts together with batch mixing ball, batch mixing 2-8 hour, until monocrystalline oxide particle and lithium salts mix;
4-4, the above-mentioned monocrystalline oxide particle that mixes and lithium salts be placed in Muffle furnace carry out multistage roasting, its sintering temperature 300-1200 DEG C, roasting time 8-30h, after multistage roasting through cooling, broken, sieving obtains the powder granule LiNi of monocrystalline pattern
mco
nmn
1-m-no
2.
5. the preparation method of high-voltage lithium ion battery cathode material according to claim 4, it is characterized in that, the nickel cobalt manganese material salting liquid in step 1-1, comprises nickel salt, cobalt salt and manganese salt and is sulfate soluble in water, chlorate, nitrate, acetate.
6. the preparation method of high-voltage lithium ion battery cathode material according to claim 4, it is characterized in that, in step 2, described dispersant is copolymer containing acidic-group or solution, selects the one in BYK-W995, BYK-W996, BYK-W972, BYK-9010 of German Bi Ke company.
7. the preparation method of high-voltage lithium ion battery cathode material according to claim 4, it is characterized in that, in step 4, described lithium salts easily decomposes the lithium salts reacted with presoma under adopting high temperature, selects the one in lithium carbonate, lithium hydroxide, lithium nitrate and lithium acetate.
8. the preparation method of high-voltage lithium ion battery cathode material according to claim 4, it is characterized in that, step 2 is in step 4, and shattering process all uses hard medium, and described hard medium comprises zirconium ball and corundum ball.
9. the preparation method of high-voltage lithium ion battery cathode material according to claim 4, is characterized in that, in step 4, described monocrystalline oxide with adopt hard medium to impel in the mixed process of lithium source to mix, described hard medium comprises zirconium ball and corundum ball.
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| CN106229489A (en) * | 2016-08-29 | 2016-12-14 | 青海泰丰先行锂能科技有限公司 | A kind of high voltage ternary lithium ion anode material of monocrystalline pattern and preparation method thereof |
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| CN109153582A (en) * | 2016-05-27 | 2019-01-04 | 尤米科尔公司 | The manufacturing method of the nickel lithium metal composite oxide powder of small particle |
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