CN103280574A - Lithium-enriched ternary anode material of power lithium-ion battery and preparation method of lithium-enriched ternary anode material - Google Patents
Lithium-enriched ternary anode material of power lithium-ion battery and preparation method of lithium-enriched ternary anode material Download PDFInfo
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Abstract
The invention discloses a lithium-enriched ternary anode material of a power lithium-ion battery and a preparation method of the lithium-enriched ternary anode material. The molecule formula of the lithium-enriched ternary anode material of the power lithium-ion battery is Li1.2Ni0.13Co0.13Mn0.54O2. The preparation method comprises the following steps of: dissolving lithium acetate, cobaltous acetate, nickel acetate and manganese acetate in deionized water according to the molar ratio of Li: Co: Ni: Mn: O being 1.2: 0.13: 0.13: 0.54: 2 to obtain a solution 1; adding citric acid according to the ratio of the molar weight of the citric acid to the total molar weight of Ni, Co and Mn being 1:1 to obtain a solution 2; dropwise adding the solution 2 into the solution 1, and then adjusting the pH value to 9, continuously stirring the solution at the temperature of 80 DEG C until purple gel is formed, and then sequentially drying, ball milling, calcining segment by segment and grinding to obtain the lithium-enriched ternary anode material of the power lithium-ion battery with large discharging specific capacity and good cycling performance.
Description
Technical field
The invention belongs to the anode material for lithium-ion batteries preparing technical field, be specifically related to rich lithium tertiary cathode material of a kind of power-type lithium ion battery and preparation method thereof.
Background technology
Performances such as the electric weight of anode material for lithium-ion batteries, voltage are the key factors that influences energy content of battery density, security performance and cycle life.At present, business-like anode material for lithium-ion batteries LiCoO on the market
2, LiFePO
4Capacity be respectively 140mAh/g, 160mAh/g, the anode material for lithium-ion batteries of therefore developing high power capacity becomes exigence.Since U.S. Argonne National Laboratory has applied for rich lithium layered cathode material patent in calendar year 2001, this kind material relies on its height ratio capacity (greater than 200mAh/g), excellent cycle performance, cost lower (cobalt element content is low), advantages of environment protection has obtained extensive concern, and has bright development prospect.
The rich lithium tertiary cathode material of lithium ion battery is as Li
1.2Ni
0.175Co
0.1Mn
0.525O
2, Li
1.2Ni
0.2Mn
0.6O
2Deng, the most frequently used preparation method is solid reaction process, but is to use the material of this method preparation can not reach mixed uniformly level, and introduces impurity in the process of preparation easily, can produce bigger influence to the chemical property of material.Therefore, can adopt some other softening method to improve the chemical property of material, generally comprise sol-gel process, spray drying process, hydro thermal method etc.Wherein, it is good that the Prepared by Sol Gel Method positive electrode has a chemical uniformity, narrow diameter distribution, purity height, advantage such as grain diameter is little.But also exist some shortcomings:
(1) often need in the preparation process to consume a large amount of expensive organic acid or alcohol, cost is higher, is unsuitable for large-scale production.
(2) whole process of preparation needs the ageing process of a long period, and time cost is too high.
(3) when presoma is calcined, traditional calcine technology adopts the one-step calcination method, and calcination time is long, is generally 20h, therefore the energy is produced waste.
Therefore the present invention provides the rich lithium tertiary cathode material of a kind of power-type lithium ion battery Li in order to solve this technical problem
1.2Ni
0.13Co
0.13Mn
0.54O
2Novel preparation method.
Summary of the invention
Purpose of the present invention is in order to solve on the market business-like anode material for lithium-ion batteries LiCoO
2, LiFePO
4The defective that capacity is low and provide a kind of power-type lithium ion battery rich lithium tertiary cathode material.
Two of purpose of the present invention is for the preparation method of the rich lithium tertiary cathode material of above-mentioned a kind of power-type lithium ion battery is provided.
Know-why of the present invention
Be raw material with lithium acetate, cobalt acetate, nickel acetate and manganese acetate, citric acid is that chelating agent has synthesized the precursor of the rich lithium tertiary cathode material of power-type lithium ion battery and obtained the rich lithium tertiary cathode material of power-type lithium ion battery by a minute section calcining.
Technical scheme of the present invention
The rich lithium tertiary cathode material of a kind of power-type lithium ion battery, its molecular formula is Li
1.2Ni
0.13Co
0.13Mn
0.54O
2
The preparation method of the above-mentioned rich lithium tertiary cathode material of a kind of power-type lithium ion battery, namely calculate at first in molar ratio, it is the ratio of Li:Co:Ni:Mn:O=1.2:0.13:0.13:0.54:2, lithium acetate, cobalt acetate, nickel acetate and manganese acetate are dissolved in the deionized water, obtain solution 1, used lithium acetate is excessive 5% in the actual fabrication process, the loss of lithium when remedying follow-up calcining;
Calculate in molar ratio, namely the integral molar quantity of the mole of citric acid: Ni, Co and Mn is the ratio of 1:1, and citric acid is joined in the deionized water, obtains solution 2 again;
Then, be added drop-wise to solution 2 in the solution 1 and after mixing, with mass percentage concentration be 28% ammoniacal liquor to regulate pH be 9, continue down to stir until forming purple gel at 80 ℃;
Then, use ball mill with its ball milling after the oven dry down at 200 ℃ the purple gel that obtains, namely get the precursor pressed powder;
At last, the precursor pressed powder that obtains is carried out the branch section calcining, the material after the calcining is ground, namely get the rich lithium tertiary cathode material of power-type lithium ion battery.
The above-mentioned rich lithium tertiary cathode material of a kind of power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2The preparation method, specifically comprise the steps:
(1), calculates in molar ratio, be the ratio of Li:Co:Ni:Mn:O=1.2:0.13:0.13:0.54:2 with lithium acetate, nickel acetate cobalt acetate and manganese acetate, be dissolved in the deionized water, form solution 1, wherein used lithium acetate is excessive 5%, the loss of lithium when remedying follow-up calcining;
(2), in molar ratio calculate, namely the ratio of the integral molar quantity of the mole of citric acid: Ni, Co and Mn is 1:1, and citric acid as chelating agent, is dissolved in the deionized water, forms solution 2;
(3), the control drop rate is 2ml/min, solution 2 is dropwise added in the solution 1, then with mass percentage concentration be 28% ammoniacal liquor to regulate pH be 9, the control temperature is 80 ℃ and continues down to stir until forming purple gel;
(4), the purple gel of gained is transferred to after the oven dry down in 200 ℃ carries out ball milling in the ball mill, namely get the precursor pressed powder;
(5), the precursor pressed powder of step (4) gained being controlled temperature in high temperature process furnances is 400 ℃ and carries out precalcining 4h, speed with 5 ℃/min is warming up to 900 ℃ of calcining 8h then, grind fully after the calcining, namely get the rich lithium tertiary cathode material of power-type lithium ion battery.
Beneficial effect of the present invention
The rich lithium tertiary cathode material of a kind of power-type lithium ion battery of the present invention, capacity is higher, and after the circulation 50 times, residual capacity is about 250.5mAh/g, than the LiCoO of commerce under the low range
2Almost exceed one times.Its irreversible capacity loss only is 23mAh/g, and the cycle performance excellence becomes and is expected to substitute LiCoO
2Anode material for lithium-ion batteries of new generation.
Further, the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery of the present invention, owing to adopt the novel sol-gal process under the certain material proportioning, namely utilize lithium acetate, cobalt acetate, nickel acetate and manganese acetate to be raw material, citric acid is that chelating agent has synthesized the rich lithium tertiary cathode material of power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Precursor, and prepare the rich lithium tertiary cathode material of power-type lithium ion battery Li by novel calcine technology
1.2Ni
0.13Co
0.13Mn
0.54O
2, as its well-formed of electrode material, grain diameter is little, is evenly distributed, and battery performance is good.
Further, the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery of the present invention, owing to added the organic acid citric acid as chelating agent, each raw material is evenly mixed in the molecule rank, it is good to have chemical uniformity, the presoma narrow diameter distribution of final gained, purity height, advantages such as grain diameter is little are conducive to follow-up calcination process.
Further, the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery of the present invention compares with traditional sol-gal process, this method adopts citric acid as chelating agent, its consumption only is traditional 40%, greatly reduces production cost, is conducive to realize large-scale production.
Further, the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery of the present invention, because, owing to adopt magnetic agitation only to need 4h just can obtain purple gel shape material, obtain the required digestion time of gel thereby reduced, improved production efficiency.
Further, the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery of the present invention, owing to adopt to divide section calcining, namely the control temperature is 400 ℃ and carries out precalcining 4h that the speed with 5 ℃/min is warming up to 900 ℃ of calcining 8h then in high temperature process furnances.Compare with traditional calcine technology, its calcination time only is traditional 60%, thereby has reduced the loss of the energy, has also further reduced production cost.
In sum, the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery of the present invention, production cost is low, the production efficiency height, be conducive to realize large-scale production, the rich lithium tertiary cathode material of the power-type lithium ion battery of gained capacity is higher, under the low range circulation 50 times after, residual capacity is about 250.5mAh/g, and its irreversible capacity loss only is 23mAh/g, the cycle performance excellence, as its well-formed of electrode anode material, grain diameter is little, is evenly distributed, and battery performance is good.
Description of drawings
Fig. 1, the rich lithium tertiary cathode material of embodiment 1 gained power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2The XRD picture;
Fig. 2 a, the rich lithium tertiary cathode material of embodiment 1 gained power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Multiplication factor is 5000 times of SEM pictures that obtain down;
Fig. 2 b, the rich lithium tertiary cathode material of embodiment 1 gained power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Multiplication factor is 10000 times of SEM pictures that obtain down;
Fig. 3, the rich lithium tertiary cathode material of power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2 Cyclic voltammetry curve 3 times, sweep limits be 2.5V to 4.8V, sweep speed is 0.1mV/s;
Fig. 4, the rich lithium tertiary cathode material of power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Preceding 50 charging and discharging capacities after the assembled battery under the 0.2C multiplying power and enclosed pasture efficiency curve;
Fig. 5, the rich lithium tertiary cathode material of power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2After the assembled battery first with the 50th charging and discharging capacity curve.
Embodiment
Also by reference to the accompanying drawings the present invention is further set forth below by specific embodiment, but do not limit the present invention.
The rich lithium tertiary cathode material of a kind of power-type lithium ion battery, its molecular formula is Li
1.2Ni
0.13Co
0.13Mn
0.54O
2
The above-mentioned rich lithium tertiary cathode material of a kind of power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2The preparation method, specifically comprise the steps:
(1), with the 3.2136g lithium acetate, the 0.8302g cobalt acetate, the 0.8294g nickel acetate, the 3.2678g manganese acetate is dissolved in the deionized water, forms solution 1;
The amount of above-mentioned used lithium acetate, nickel acetate cobalt acetate and manganese acetate is pressed the mol ratio of Li:Co:Ni:Mn:O and is calculated, and namely Li:Co:Ni:Mn:O is 1.26:0.13:0.13:0.54:2;
Above-mentioned used lithium acetate is excessive 5%, the loss of lithium when remedying follow-up calcining;
(2), with 4.2028g citric acid citric acid, be dissolved in the deionized water, form solution 2;
The amount of above-mentioned used citric acid, calculate in molar ratio, i.e. the mole of citric acid: the ratio of the integral molar quantity of transition metal ions Ni, Co and Mn is 1:1;
(3), the control drop rate is 2ml/min, solution 2 is dropwise added in the solution 1, be that 28% ammoniacal liquor is regulated pH and is 9,80 ℃ and continues to stir 4h at the magnetic force heating stirrer with mass percentage concentration then, until forming purple gel;
(4), the purple gel of step (3) gained is put into baking oven, at 200 ℃ of oven dry 12h, in the process of oven dry, gel can be expanded to sphere gradually, its volume is the several times of gel, and obtaining the precursor solid transfer, to be milled to particle diameter to the ball mill be 150-300nm, namely gets the precursor pressed powder;
(5), the precursor pressed powder of step (4) gained being controlled temperature in the high-temperature tubular furnace system is 400 ℃ and carries out precalcining 4h, speed with 5 ℃/min is warming up to 900 ℃ of calcining 8h then, material after the calcining is ground to particle diameter in mortar be 100-250nm, namely gets the rich lithium tertiary cathode material of power-type lithium ion battery Li
1.2Ni
0.13Co
0.13Mn
0.54O
2
The rich lithium tertiary cathode material of power-type lithium ion battery Li with above-mentioned gained
1.2Ni
0.13Co
0.13Mn
0.54O
2Utilize X-ray diffractometer (D8-ADVANCE type, German Bruker company produces) scanning, scanning result as shown in Figure 1, as can be seen from Figure 1, it is sharp-pointed that it goes out the peak, and it is obvious that (006)/(012) and (108)/(110) split the peak, and (003) is to the ratio of (104) peak strength
I (003)/
I (104)Greater than 1.2, shown the positive electrode material of multi-component composite lithium ion cell Li of the rich lithium of embodiment 1 gained thus
1.2Ni
0.13Co
0.13Mn
0.54O
2Has good layer structure.
The rich lithium tertiary cathode material of the power-type lithium ion battery of above-mentioned gained Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Observe by scanning electron microscopy (JSM-5900 type, Japanese JEOL company produces), it is that 5000,10000 times of SEM figure that obtain down see respectively shown in Fig. 2 a, Fig. 2 b in multiplication factor; From Fig. 2 a, Fig. 2 b, find out the rich lithium tertiary cathode material of the power-type lithium ion battery of embodiment 1 gained Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Particle is spherical and is evenly distributed.
Application Example 1
The rich lithium tertiary cathode material of power-type lithium ion battery Li with embodiment 1 gained
1.2Ni
0.13Co
0.13Mn
0.54O
2Be assembled into battery, number of assembling steps is as follows:
1, the preparation of anode pole piece
The rich lithium tertiary cathode material of power-type lithium ion battery Li with embodiment 1 gained
1.2Ni
0.13Co
0.13Mn
0.54O
2, conductive agent Super-p and binding agent PVDF be that the ratio of 80:10:10 is mixed in mass ratio, place then and stir into uniform sizing material on the magnetic stirring apparatus, evenly coat on the aluminium foil, behind 100 ℃ of air drying 2h, making diameter is the circular anode pole piece of 14mm;
2, the preparation of battery cathode
Scrape off high-purity lithium sheet surface oxide layer in the glove box of drying, the metal surface of exposing gloss namely gets battery cathode;
3, button Experimental cell assembling
In being full of the vacuum glove box of argon gas, be assembled into CR2016 type button cell.Electrolyte is LiPF
6/ EC (ethylene carbonate)+DMC (dimethyl carbonate) (volume ratio is 1:1), metal lithium sheet is battery cathode, barrier film is the Celgard2400 polypropylene film.In CR2016 type button cell anode cover, put into anode pole piece, barrier film is covered on the anode pole piece, after dripping electrolyte, be that battery cathode places on the barrier film gently again with metal lithium sheet, put into the nickel foam as backing material again, the battery cathode cap to anode cover, and then is assembled into CR2016 type button Experimental cell.
The CR2016 type button Experimental cell for preparing is connected on the CHI660C electrochemical workstation, and work electrode connects anode, and reference electrode and be lithium metal to electrode carries out the cyclic voltammetric test, and concrete outcome is seen Fig. 3.
Fig. 3 is the rich lithium tertiary cathode material of the power-type lithium ion battery Li of embodiment 1 gained
1.2Ni
0.13Co
0.13Mn
0.54O
2 Cyclic voltammetry curve 3 times, sweep limits be 2.5V to 4.8V, sweep speed is 0.1mV/s.
As can be seen from Figure 3, the redox peak is compared with back 2 times and is had significantly skew in the cyclic process for the first time, and the rich lithium tertiary cathode material of charge and discharge process medium power type lithium ion battery generation irreversible transition for the first time is described, causes irreversible capacity loss.Later first cyclic voltammetry curve is overlapping substantially, illustrates that invertibity is good, and in this discharged and recharged the interval, the electro-chemical activity of the rich lithium tertiary cathode material of power-type lithium ion battery was good.
The rich lithium tertiary cathode material of the power-type lithium ion battery of embodiment 1 gained Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Battery performance by the assembling after CR2016 type button cell, CT2001A tests at the LAND battery test system, adopts the multiplying power condition of 0.1C, 0.2C and 0.5C to test respectively.Test result is seen Fig. 4 and Fig. 5.
Fig. 4 is the rich lithium tertiary cathode material of the power-type lithium ion battery Li of embodiment 1 gained
1.2Ni
0.13Co
0.13Mn
0.54O
2Be assembled into preceding 50 the charge and discharge specific capacities under the 0.2C multiplying power and enclosed pasture efficient (i.e. efficiency for charge-discharge among a figure) curve behind the button Experimental cell.As can be seen from Figure 4,0.2C discharges and recharges the rich lithium tertiary cathode material of the power-type lithium ion battery Li of embodiment 1 gained under the condition
1.2Ni
0.13Co
0.13Mn
0.54O
2Charge and discharge specific capacity first be 347.2mAh/g and 255.3mAh/g, 50 times circulation back residual capacity is 231.6mAh/g, capability retention is 90.71%.
Fig. 5 is the rich lithium tertiary cathode material of the power-type lithium ion battery Li of embodiment 1 gained
1.2Ni
0.13Co
0.13Mn
0.54O
2Be assembled into behind the button Experimental cell under the 0.2C multiplying power first with the 50th charging and discharging capacity.Among Fig. 5,1 for charging curve first, 2 for discharge curve, 3 first be that the 50th charging curve, 4 is the 50th discharge curve.Initial charge curve from Fig. 5 as can be seen, there is tangible 4.5V high-voltage charge platform in the rich lithium tertiary cathode material of embodiment 1 gained power-type lithium ion battery, 50 times its irreversible capacity loss of circulation back only be 23.7mAh/g, has shown that thus the battery performance of power-type lithium ion battery richness lithium tertiary cathode material of embodiment 1 gained is good.
In sum, the rich lithium tertiary cathode material of the power-type lithium ion battery of a kind of gained provided by the invention Li
1.2Ni
0.13Co
0.13Mn
0.54O
2Have that specific discharge capacity is big, cycle performance is good, production cost is low, and the advantage of energy savings is conducive to realize industrial-scale production.
The above only is giving an example of embodiments of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (5)
1. the rich lithium tertiary cathode material of power-type lithium ion battery is characterized in that the molecular formula of the rich lithium tertiary cathode material of described power-type lithium ion battery is Li
1.2Ni
0.13Co
0.13Mn
0.54O
2
2. the preparation method of the rich lithium tertiary cathode material of power-type lithium ion battery as claimed in claim 1 is characterized in that comprising the steps:
Calculate at first in molar ratio, namely the ratio of Li:Co:Ni:Mn:O=1.2:0.13:0.13:0.54:2 is dissolved in lithium acetate, cobalt acetate, nickel acetate and manganese acetate in the deionized water, obtains solution 1;
Calculate in molar ratio, namely the integral molar quantity of the mole of citric acid: Ni, Co and Mn is the ratio of 1:1, and citric acid is joined in the deionized water, obtains solution 2 again;
Be added drop-wise to solution 2 in the solution 1 and after mixing, regulating pH with ammoniacal liquor is 9, continues down to stir until forming purple gel at 80 ℃;
Use ball mill with its ball milling after the oven dry down at 200 ℃ the purple gel that obtains, namely get the precursor pressed powder;
The precursor pressed powder that obtains is carried out the branch section calcining in high temperature process furnances, the material after the calcining is ground, namely get the rich lithium tertiary cathode material of power-type lithium ion battery.
3. the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery as claimed in claim 2, it is characterized in that described minute section calcining namely at first control temperature and be 400 ℃ and carry out precalcining 4h that the speed with 5 ℃/min is warming up to 900 ℃ of calcining 8h then.
4. the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery as claimed in claim 3 is characterized in that described ammoniacal liquor, and its mass percentage concentration is 28%.
5. the preparation method of the rich lithium tertiary cathode material of a kind of power-type lithium ion battery as claimed in claim 4 is characterized in that lithium acetate used in the preparation process is excessive 5%, the loss of lithium when remedying follow-up calcining.
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