CN103035898A - Nano flaky positive electrode material of lithium ion battery and preparation method for positive electrode material - Google Patents
Nano flaky positive electrode material of lithium ion battery and preparation method for positive electrode material Download PDFInfo
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Abstract
The invention discloses a nano flaky positive electrode material of a lithium ion battery. The general formula of the positive electrode material is LiNixCoyMn(1-x-y)O2, wherein x is more than or equal to 0 and less than or equal to 1; and y is more than or equal to 0 and less than or equal to 1. The positive electrode material has a flaky appearance and is less than 100 nanometers in thickness. The invention further discloses a preparation method for the positive electrode material. The preparation method comprises the following steps: (1), dissolving soluble nickel salt, cobalt salt and manganese salt to obtain a mixed solution A; (2), preparing an alkaline solution B from sodium hydroxide and deionized water; and (3), heating the solution A and the solution B to a certain temperature, adding the solution A and the solution B into a supergravity reactor, performing rapid precipitation reaction to obtain precursor pulp, washing and drying to obtain a hydroxide precursor, mixing lithium, sintering, cooling to room temperature, crushing and sieving to obtain the nano flaky positive electrode material of the lithium ion battery. The material prepared by the method has a flaky appearance and is only dozens of nanometers in thickness. Due to the nanoscale thickness, the rate capability of the material is greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, particularly a kind of nano-sheet anode material for lithium-ion batteries and preparation method thereof.
Background technology
The advantage such as lithium rechargeable battery has the energy density height, have extended cycle life and self discharge is little, now be widely used on all kinds of portable type electronic products and the mobile device, and the positive electrode of lithium ion battery is the important component part of such battery, and the performance of positive electrode is then restricting power and the energy density of lithium ion battery.
The preparation method of anode material for lithium-ion batteries has now developed the kinds of processes type, and existing preparation method then respectively has its pluses and minuses.The coprecipitation reaction method that existing preparation ternary cathode material of lithium ion battery adopts, reaction time is long, yields poorly.And to add a certain amount of ammoniacal liquor in the course of reaction, make the cost of sewage disposal and difficulty increase a lot.Simultaneously, present ternary cathode material of lithium ion battery all is the secondary ball of being reunited and being formed by the crystal grain about the 0.2-2 micron, and the D50 of spheroid is about the 5-15 micron.Such pattern has following shortcoming: 1), second particle causes too greatly electronic conductivity to descend, and affects the high rate performance of material.2), second particle is too closely knit and cause electrolyte to infiltrate not exclusively, affects the capacity performance.3), the presoma second particle is larger, so its sintering time that needs is long, sintering temperature is high, so power consumption is larger.
Summary of the invention
The object of the invention is to provide a kind of nano-sheet anode material for lithium-ion batteries LiNi for the shortcoming of above-mentioned prior art existence
xCo
yMn
(1-x-y)O
2, the technical problem of solution be improve the high rate performance of material, comprehensively releasable material charge/discharge capacity, improve cycle performance.
Another object of the present invention provides a kind of nano-sheet anode material for lithium-ion batteries LiNi
xCo
yMn
(1-x-y)O
2The preparation method.
The technical solution used in the present invention is as follows:
A kind of nano-sheet anode material for lithium-ion batteries, the general formula of this positive electrode are LiNi
xCo
yMn
(1-x-y)O
2, 0≤x≤1,0≤y≤1 wherein, this positive electrode pattern is sheet, and thickness is less than 100 nanometers.
A kind of preparation method of nano-grade anode material for lithium-ion batteries may further comprise the steps:
(1) being x:y:(1-x-y with mol ratio) soluble nickel salt, cobalt salt, the manganese salt of (0≤x≤1,0≤y≤1) obtains the mixed solution A of concentration 0.5～2M with deionized water dissolving;
(2) NaOH and deionized water are mixed with the mixed solution B of concentration 1～6M;
(3) above-mentioned two kinds of mixed solution A, B are heated to uniform temperature after, add in the supergravity reactor fast and react, obtaining structural formula is Ni
xCo
yMn
(1-x-y)(OH)
2The precursor pulp of (0≤x≤1,0≤y≤1), then washing, drying obtains the hydroxide presoma;
(4) above-mentioned hydroxide and lithium salts are mixed to evenly M=Ni described in the formula in Li:M=1.0 ~ 1.2 in molar ratio
xCo
yMn
(1-x-y)(0≤x≤1,0≤y≤1);
(5) sintering: the mixture that obtains is carried out high-temperature calcination, temperature range 700-1000 ℃, calcination time 2-12 hour, then be cooled to room temperature, pulverize, sieving obtains the nano-sheet anode material for lithium-ion batteries.
Soluble nickel salt of the present invention is selected from one or more in nickelous sulfate, nickel nitrate, the nickel chloride, described solubility cobalt salt is selected from one or more in cobaltous sulfate, cobalt nitrate, the cobalt chloride, described soluble manganese salt is selected from one or more in manganese sulfate, manganese nitrate, the manganese chloride, and described lithium salts is selected from one or more in lithium carbonate, lithium hydroxide, the lithium fluoride.
Wherein, consersion unit is supergravity reactor described in the step of the present invention (3), and described reaction control pH is at 10-12.
Wherein, mixed method is dry method batch mixing or material by wet type mixing in the step of the present invention (4).
Compared with prior art, a kind of nano-sheet anode material for lithium-ion batteries Ni of the present invention
xCo
yMn
(1-x-y)O
2The preparation method owing to adopt the hypergravity method, following advantage is arranged: nano-particles size is controlled, narrow diameter distribution, technique is simple, production efficiency is high, cost is low, engineering is amplified the advantages such as easy.Need not add ammoniacal liquor etc. in the course of reaction, follow-up cost of sewage disposal reduces.Simultaneously, prepare the nano-sheet positive electrode by gravity Method, following advantage arranged:
(1) the material pattern of preparing is laminar, and thickness only has tens nanometers, and nano level thickness has promoted the high rate performance of material greatly, and micron-sized diameter makes its processing characteristics (positive electrode is sized mixing) be better than common nano material.Electrolyte infiltrates good, so capacity is high than conventional products, and multiplying power and cycle performance are excellent.
(2) sintering temperature and sintering time all are lower than conventional material, have greatly reduced power consumption, save cost.
Brief Description Of Drawings:
Fig. 1 is the anode material for lithium-ion batteries electron scanning micrograph of the embodiment of the invention 1 preparation.
Fig. 2 is the circulating battery capacity curve figure of the embodiment of the invention 1.
Fig. 3 is the embodiment of the invention 1 battery multiplying power discharging curve.
Fig. 4 is Comparative Examples anode material for lithium-ion batteries electron scanning micrograph.
Fig. 5 is Comparative Examples circulating battery capacity curve.
Fig. 6 is Comparative Examples battery different multiplying discharge curve.
Embodiment:
Describe the specific embodiment of the present invention in detail below in conjunction with Figure of description and embodiment:
Fig. 1 shows the anode material for lithium-ion batteries electron scanning micrograph of the embodiment of the invention 1 preparation.
Fig. 2 shows the circulating battery capacity curve figure of the embodiment of the invention 1.
Fig. 3 shows the embodiment of the invention 1 battery multiplying power discharging curve.
Fig. 4 is Comparative Examples anode material for lithium-ion batteries electron scanning micrograph.
Fig. 5 is Comparative Examples circulating battery capacity curve.
Fig. 6 is Comparative Examples battery different multiplying discharge curve
Implement the present invention and adopt following preparation method:
(1) being x:y:(1-x-y with mol ratio) soluble nickel salt, cobalt salt, the manganese salt of (0≤x≤1,0≤y≤1) obtains the mixed solution A of concentration 0.5～2M with deionized water dissolving;
(2) NaOH and deionized water are mixed with the mixed solution B of concentration 1～6M;
(3) above-mentioned two kinds of mixed solution A, B are heated to uniform temperature after, add in the supergravity reactor fast and react, obtaining structural formula is Ni
xCo
yMn
(1-x-y)(OH)
2The precursor pulp of ﹒ (0≤x≤1,0≤y≤1), then washing, drying obtains the hydroxide presoma;
(4) above-mentioned hydroxide and lithium salts are mixed to evenly M=Ni described in the formula in Li:M=1.0 ~ 1.2 in molar ratio
xCo
yMn
(1-x-y)(0≤x≤1,0≤y≤1);
(5) sintering: the mixture that obtains is carried out high-temperature calcination, temperature range 700-1000 ℃, calcination time 2-12 hour, then be cooled to room temperature, pulverize, sieving obtains the nano-sheet anode material for lithium-ion batteries.
Annotate: soluble nickel salt can be used one or more in nickelous sulfate, nickel nitrate, the nickel chloride.
The solubility cobalt salt can use one or more in cobaltous sulfate, cobalt nitrate, the cobalt chloride.
Soluble manganese salt can use one or more in manganese sulfate, manganese nitrate, the manganese chloride.
Lithium salts can use one or more in lithium carbonate, lithium hydroxide, the lithium fluoride.
The concentration range 0.5-2mol/L of mixed solution A
The concentration range 1-6mol/L of mixed solution B
Be Ni:Co:Mn=5:2:3 weighing nickelous sulfate, cobaltous sulfate, manganese sulfate according to mol ratio, use deionized water dissolving, be prepared into the salting liquid of 1mol/L.Weighing NaOH and deionized water are configured to the aqueous slkali of 2mol/L.The salting liquid that configures and aqueous slkali are heated to 50 ℃ and constant temperature, add in the supergravity reactor fast and react, the control ph value of reaction filters the precursor pulp that obtains 11, with dry after the deionized water washing 5 times, obtains the hydroxide presoma.The above-mentioned hydroxide presoma of weighing and lithium carbonate be Li:M=1.05(M=Ni wherein in molar ratio
0.5Co
0.3Mn
0.2) in mixer, be mixed to evenly.Mixture is put into sintering kiln, and at 850 ℃ of lower sintering cool to room temperature after 8 hours, grinding is sieved, and obtains the nano-sheet anode material for lithium-ion batteries.
Resulting material pattern is laminar about diameter 3-5 μ m, about thickness 50nm.In button cell, discharge and recharge under the 0.2C multiplying power, first run capacity can reach 161.8mAh/g.50 take turns the circulation after capability retention be 98%.Be made into 18650 battery testing multiplying powers, the 10C discharge capacitance is 97.4%.
Embodiment 2:
Be Ni:Co:Mn=7:1.5:1.5 weighing nickelous sulfate, cobaltous sulfate, manganese sulfate according to mol ratio, use deionized water dissolving, be prepared into the salting liquid of 2mol/L.Weighing NaOH and deionized water are configured to the aqueous slkali of 4mol/L.The salting liquid that configures and aqueous slkali are heated to 50 ℃ and constant temperature, add in the supergravity reactor fast and react, the control ph value of reaction filters the precursor pulp that obtains 12, with dry after the deionized water washing 5 times, obtains the hydroxide presoma.The above-mentioned hydroxide presoma of weighing 1200g is with lithium hydroxide Li:M=1.14(M=Ni wherein in molar ratio
0.7Co
0.15Mn
0.15) in mixer, be mixed to evenly.Mixture is put into sintering kiln, and at 750 ℃ of lower sintering cool to room temperature after 6 hours, grinding is sieved, and obtains the nano-sheet anode material for lithium-ion batteries.
Resulting material pattern is laminar about diameter 2-5 μ m, about thickness 50nm.In button cell, discharge and recharge under the 0.2C multiplying power, first run capacity can reach 169.3mAh/g.50 take turns the circulation after capability retention be 97%.Be made into 18650 battery testing multiplying powers, the 10C discharge capacitance is 94.6%.
Embodiment 3:
Be Ni:Co:Mn=1:1:1 weighing nickel chloride, cobalt chloride, manganese chloride according to mol ratio, use deionized water dissolving, be prepared into the salting liquid of 0.5mol/L.Weighing sodium hydroxide and deionized water are configured to the aqueous slkali of 1mol/L.The salting liquid that configures and aqueous slkali are heated to 50 ℃ and constant temperature, add in the supergravity reactor fast and react, the control ph value of reaction filters the precursor pulp that obtains 10.5, with dry after the deionized water washing 5 times, obtains the hydroxide presoma.The above-mentioned hydroxide presoma of weighing 1300g is with lithium hydroxide Li:M=1.02(M=Ni wherein in molar ratio
1/3Co
1/3Mn
1/3) in mixer, be mixed to evenly.Mixture is put into sintering kiln, and at 900 ℃ of lower sintering cool to room temperature after 10 hours, grinding is sieved, and obtains the nano-sheet anode material for lithium-ion batteries.
Resulting material pattern is laminar about diameter 3-5 μ m, about thickness 60nm.In button cell, discharge and recharge under the 0.2C multiplying power, first run capacity can reach 148mAh/g.50 take turns the circulation after capability retention be 99.6%.Be made into 18650 battery testing multiplying powers, the 10C discharge capacitance is 95.3%.
Comparative Examples:
Be Ni:Co:Mn=5:2:3 weighing nickelous sulfate, cobaltous sulfate, manganese sulfate according to mol ratio, use deionized water dissolving, be prepared into the salting liquid of 1mol/L.Weighing NaOH and deionized water are configured to the aqueous slkali of 2mol/L, and add a certain amount of ammoniacal liquor and mix, and the volume ratio of ammoniacal liquor and sodium hydroxide solution is 1:10.The salting liquid that configures and aqueous slkali added in the conventional coprecipitation reaction device with certain flow rate with pump carry out precipitation reaction, reaction temperature is controlled to be 50 ℃, and ph value of reaction is controlled at 11, constantly stirs until reaction finishes.The precursor pulp that obtains is filtered, with dry after the deionized water washing 5 times, obtain the hydroxide presoma.The above-mentioned hydroxide presoma of weighing and lithium carbonate in molar ratio Li:M=1.05 are mixed in mixer evenly.Mixture is put into sintering kiln, and at 950 ℃ of lower sintering cool to room temperature after 20 hours, grinding is sieved, and obtains ball-shaped lithium-ion battery anode material.
Resulting material pattern is the micron order spherical particle.In button cell, discharge and recharge under the 0.2C multiplying power, first run capacity is 155mAh/g.50 take turns the circulation after capability retention be 90%.Be made into 18650 battery testing multiplying powers, the 10C discharge capacitance is 27.3%.
Claims (6)
1. nano-sheet anode material for lithium-ion batteries, it is characterized in that: the general formula of this positive electrode is
LiNi
xCo
yMn
(1-x-y)O
2, 0≤x≤1,0≤y≤1 wherein, this positive electrode pattern is sheet, and thickness is less than 100 nanometers.
2. the preparation method of a nano-grade anode material for lithium-ion batteries may further comprise the steps:
(1) being x:y:(1-x-y with mol ratio) soluble nickel salt, cobalt salt, the manganese salt of (wherein 0≤x≤1,0≤y≤1) obtains the mixed solution A of concentration 0.5～2M with deionized water dissolving;
(2) NaOH and deionized water are mixed with the mixed solution B of concentration 1～6M;
(3) above-mentioned two kinds of mixed solution A, B are heated to uniform temperature after, add in the supergravity reactor fast and react, obtaining structural formula is Ni
xCo
yMn
(1-x-y)(OH)
2The precursor pulp of (wherein 0≤x≤1,0≤y≤1), then washing, drying obtains the hydroxide presoma;
(4) above-mentioned hydroxide and lithium salts are mixed to evenly M=Ni described in the formula in Li:M=1.0 ~ 1.2 in molar ratio
xCo
yMn
(1-x-y)(wherein 0≤x≤1,0≤y≤1);
(5) sintering: the mixture that obtains is carried out high-temperature calcination, temperature range 700-1000 ℃, calcination time 2-12 hour, then be cooled to room temperature, pulverize, sieving obtains the nano-sheet anode material for lithium-ion batteries.
3. the preparation method of nano-grade anode material for lithium-ion batteries according to claim 2, it is characterized in that: described soluble nickel salt is selected from one or more in nickelous sulfate, nickel nitrate, the nickel chloride, described solubility cobalt salt is selected from one or more in cobaltous sulfate, cobalt nitrate, the cobalt chloride, described soluble manganese salt is selected from one or more in manganese sulfate, manganese nitrate, the manganese chloride, and described lithium salts is selected from one or more in lithium carbonate, lithium hydroxide, the lithium fluoride.
4. the preparation method of nano-grade anode material for lithium-ion batteries according to claim 2, it is characterized in that: consersion unit is supergravity reactor described in the step (3).
5. the preparation method of nano-grade anode material for lithium-ion batteries according to claim 2 is characterized in that: react control pH described in the step (3) at 10-12.
6. the preparation method of nano-grade anode material for lithium-ion batteries according to claim 2 is characterized in that: mixed method is dry method batch mixing or material by wet type mixing in the step (4).
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Cited By (9)
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| CN104362305A (en) * | 2014-08-18 | 2015-02-18 | 香港应用科技研究院有限公司 | Composite material and production method thereof |
| CN105244495A (en) * | 2015-10-08 | 2016-01-13 | 昆明理工大学 | Preparation method for composite hydroxide nanosheet |
| CN105731553A (en) * | 2016-02-03 | 2016-07-06 | 广东佳纳能源科技有限公司 | Drusy ternary anode material precursor and preparation method thereof |
| CN106745336A (en) * | 2016-12-28 | 2017-05-31 | 杉杉能源（宁夏）有限公司 | A kind of precursor of nickel-cobalt-lithium-manganese-oxide of nanometer sheet reunion second particle and preparation method thereof |
| CN107248572A (en) * | 2017-08-28 | 2017-10-13 | 北京理工大学 | A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery |
| CN108264098A (en) * | 2018-02-26 | 2018-07-10 | 重庆大学 | The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen |
| CN113036095A (en) * | 2020-03-27 | 2021-06-25 | 湖南杉杉能源科技股份有限公司 | Preparation method of single-crystal-morphology lithium ion battery positive electrode material |
| CN114530592A (en) * | 2022-04-24 | 2022-05-24 | 宜宾锂宝新材料有限公司 | Ternary cathode material and preparation method thereof |
| WO2023246724A1 (en) * | 2022-06-22 | 2023-12-28 | 浙江钠创新能源有限公司 | Anode material precursor, anode material, method for preparing same, and use thereof |
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| CN104362305A (en) * | 2014-08-18 | 2015-02-18 | 香港应用科技研究院有限公司 | Composite material and production method thereof |
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| CN105244495A (en) * | 2015-10-08 | 2016-01-13 | 昆明理工大学 | Preparation method for composite hydroxide nanosheet |
| CN105731553A (en) * | 2016-02-03 | 2016-07-06 | 广东佳纳能源科技有限公司 | Drusy ternary anode material precursor and preparation method thereof |
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| CN106745336B (en) * | 2016-12-28 | 2018-02-13 | 杉杉能源（宁夏）有限公司 | A kind of precursor of nickel-cobalt-lithium-manganese-oxide of nanometer sheet reunion second particle and preparation method thereof |
| CN107248572A (en) * | 2017-08-28 | 2017-10-13 | 北京理工大学 | A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery |
| CN108264098A (en) * | 2018-02-26 | 2018-07-10 | 重庆大学 | The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen |
| CN108264098B (en) * | 2018-02-26 | 2019-10-25 | 重庆大学 | The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen |
| CN113036095A (en) * | 2020-03-27 | 2021-06-25 | 湖南杉杉能源科技股份有限公司 | Preparation method of single-crystal-morphology lithium ion battery positive electrode material |
| CN114530592A (en) * | 2022-04-24 | 2022-05-24 | 宜宾锂宝新材料有限公司 | Ternary cathode material and preparation method thereof |
| CN114530592B (en) * | 2022-04-24 | 2022-07-19 | 宜宾锂宝新材料有限公司 | Ternary cathode material and preparation method thereof |
| WO2023246724A1 (en) * | 2022-06-22 | 2023-12-28 | 浙江钠创新能源有限公司 | Anode material precursor, anode material, method for preparing same, and use thereof |
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Application publication date: 20130410 |