CN108493435B - Lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2And preparation method - Google Patents
Lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2And preparation method Download PDFInfo
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Abstract
The invention belongs to the field of lithium ion batteries, and provides a lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1‑xYxO2And a process for the preparation thereof, wherein 0<x is less than or equal to 0.05 and is used for overcoming LiNi0.8Mn0.1Co0.1O2Poor electrochemical cycle performance and poor safety performance. The invention adopts bulk phase doping modification, reduces cation mixed discharge of the material by doping a very small amount of yttrium element, and enlarges Li+Diffusion channel, increasing Li in the material+The diffusion capability of the material stabilizes the internal structure of the material, and obviously improves the cycling stability of the material; and by utilizing the function of oxygen storage of metal yttrium ions, when the material is subjected to large-proportion delithiation under high voltage, Ni in the material4+The ions have extremely high oxidation activity, while the yttrium ions have O absorption2‑Function of (2) can be Ni4+The ion surface is passivated, so that the oxidability of the electrolyte is weakened, and the safety of charge and discharge under high voltage is improved; simultaneous surface generation of LiYO2The lithium fast ion conductor not only enhances the ionic conductivity, but also reduces the surface alkalinity of the material. Namely, the lithium ion battery anode material can meet the requirements of large-rate charge and discharge and high energy density, and greatly improves the safety under the high-voltage charge and discharge condition.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and relates to a lithium ion battery anode material and a preparation method thereof, in particular to a lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2And a process for the preparation thereof, wherein 0<x≤0.05。
Background
Under the promotion of new energy material research and development and related industries, the lithium ion battery anode material is rapidly developing towards the direction of higher energy density, volumetric specific energy, cycle life, safety and lower cost. Among the various types of positive electrode materials, the currently industrialized positive electrode materials mainly include the following: lithium cobaltate, lithium iron phosphate, lithium manganate and ternary materials; the ternary material can be divided into two categories of nickel-cobalt-manganese and nickel-cobalt-aluminum according to chemical components. The nickel-cobalt-manganese ternary cathode material with high nickel content is different from the traditional ternary cathode materials (111 type, 424 type and 523 type) with low nickel content, the nickel content of the ternary cathode material with high nickel content is higher than 0.6, and the ternary cathode material with high nickel content has the advantages of high energy density, low cost and the like, and becomes a hot spot for research and development and production in the cathode material of an industrial power lithium ion battery in recent years.
However, high nickel ternary positive electrode materials have a Ni content that increases with increasing nickel content2+And Li+The cation-mixing phenomenon is more serious, so that the cycling stability of the material is not ideal; in order to solve the problem of poor cycling stability in the high-nickel ternary cathode material, modification means such as doping and cladding are often adopted. Compared with coating, the doping process is simpler and is easier to realize industrialization, but the doping often replaces a small amount of elements with electrochemical activity, so that the specific discharge capacity of the material is reduced.
Disclosure of Invention
The invention aims to provide a layered high nickel cobalt lithium manganate (LiNi) as a lithium ion battery cathode material0.8Mn0.1Co0.1O2) Poor electrochemical cycle performance and poor safety performanceProvides a lithium ion battery anode material Li (Ni) doped and modified by a lithium excess binder phase0.8Co0.1Mn0.1)1-xYxO2And a process for the preparation thereof, wherein 0<x is less than or equal to 0.05. The lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2The preparation method has the advantages that the preparation method adopts the traditional solid phase method to carry out bulk phase doping, the operation flow and the process are simple, the industrial production is easy to realize, the product has high crystallization quality, fine particles, uniform distribution and low manufacturing cost.
In order to achieve the purpose, the invention adopts the technical scheme that:
lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2The lithium ion battery anode material is characterized in that the molecular expression of the lithium ion battery anode material is Li (Ni)0.8Co0.1Mn0.1)1-xYxO2Wherein, 0<x≤0.05。
The lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2The preparation method is characterized by comprising the following steps:
step 1, dissolving a lithium source raw material in deionized water, adding an yttrium source material, uniformly mixing, and grinding to obtain a mixed slurry, wherein the molar ratio of Li: y ═ 1.1 to 1.2: x, 0< x is less than or equal to 0.05;
step 2, adding Ni into the mixed slurry obtained in the step 10.8Co0.1Mn0.1(OH)2And (2) continuously grinding the precursor and absolute ethyl alcohol until the mixed slurry is in a uniform flow state, and continuously grinding under an infrared lamp until the mixed slurry is completely mixed into powder, wherein the molar ratio of Li: ni0.8Co0.1Mn0.1(OH)2：Y＝(1.1～1.2)：1-x：x；
Step 3, the product obtained in the step 2The uniformly ground mixed powder is placed in a tube furnace, the temperature is increased to 470-550 ℃ at the speed of 2-5 ℃/min under the oxygen atmosphere for pre-sintering for 6-10 h, the temperature is increased to 750-850 ℃ at the speed of 2-3 ℃/min for roasting for 15-20 h, the temperature is reduced to 450-500 ℃ at the speed of 2 ℃/min, and finally the temperature is cooled to room temperature along with the furnace, so that Li (Ni) is prepared0.8Co0.1Mn0.1)1-xYxO2。
In the step 1 and the step 2, the molar ratio of the lithium source raw material, the yttrium source raw material and the precursor is (1.10-1.20): x (1-x).
In step 1, the lithium source raw material is at least one of lithium carbonate, lithium nitrate, lithium acetate, lithium chloride and lithium hydroxide.
In step 1, the yttrium source raw material is at least one of yttrium nitrate, yttrium hydroxide, yttrium sulfate, yttrium chloride and yttrium oxide.
In terms of working principle: the invention relates to a high nickel ternary positive electrode material LiNi0.8Mn0.1Co0.1O2The material is doped with a small amount of yttrium metal element, and trivalent yttrium metal element can enlarge the unit cell volume of the material by virtue of larger ionic radius (0.090nm), thereby enlarging Li+Escape and insertion path, reduction of Li+Resistance to deintercalation while also reducing Li+The damage to the crystal structure in the de-intercalation process stabilizes the skeleton structure of the material, improves the electrochemical performance of the material and also improves the stability of the crystal structure of the material; meanwhile, the metal element yttrium ions are doped into the material crystal lattice, so that the material particles can be refined and more uniform, and the conductivity of the material is increased; in addition, the addition of the excessive lithium source can compensate the lithium loss of the material at high temperature, so that the material has more lithium ions, thereby having higher specific discharge capacity and further improving the energy density of the material. More importantly, because the metal yttrium ions have the functions of oxygen overflow and oxygen storage, when the material is subjected to large-proportion delithiation under the high voltage of 4.5V, Ni in the material4+Increased ion ratio and large amount of Ni4+The ions have extremely high oxidation activity, while the yttrium ions have O absorption2-Function of (2) can be Ni4+Passivation of ion surface(reduction to stable Ni)3+) Thus, the oxidation of the electrolyte is weakened, thereby improving the safety of charge and discharge at high voltage. It has also been found that, due to the addition of Y, LiYO is formed on the surface of the material to a thickness of about 5 to 20nm2The lithium fast ion conductor not only enhances the ionic conductivity, but also reduces the surface alkalinity of the material, reduces the pH value and obviously improves the price performance.
In summary, the invention has the following advantages:
1. the invention reduces the cation mixed discharge of the material by doping a very small amount of yttrium element, and enlarges Li+Diffusion channel, increasing Li in the material+The internal structure of the material is stabilized, and the rate capability and the cycling stability of the material are obviously improved.
2. The layered lithium ion battery anode material Li (Ni) prepared by the invention0.8Co0.1Mn0.1)1-xYxO2By means of the large lithium excess amount of 10% -20%, the lithium loss of the material at high temperature is made up, and the specific discharge capacity of the material is increased.
3. The invention utilizes the function of oxygen storage of metal yttrium ions (which is commonly used by high-temperature fuel cells), and when the material is subjected to large-proportion delithiation under high voltage, Ni in the material4+The ions have extremely high oxidation activity, while the yttrium ions have O absorption2-Function of (2) can be Ni4+The ion surface is passivated, so that the oxidability of the electrolyte is weakened, and the safety of charge and discharge under high voltage is improved.
4. The layered lithium ion battery anode material Li (Ni) prepared by the invention0.8Co0.1Mn0.1)1-xYxO2The material has high specific discharge capacity and very excellent cycle performance; under the room temperature environment, when the voltage range is 2.8-4.3V and the constant current charge-discharge multiplying power is 0.5C, the first discharge specific capacity of the lithium ion battery anode material can reach 180.4mAh g-1183.9mAh g after 100 times of circulation-1The capacity retention rate is as high as 101.9%; when the voltage range is 2.8-4.5V and the constant current charge-discharge multiplying power is 0.5CThe initial specific discharge capacity of the lithium ion battery anode material can reach 192.0mAh g-1189.4mAh g after 100 times of circulation-1The capacity retention rate was 98.6%.
5. In the invention, due to the addition of Y, LiYO with the thickness of about 5-20nm is generated on the surface of the material2The lithium fast ion conductor not only enhances the ionic conductivity, but also reduces the surface alkalinity of the material, reduces the pH value and obviously improves the processing performance.
6. The method has the advantages of simple process flow, environmental protection, simpler equipment used in the process, wide raw material source and easy realization of large-scale industrial production.
Drawings
FIG. 1 shows the preparation of Li (Ni) as the positive electrode material of lithium ion battery0.8Co0.1Mn0.1)1-xYxO2The process flow diagram of (1).
FIG. 2 shows the preparation of Li (Ni) as the positive electrode material of the lithium ion battery in example 1 of the present invention0.8Co0.1Mn0.1)1-xYxO2XRD pattern of (a).
FIG. 3 shows the preparation of Li (Ni) as the positive electrode material of the lithium ion battery in example 1 of the present invention0.8Co0.1Mn0.1)1-xYxO2SEM image of (d).
FIG. 4 shows the preparation of Li (Ni) as the positive electrode material of the lithium ion battery in example 1 of the present invention0.8Co0.1Mn0.1)1-xYxO2And in a voltage range of 2.8-4.3V, charging and discharging at 0.5C multiplying power, and carrying out an initial charging and discharging curve chart.
FIG. 5 shows the preparation of Li (Ni) as the positive electrode material of the lithium ion battery in example 1 of the present invention0.8Co0.1Mn0.1)1-xYxO2In the voltage range of 2.8-4.3V, the charge and discharge are carried out at 0.5C multiplying power, and the cycle performance curve chart is shown.
FIG. 6 shows the preparation of Li (Ni) as the positive electrode material of the lithium ion battery in example 1 of the present invention0.8Co0.1Mn0.1)1-xYxO2Charging at 0.5C rate within 2.8-4.5VDischarge, initial charge and discharge curve.
FIG. 7 shows that the positive electrode material Li (Ni) of the lithium ion battery prepared in example 1 of the present invention0.8Co0.1Mn0.1)1-xYxO2In the voltage range of 2.8-4.5V, the charge and discharge are carried out at 0.5C multiplying power, and the cycle performance curve chart is shown.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and the accompanying drawings.
Example 1
When the excess amount of lithium and the amount of doped yttrium were 10% and 0.02% (i.e., x was 0.02), 1.1656g of LiOH · H was weighed out2O, dissolved in 10ml of deionized water, 0.0565g Y was added2O3Uniformly grinding, adding 2.2852g of precursor and absolute ethyl alcohol, grinding until a fluid state mixed slurry is obtained, and then continuously grinding under an infrared lamp until the mixed slurry is completely mixed into mixed powder; drying in a baking oven, grinding into fine powder, pre-sintering at 3 deg.C/min for 6 hr in a tubular furnace under oxygen atmosphere (oxygen flow rate of 400ml/min) to 470 deg.C, baking at 2 deg.C/min to 780 deg.C for 15 hr, cooling to 450-500 deg.C at 2 deg.C/min, cooling to room temperature, and grinding to obtain Li (Ni)0.8Co0.1Mn0.1)0.98Y0.02O2。
For the prepared lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)0.98Y0.02O2The constant current charge and discharge test is carried out, the test results are shown in fig. 2-7, and the test results show that the anode material has high specific discharge capacity and excellent cycling stability; under the room temperature environment, when the voltage range is 2.8-4.3V and the constant current charge-discharge multiplying power is 0.5C, the first discharge specific capacity of the lithium ion battery anode material can reach 180.4mAh g-1183.9mAh g after 100 times of circulation-1The capacity retention rate is as high as 101.9%; when the voltage range is 2.8-4.5V and the constant current charge-discharge multiplying power is 0.5C, the initial discharge of the lithium ion battery anode materialThe specific capacity can reach 192.0mAh g-1After 100 times of circulation, the amount of the solution can still reach 189.4mAh g-1The capacity retention rate was 98.6%.
Respectively counter-doping Li (Ni)0.8Co0.1Mn0.1)O2And doped Li (Ni)0.8Co0.1Mn0.1)0.98Y0.02O2The material is subjected to a surface residual alkali test, the content of LiOH before doping is 0.27%, the pH value is 13.35, the content of LiOH after doping is only 0.13%, and the pH value is 12.53.
Example 2
When the excess amount of lithium and the amount of doped yttrium were 5% and 0.02% (i.e., x was 0.02), 1.1126g of LiOH · H was weighed out2O, dissolved in 10ml of deionized water, 0.0565g Y was added2O3Uniformly grinding, adding 2.2852g of precursor and absolute ethyl alcohol, grinding until a fluid state mixed slurry is obtained, and then continuously grinding under an infrared lamp until the mixed slurry is completely mixed into mixed powder; drying in a drying oven, grinding, heating to 470 deg.C in oxygen atmosphere (oxygen flow rate of 400ml/min) for 6 hr, heating to 780 deg.C at 2 deg.C/min for 15 hr, cooling to 450-500 deg.C at 2 deg.C/min, and grinding to obtain Li (Ni)0.8Co0.1Mn0.1)0.98Y0.02O2。
For the prepared lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)0.98Y0.02O2Constant current charge and discharge tests are carried out, and the test result shows that the anode material still has high specific discharge capacity and excellent cycling stability; under the room temperature environment, when the voltage range is 2.8-4.3V and the constant current charge-discharge multiplying power is 0.5C, the first discharge specific capacity of the lithium ion battery anode material can reach 181.8mAh g-1183.4mAh g can be achieved after 100 times of circulation-1The capacity retention rate is as high as 100.9%; when the voltage range is 2.8-4.5V and the constant current charge-discharge multiplying power is 0.5C, the initial discharge specific capacity of the lithium ion battery anode material can reachTo 192.5mAh g-1After 100 times of circulation, the amount of the active carbon can still reach 189.9mAh g-1The capacity retention rate was 98.6%.
Respectively counter-doping Li (Ni)0.8Co0.1Mn0.1)O2And doped Li (Ni)0.8Co0.1Mn0.1)0.98Y0.02O2The material is subjected to a surface residual alkali test, the content of LiOH before doping is 0.16%, the pH value is 13.08, the content of LiOH after doping is only 0.06%, and the pH value is 11.73.
Example 3
When the excess amount of lithium and the amount of doped yttrium were 10% and 0.01% (i.e., x was 0.01), 1.1656g of LiOH · H was weighed out2O, dissolved in 10ml of deionized water, 0.0283g Y was added2O3Uniformly grinding, adding 2.2509g of precursor and absolute ethyl alcohol, grinding until a fluid state mixed slurry is obtained, and then continuously grinding under an infrared lamp until the mixed slurry is completely mixed into mixed powder; drying in a drying oven, grinding, heating to 470 deg.C in oxygen atmosphere (oxygen flow rate of 400ml/min) for 6 hr, heating to 780 deg.C at 2 deg.C/min for 15 hr, cooling to 450-500 deg.C at 2 deg.C/min, and grinding to obtain Li (Ni)0.8Co0.1Mn0.1)0.99Y0.01O2。
For the prepared lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)0.99Y0.01O2Constant current charge and discharge tests are carried out, and the test result shows that the anode material still has high specific discharge capacity and excellent cycling stability; under the room temperature environment, when the voltage range is 2.8-4.3V and the constant current charge-discharge multiplying power is 0.5C, the first discharge specific capacity of the lithium ion battery anode material can reach 184.5mAh g-1184.9mAh g can be achieved after 100 times of circulation-1The capacity retention rate is as high as 100.2%; when the voltage range is 2.8-4.5V and the constant current charge-discharge multiplying power is 0.5C, the initial discharge specific capacity of the lithium ion battery anode material can reach 195.6mAh g-1After 100 times of circulation, the amount of the solution can still reach as high as 195.4mAh g-1The capacity retention rate was 99.9%.
Respectively counter-doping Li (Ni)0.8Co0.1Mn0.1)O2And doped Li (Ni)0.8Co0.1Mn0.1)0.99Y0.01O2The material is subjected to a surface residual alkali test, the content of LiOH before doping is 0.27%, the pH value is 13.35, the content of LiOH after doping is only 0.15%, and the pH value is 12.62.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (4)
1. Lithium ion battery anode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2The lithium ion battery anode material is characterized in that the molecular expression of the lithium ion battery anode material is as follows: li (Ni)0.8Co0.1Mn0.1)1-xYxO2Wherein, 0<x is less than or equal to 0.05; the surface of the lithium ion battery anode material is provided with LiYO with the thickness of 5-20nm2A lithium fast ion conductor;
the lithium ion battery cathode material Li (Ni)0.8Co0.1Mn0.1)1-xYxO2The preparation method comprises the following steps:
step 1, dissolving a lithium source raw material in deionized water, adding an yttrium source raw material, uniformly mixing, and grinding to obtain mixed slurry;
step 2, adding Ni into the mixed slurry obtained in the step 10.8Co0.1Mn0.1(OH)2Continuously grinding the precursor and absolute ethyl alcohol until the mixed slurry is in a uniform flow state, and continuously grinding under an infrared lamp until the mixed slurry is completely mixed into mixed powder;
step 3, the product obtained in the step 2The uniformly ground mixed powder is placed in a tube furnace, the temperature is increased to 470-550 ℃ at the speed of 2-5 ℃/min under the oxygen atmosphere for pre-sintering for 6-10 h, the temperature is increased to 750-850 ℃ at the speed of 2-3 ℃/min for roasting for 15-20 h, the temperature is reduced to 450-500 ℃ at the speed of 2 ℃/min, and finally the temperature is cooled to room temperature along with the furnace, so that Li (Ni) is prepared0.8Co0.1Mn0.1)1-xYxO2。
2. The positive electrode material Li (Ni) for lithium ion battery according to claim 10.8Co0.1Mn0.1)1-xYxO2In the step 1 and the step 2, the molar ratio of the lithium source raw material, the yttrium source raw material and the precursor is (1.10-1.20): x (1-x).
3. The positive electrode material Li (Ni) for lithium ion battery according to claim 10.8Co0.1Mn0.1)1-xYxO2And in the step 1, the lithium source raw material is at least one of lithium carbonate, lithium nitrate, lithium acetate, lithium chloride and lithium hydroxide.
4. The positive electrode material Li (Ni) for lithium ion battery according to claim 10.8Co0.1Mn0.1)1-xYxO2In step 1, the yttrium source raw material is at least one of yttrium nitrate, yttrium hydroxide, yttrium sulfate, yttrium chloride and yttrium oxide.
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| CN112599756B (en) * | 2021-01-13 | 2022-03-22 | 湖南长远锂科股份有限公司 | Fast ion conductor doped coating modified ternary positive electrode material and preparation method thereof |
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