CN113410464B - Multi-element rare earth doped high-nickel oxide lithium battery positive electrode material and preparation method thereof - Google Patents
Multi-element rare earth doped high-nickel oxide lithium battery positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multi-element rare earth doped high nickel oxide lithium battery positive electrode material and a preparation method thereof. In the preparation process of the yttrium and mixed rare earth doped high-nickel oxide positive electrode material, the surface yttrium element and bulk phase mixed rare earth element doped oxide positive electrode material is obtained by adopting a liquid nitrogen quenching and rapid cooling mode after high-temperature sintering, and the obtained electrode material has the advantages of good sphericity, high tap density, high discharge capacity and excellent capacity retention rate.
Description
Technical Field
The invention relates to the technical field of high specific energy positive electrode materials, in particular to a multi-element rare earth doped high-nickel oxide lithium battery positive electrode material and a preparation method thereof.
Background
With the rapid development of the global electric vehicle market, the energy storage device with high energy density becomes a main influencing factor limiting the commercialization of the electric vehicle. Lithium ion batteries have received much attention from the market due to their high energy density and operating voltage. Among them, the high nickel oxide positive electrode material is considered as the next generation lithium ion power battery positive electrode material with great application prospect. The high nickel oxide anode material has the advantages of high specific capacity, good rate capability and low cost. However, as the nickel content in the system increases, the cycle life and safety performance of the material deteriorate dramatically, thereby limiting its commercial application.
The high nickel oxide anode material applied in the current market is mainly nickel-cobalt-manganese ternary oxide (Li (Ni) x Co y Mn z )O 2 NCM) and nickel cobalt aluminum (Li (Ni) x Co y Al z )O 2 NCA). These oxides have relatively high discharge capacities, high tap densities and low costs. However, the content of nickel oxide is generally about 0.8 or less than 0.8, and the specific capacity of the nickel oxide is still not competitive in future high-specific-energy lithium ion batteries. Further increasing the nickel content can increase the specific capacity of the electrode, and also becomes a development trend of high specific energy positive electrode materials. However, it is pointed out that higher nickel contents inevitably lead to cyclic cracking of the electrode and poor thermal stability. From the prior technical method for improving the oxide anode, element doping is an effective method for improving the electrode cycle performance and the thermal stability, and particularly, different structural characteristics and chemical properties of multi-element metals are utilized to realize synergistic action, so that the aim of synergistic doping modification is fulfilled.
Chinese patents CN108807972A, CN111018004A and CN109713241A adopt rare earth single elements to dope and modify the anode material, and can improve the cycling stability of the electrode. CN111320214A, CN110911687A and CN111009656A adopt a parallel mode of rare earth single element doping and rare earth compound (oxide, nitride or nitrate) coating, reduce the internal resistance of electrode materials and improve the internal chemical stability of the battery. The method adopts doping modification based on rare earth single elements to improve the stability of the anode. The stability of the electrode is improved by introducing multiple rare earth elements, particularly mixed rare earth elements into the high-nickel oxide positive electrode material, which is not reported yet. Meanwhile, the mixed rare earth elements have good affinity effect on oxygen and moderate ionic radius, and the effect of improving the structure of the high-nickel oxide can be achieved by doping a small amount. Therefore, by utilizing the synergistic effect among the multiple rare earth elements, the oxygen precipitation of the electrode under high voltage can be inhibited, and the cycle stability and the thermal stability of the high nickel oxide electrode can be ensured.
Disclosure of Invention
The invention aims to solve the technical problem of providing a multi-element rare earth doped high nickel oxide cathode material and a preparation method thereof, which are used for doping yttrium element on the surface of high nickel oxide and bulk mixed rare earth element (Misch metal, mm), and improving the stability of the whole oxygen frame of the high nickel oxide material by utilizing the oxygen fixation characteristic of the yttrium element and the mixed rare earth element, thereby prolonging the cycle life of the material.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the multielement rare earth doped high-nickel oxide lithium battery positive electrode material is characterized in that the multielement rare earth comprises yttrium element and mixed rare earth element, the doping amount of the yttrium element is 1% -10% of the molar content of the total metal elements except lithium element, the mixed rare earth element comprises La, ce, pr and Nd, wherein the molar ratio of La is 41% -56%, the molar ratio of Ce is 1% -5%, the molar ratio of Pr is 6% -13%, the molar ratio of Nd is 37% -41%, and the doping amount of the mixed rare earth element is 1% -10% of the molar content of the total metal elements.
The preparation method of the multi-element rare earth doped high-nickel oxide lithium battery positive electrode material comprises the following steps:
step 1, pumping a metal salt solution, an yttrium salt solution and an alkali solution into a coprecipitation reaction kettle in a parallel flow mode to carry out coprecipitation reaction;
and 3, uniformly mixing the hydroxide precursor obtained in the step 2 with a lithium source, roasting in a tubular furnace in an oxygen atmosphere, and carrying out liquid nitrogen quenching treatment and rapid cooling to obtain the multi-element rare earth doped high-nickel oxide lithium battery positive electrode material.
The metal salt comprises one or more of nickel salt, magnesium salt, calcium salt, mixed rare earth salt and zirconium salt, and the nickel salt, the magnesium salt, the calcium salt, the mixed rare earth salt, the zirconium salt and the yttrium salt are one or more of sulfate, chloride, acetate, nitrate and oxalate.
The alkaline solution is a mixed aqueous solution containing a precipitator and a complexing agent, the precipitator comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate and potassium carbonate, and the complexing agent comprises one or more of ammonia water, oxalic acid, citric acid and disodium ethylene diamine tetraacetate.
The lithium source is one or more of lithium hydroxide, lithium carbonate, lithium oxide, lithium acetate and lithium oxalate, and the molar ratio of the doped molar amount to the precursor is 0.9-1.05.
In the step 1, the pH value of the system in the reaction kettle is stabilized at 10.6-11.5, the temperature is controlled at 40-60 ℃, and the stirring speed is controlled at 500-800 rpm/min.
The roasting temperature in the roasting process of the step 3 is 600-900 ℃, the time is 8-16 h, and the heating rate is 2-10 ℃ for min -1 And placing the mixture in liquid nitrogen for standing and quenching for 30-60 min.
The yttrium salt solution is a mixed solution which is prepared by mixing yttrium salt and citric acid according to the mass ratio of 1 (1-4) and then adding ammonia water to adjust the pH value to 7.0-10.0.
The concentration of the metal salt solution is 0.5-3 mol L -1 The concentration of yttrium salt solution is 0.5-3 mol L -1 The concentration of the precipitating agent is 1-8 mol L -1 The mixing amount of the complexing agent is 1-5 mol L -1 。
The beneficial effects of the invention are:
(1) By doping the multi-element rare earth (yttrium and mixed rare earth) to the high-nickel oxide cathode material, wherein the yttrium element is used for doping the surface of the high-nickel oxide, the side reaction between the active material and the electrolyte is inhibited, and the collapse of the surface structure is inhibited; the mixed rare earth elements carry out bulk phase doping on the high-nickel oxide, and the degradation of the body structure of the material in the circulating process is inhibited. Therefore, the yttrium and the mixed rare earth element cooperate to jointly improve the structural stability of the material from the two aspects of the surface and the body of the material, thereby effectively improving the cycle stability of the high-nickel oxide cathode material.
(2) In the preparation method, in order to avoid diffusion of doped ions in the slow annealing process, the doping positions of yttrium and the mixed rare earth elements are fixed in a liquid nitrogen quenching and rapid cooling mode, so that the surface doping of the yttrium element and the bulk doping of the mixed rare earth elements are ensured. Meanwhile, the obtained anode material has high particle sphericity and high tap density, and can effectively improve the volume energy density of the electrode material.
Drawings
FIG. 1 is a scanning electron micrograph of a positive electrode material according to example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a positive electrode material according to example 2 of the present invention.
FIG. 3 is a SEM image of the cathode material in example 3 of the present invention.
Fig. 4 is an X-ray diffraction pattern of the positive electrode material of example 1 of the invention.
FIG. 5 shows the cathode material of example 1 of the present invention at 20mA g -1 First circle charge-discharge curve under current density.
FIG. 6 shows that the positive electrode material of example 1 of the present invention is 200mA g -1 Cycling performance curve at current density.
Detailed Description
For a better understanding of the present disclosure, reference will now be made in detail to the present disclosure with reference to the following examples and accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The preparation method of the Mg, Y, mixed rare earth and Zr element doped high nickel oxide lithium battery positive electrode material comprises the following specific steps:
step 1: preparing a metal salt solution with the concentration of 1mol L -1 Wherein the metal salt is a mixture of nickel chloride, magnesium chloride, mixed rare earth chloride and zirconium chloride. 1mol of L is prepared -1 The yttrium salt solution of (1), wherein yttrium chloride and citric acid are prepared according to the mass ratio of 1. Moles of five raw materials of Ni, mg, Y, misch metal and Zr elementsRatio 0.95. Preparing mixed alkali solution of sodium hydroxide and ammonia water, wherein the concentration of the sodium hydroxide is 5mol L -1 And the concentration of ammonia water is 3mol L -1 。
Step 2: adding 2.5L of deionized water into the reaction kettle, and adjusting the stirring speed to 600rpm min -1 The temperature was 50 ℃. Pumping the metal salt solution and the yttrium salt solution prepared in the step 1 into a reaction kettle by using a peristaltic pump, and automatically controlling the pumping of the alkali solution during the pumping so as to stabilize the pH value of the system at 11.0. And (5) carrying out coprecipitation reaction for 40h after the system reacts to obtain hydroxide precursor solution.
And 3, step 3: and (3) taking out the precursor solution obtained in the step (2) from the reaction kettle, washing and filtering by using ethanol, and drying for 12 hours by using a forced air drying oven at 100 ℃ to obtain hydroxide precursor powder.
And 4, step 4: fully mixing the hydroxide precursor powder obtained in the step 3 and lithium hydroxide monohydrate in an agate mortar, weighing according to the principle that the molar weight of a lithium element is more than 2% of that of a metal element, roasting in a tubular furnace in an oxygen atmosphere, and roasting at the temperature of 3 ℃ for min -1 The temperature rise rate is increased to 700 ℃, the temperature is kept for 10 hours, and liquid nitrogen quenching is carried out for 30min, so as to obtain the finished product of the high nickel oxide cathode material.
As shown in fig. 1, which is a scanning electron microscope image of the cathode material prepared in example 1, it can be seen that the sample has a uniform spherical morphology, and the spherical particles are formed by aggregation of many primary nanocrystals. It can also be seen that the diameter of the spherical particles is between 15 and 30 microns.
As shown in fig. 4, which is an X-ray diffraction pattern of the cathode material obtained in example 1, the diffraction peak of the sample was found to coincide with the standard diffraction peak of lithium nickelate, and to exhibit a hexagonal structure characteristic.
As shown in FIG. 5, the cathode material prepared in example 1 was charged at 20mA g -1 The first circle charging and discharging curve under the current density shows that the first cycle discharging specific capacity can reach 227.2mAh g -1 The nickel oxide anode has the advantage of high specific capacity, and the charge-discharge curve of the nickel oxide anode has the remarkable characteristics of a multi-platform nickel oxide anode.
As shown in FIG. 6, the cathode material prepared in example 1 was charged at 200mA g -1 Electric currentCycle performance curve at density, 200mA g -1 The amplification capacity of more than 200mAh g can be released under the current density -1 . Meanwhile, the capacity retention rate of the cathode material after 100 weeks of circulation is 92.3%, and the cathode material has excellent circulation performance.
Example 2
The preparation method of the Ca, Y, mixed rare earth and Zr element doped high nickel oxide lithium battery positive electrode material comprises the following specific steps:
step 1: preparing a metal salt solution with the concentration of 1mol L -1 Wherein the metal salt is a mixture of nickel chloride, calcium chloride, mixed rare earth chloride and zirconium chloride. 1mol of L is prepared -1 The yttrium salt solution of (1), wherein yttrium chloride and citric acid are prepared according to the mass ratio of 1. The molar ratio of the five raw materials of Ni, ca, Y, misch metal and Zr element is 0.95. Preparing a mixed alkali solution of sodium hydroxide and ammonia water, wherein the concentration of the sodium hydroxide is 5mol L -1 And the concentration of ammonia water is 3mol L -1 。
Step 2: adding 2.5L of deionized water into the reaction kettle, and adjusting the stirring speed to 600rpm for min -1 The temperature was 50 ℃. Pumping the metal salt solution and the yttrium salt solution prepared in the step 1 into a reaction kettle by using a peristaltic pump, and automatically controlling the pumping of the alkali solution during the pumping so as to stabilize the pH value of the system at 11.2. And (5) carrying out coprecipitation reaction for 40h after the system reacts to obtain hydroxide precursor solution.
And step 3: and (3) taking out the precursor solution obtained in the step (2) from the reaction kettle, washing and filtering by using ethanol, and drying for 12 hours by using a forced air drying oven at 100 ℃ to obtain hydroxide precursor powder.
And 4, step 4: fully mixing the hydroxide precursor powder obtained in the step 3 and lithium hydroxide monohydrate in an agate mortar, weighing according to the principle that the molar weight of a lithium element is more than 2% of that of a metal element, roasting in a tubular furnace in an oxygen atmosphere, and roasting at the temperature of 3 ℃ for min -1 The temperature rise rate is increased to 700 ℃, the temperature is kept for 10 hours, and liquid nitrogen quenching is carried out for 50min, so as to obtain the finished product of the high nickel oxide cathode material.
As shown in fig. 2, which is a scanning electron micrograph of the positive electrode material prepared in example 2, it can be seen that the sample has a spherical morphology, and the spherical particles are formed by aggregation of a plurality of primary nanocrystals. It can also be seen that the diameter of the spherical particles is between 10 and 30 microns.
Example 3
The preparation method of the Mg, mixed rare earth and Zr element doped high nickel oxide lithium battery anode material comprises the following specific steps:
step 1: preparing a metal salt solution with the concentration of 1mol L -1 Wherein the metal salt is a mixture of nickel chloride, magnesium chloride, mixed rare earth chloride and zirconium chloride, and the molar ratio of the four raw materials is 0.96. Preparing mixed alkali solution of sodium hydroxide and ammonia water, wherein the concentration of the sodium hydroxide is 5mol L -1 And the concentration of ammonia water is 3mol L -1 。
Step 2: adding 2.5L of deionized water into the reaction kettle, and adjusting the stirring speed to 600rpm for min -1 The temperature was 50 ℃. Pumping the metal salt solution prepared in the step 1 into a reaction kettle by using a peristaltic pump, and automatically controlling the pumping of the alkali solution during the pumping so as to stabilize the pH value of the system at 11.0. And (5) carrying out coprecipitation reaction for 40h after the system reacts to obtain hydroxide precursor solution.
And step 3: and (3) taking out the precursor solution obtained in the step (2) from the reaction kettle, washing and filtering by using ethanol, and drying for 12 hours by using a forced air drying oven at 100 ℃ to obtain hydroxide precursor powder.
And 4, step 4: fully mixing the hydroxide precursor powder obtained in the step 3 and lithium hydroxide monohydrate in an agate mortar, weighing according to the principle that the molar weight of a lithium element is more than 2% of that of a metal element, roasting in a tubular furnace in an oxygen atmosphere, and roasting at the temperature of 3 ℃ for min -1 The temperature rise rate is increased to 700 ℃, the temperature is kept for 10 hours, and liquid nitrogen quenching is carried out for 30min, thus obtaining the finished product of the high nickel oxide cathode material.
As shown in fig. 3, which is a scanning electron micrograph of the positive electrode material prepared in example 3, it can be seen that the sample has a spherical morphology with different sizes, and the spherical particles are also formed by aggregation of a plurality of primary nanocrystals. Wherein the diameter of the large spherical particles is between 20 and 30 microns, and the diameter of the small spherical particles is between 5 and 10 microns.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited thereto, and any modification, equivalent replacement, or improvement made by those skilled in the art without departing from the principle of the present invention shall be included in the scope of the present invention.
Claims (6)
1. The preparation method of the multi-element rare earth doped high nickel oxide lithium battery positive electrode material is characterized by comprising the following steps of:
step 1, pumping a metal salt solution, an yttrium salt solution and an alkali solution into a coprecipitation reaction kettle in a parallel flow mode to carry out coprecipitation reaction;
step 2, washing and filtering precipitates obtained after the reaction is finished by using ethanol, and drying the precipitates by using an oven to obtain a hydroxide precursor;
step 3, uniformly mixing the hydroxide precursor obtained in the step 2 with a lithium source, roasting in a tubular furnace under an oxygen atmosphere, and carrying out liquid nitrogen quenching treatment and rapid cooling to obtain a multi-element rare earth doped high-nickel oxide lithium battery positive electrode material; the roasting temperature in the roasting process is 600-900 ℃, the time is 8-16 h, the heating rate is 2-10 ℃/min, and the mixture is placed in liquid nitrogen for standing and quenching for 30-60 min;
the multi-element rare earth comprises yttrium element and mixed rare earth element, the doping amount of the yttrium element is 1% -10% of the molar content of the total metal elements except lithium element, the mixed rare earth element comprises La, ce, pr and Nd, wherein the molar ratio of La is 41% -56%, the molar ratio of Ce is 1% -5%, the molar ratio of Pr is 6% -13%, the molar ratio of Nd is 37% -41%, and the doping amount of the mixed rare earth element is 1% -10% of the molar content of the total metal elements; yttrium element is used for carrying out surface doping on the high-nickel oxide, and mixed rare earth element is used for carrying out bulk phase doping on the high-nickel oxide;
the metal salt comprises one or more of nickel salt, mixed rare earth salt, magnesium salt, calcium salt and zirconium salt, wherein the nickel salt, the magnesium salt, the calcium salt, the mixed rare earth salt, the zirconium salt and the yttrium salt are one or more of sulfate, chloride, acetate, nitrate and oxalate;
the yttrium salt solution is a mixed solution which is prepared by mixing yttrium salt and citric acid according to the mass ratio of 1 (1-4) and then adding ammonia water to adjust the pH value to 7.0-10.0.
2. The method for preparing the multi-element rare earth doped lithium nickelate battery cathode material as claimed in claim 1, wherein the alkaline solution is a mixed aqueous solution containing a precipitating agent and a complexing agent, the precipitating agent comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate and potassium carbonate, and the complexing agent comprises one or more of ammonia water, oxalic acid, citric acid and ethylene diamine tetraacetic acid.
3. The method for preparing the multi-element rare earth doped nickelic oxide lithium battery positive electrode material of claim 1, wherein the lithium source is one or more of lithium hydroxide, lithium carbonate, lithium oxide, lithium acetate and lithium oxalate, and the molar ratio of the lithium source to the precursor is 0.9-1.05.
4. The preparation method of the multi-element rare earth doped nickelic oxide lithium battery cathode material according to claim 1, wherein in the step 1, the pH of a system in a reaction kettle is stabilized at 10.6-11.5, the temperature is controlled at 40-60 ℃, and the stirring speed is controlled at 500-800 rpm/min.
5. A method for preparing a lithium battery positive electrode material of a polynary rare earth doped nickelic oxide according to claim 1, characterized in that the concentration of the metal salt solution is 0.5-3 mol/L, the concentration of the yttrium salt solution is 0.5-3 mol/L, the concentration of the precipitant is 1-8 mol/L, and the concentration of the complexing agent is 1-5 mol/L.
6. The multi-element rare earth doped high nickel oxide lithium battery positive electrode material prepared by the preparation method according to any one of claims 1 to 5.
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| CN111018004A (en) * | 2019-12-04 | 2020-04-17 | 浙江尚特新能源科技有限公司 | Preparation method of ternary precursor doped with rare earth elements in bulk phase and anode material thereof |
| CN110911687A (en) * | 2019-12-09 | 2020-03-24 | 中南大学 | Rare earth element modified lithium ion battery positive electrode material, and preparation method and application thereof |
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