CN111785913B - Preparation method of waxberry-shaped lithium-rich cathode material for lithium battery - Google Patents
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Abstract
A preparation method of a waxberry-shaped lithium-rich cathode material for a lithium battery relates to the technical field of lithium batteries. The preparation method of the waxberry-shaped lithium-rich cathode material for the lithium battery is simple in process, low in raw material cost, environment-friendly, and good in structural stability, capacity and voltage stability. The method comprises the following steps: 1) dissolving at least one of transition metal salts in deionized water to prepare a mixed salt solution A; 2) dissolving carbonate in deionized water to prepare a solution B; 3) adding a tartrate solution into a continuous stirring reaction kettle; 4) pumping the solution A and the solution B into a reaction kettle for reaction; 5) collecting the product after the reaction is finished, filtering, washing and drying in vacuum to obtain a carbonate precursor; 6) placing the dried carbonate precursor into a muffle furnace for calcining to obtain an oxide precursor; 7) and mixing the oxide precursor with a lithium salt, and performing heat treatment to prepare the waxberry-shaped lithium-rich cathode material.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a waxberry-shaped lithium-rich cathode material.
Background
Lithium ion batteries have been developed since the 20 th century and the 90 th era because of their advantages of good safety, high voltage, long life, and little pollution, and are now widely used in various fields. However, increasing energy storage requirements place higher demands on lithium ion batteries, and the development of high energy density and low cost lithium ion batteries is imminent (Zhang et al, Advanced Materials, 30(29), 1801751). The anode materials such as layered lithium cobaltate, spinel lithium manganate and olivine lithium iron phosphate have been widely researched, and the actual specific discharge capacities thereof have gradually approached their respective theoretical limit values, and still cannot meet the requirements of people in terms of energy density. Therefore, the development of new high-capacity cathode materials is a key point for further improving the energy density of lithium ion batteries.
The lithium-rich manganese-based positive electrode material has the advantages of high specific capacity (more than 250mAh/g), low cost, environmental friendliness and the like, and is a research hotspot in the field of chemical power sources at present. However, the rapid capacity and voltage decay caused by the structural instability of lithium-rich cathode Materials during cycling limits their commercial applications (zheng et al, Advanced Energy Materials, 2017, 7(6), 1601284). In recent years, in order to improve the electrochemical performance of lithium-rich cathode materials, researchers have made great research progress by adopting strategies such as surface coating, doping, microstructure regulation and the like. However, the problems of complicated preparation process, high cost, difficult batch production and the like of the lithium-rich cathode material still need to be further researched and solved.
Therefore, it is a very important research topic to develop an industrial preparation method capable of improving the cycle and voltage stability of the lithium-rich cathode material and reducing the production cost thereof.
Disclosure of Invention
The invention aims to provide a preparation method of a waxberry-shaped lithium-rich cathode material which has the advantages of simple process, low raw material cost, environmental friendliness, good structural stability, capacity and voltage stability and can be used for a lithium battery.
The invention comprises the following steps:
1) dissolving at least one of transition metal salts in deionized water to prepare a mixed salt solution A;
2) dissolving carbonate in deionized water to prepare a solution B;
3) adding a tartrate solution into a continuous stirring reaction kettle;
4) pumping the solution A and the solution B into a reaction kettle for reaction;
5) collecting the product after the reaction is finished, filtering, washing and drying in vacuum to obtain a carbonate precursor;
6) placing the dried carbonate precursor into a muffle furnace for calcining to obtain an oxide precursor;
7) and mixing the oxide precursor with a lithium salt, and performing heat treatment to prepare the waxberry-shaped lithium-rich cathode material.
In step 1), the transition metal salt can be selected from manganese salt, nickel salt, cobalt salt or other transition metal salts; the manganese salt can be at least one selected from manganese acetate, manganese nitrate, manganese sulfate, manganese chloride and the like; the nickel salt can be selected from at least one of nickel acetate, nickel nitrate, nickel sulfate, nickel chloride and the like; the cobalt salt can be at least one selected from cobalt acetate, cobalt sulfate, cobalt nitrate, cobalt chloride and the like; the molar ratio of the manganese salt, the nickel salt and the cobalt salt can be (2-4): 0-1); the molar concentration of the mixed salt solution A is 0.1-4 mol/L.
In the step 2), the carbonate can be potassium carbonate, sodium carbonate and other carbonates; the amount of carbonate is 1-1.5 times of that of the transition metal salt, and the molar concentration of the solution B is 0.1-6 mol/L.
In the step 3), the molar concentration of the tartrate solution is 0.01-0.1 mol/L.
In the step 4), the mixed salt solutions A and B are dropped into the reaction kettle at the same pump speed; when the solution A and the solution B are dripped into the reaction kettle, the flow rate of the peristaltic pump is controlled to be 0.1-1 mL/min, the reaction temperature is 40-80 ℃, the stirring speed is 300-600rpm, and inert gas is introduced for protection.
In the step 6), the calcining temperature can be 350-550 ℃, the calcining time can be 2-6 h, and the heating rate can be 1-10 ℃/min.
In step 7), the lithium salt may be selected from at least one of lithium acetate, lithium nitrate, lithium sulfate, lithium fluoride, lithium hydroxide, and lithium carbonate; the molar ratio of transition metal atoms in the oxide precursor to lithium in the lithium salt can be 1: 1-1.5; the temperature of the heat treatment can be 750-950 ℃, the time of the heat treatment can be 8-18 h, and the heating rate can be 1-10 ℃/min.
Compared with the existing lithium-rich layered cathode material, the lithium-rich layered cathode material has the following outstanding advantages:
the preparation of the carbonate precursor adopts a coprecipitation method at a lower temperature, water is used as a solvent, and only a small amount of tartrate is added as a complexing agent, so that the method is green and environment-friendly. The prepared precursor has uniform grain diameter, uniform element distribution and better consistency. The lithium-rich cathode material with excellent comprehensive performance is prepared by direct lithium mixing and calcining, modification measures such as doping and coating are not needed, the cost is low, and the industrial production is easy to realize. The lithium-rich cathode material prepared by the invention has a core-shell structure with a spherical core inside and a radial rod-shaped shell outside. The unique waxberry-shaped structure has good structural stability, capacity and voltage stability, and the unique morphology and exposed crystal faces enable the material to have excellent cycle and voltage stability and rate capability, so that the possibility is provided for the development of high-energy-density and low-cost lithium batteries. The preparation method has the advantages of simple process, low raw material cost, environmental friendliness and the like, and is favorable for realizing large-scale production.
Drawings
FIG. 1 shows Li obtained in example 11.2Mn0.54Co0.13Ni0.13O2XRD pattern of lithium-rich cathode material. In fig. 1, the abscissa is the 2 θ diffraction angle, and the ordinate is the diffraction intensity.
FIG. 2 shows Li obtained in example 11.2Mn0.54Co0.13Ni0.13O2Scanning electron microscopy of lithium-rich cathode materials. In FIG. 2, a is 2 μm on a scale and b is 1 μm on a scale.
FIG. 3 shows Li obtained in example 11.2Mn0.54Co0.13Ni0.13O2Transmission electron microscope image after FIB slicing of lithium-rich cathode material.
FIG. 4 shows Li obtained in example 11.2Mn0.54Co0.13Ni0.13O2Rate performance graph of lithium-rich cathode material.
FIG. 5 shows Li obtained in example 11.2Mn0.54Co0.13Ni0.13O2Electrochemical performance of the lithium-rich cathode material at a current density of 1C (250 mA/g).
Detailed Description
The invention will be described and illustrated in more detail with reference to specific examples.
The embodiment of the invention comprises the following steps:
1) dissolving at least one of transition metal salts in deionized water to prepare a mixed salt solution A; the transition metal salt can be selected from manganese salt, nickel salt, cobalt salt or other transition metal salts; the manganese salt can be at least one selected from manganese acetate, manganese nitrate, manganese sulfate, manganese chloride and the like; the nickel salt can be selected from at least one of nickel acetate, nickel nitrate, nickel sulfate, nickel chloride and the like; the cobalt salt can be at least one selected from cobalt acetate, cobalt sulfate, cobalt nitrate, cobalt chloride and the like; the molar ratio of the manganese salt, the nickel salt and the cobalt salt can be (2-4): 0-1); the molar concentration of the mixed salt solution A is 0.1-4 mol/L.
2) Dissolving carbonate in deionized water to prepare a solution B; the carbonate can be selected from carbonate such as potassium carbonate and sodium carbonate; the amount of carbonate is 1-1.5 times of that of the transition metal salt, and the molar concentration of the solution B is 0.1-6 mol/L.
3) Adding a tartrate solution into a continuous stirring reaction kettle; the molar concentration of the tartrate solution is 0.01-0.1 mol/L.
4) Pumping the mixed salt solution A and the solution B into a reaction kettle for reaction; the mixed salt solution A and the solution B are dropped into the reaction kettle at the same pump speed; when the mixed salt solution A and the solution B are dripped into the reaction kettle, the flow rate of a peristaltic pump is controlled to be 0.1-1 mL/min, the reaction temperature is 40-80 ℃, the stirring speed is 300-600rpm, and inert gas is introduced for protection.
5) Collecting the product after the reaction is finished, filtering, washing and drying in vacuum to obtain a carbonate precursor;
6) placing the dried carbonate precursor into a muffle furnace for calcining to obtain an oxide precursor; the calcining temperature can be 350-550 ℃, the calcining time can be 2-6 h, and the heating rate can be 1-10 ℃/min.
7) And mixing the oxide precursor with a lithium salt, and performing heat treatment to prepare the waxberry-shaped lithium-rich cathode material. The lithium salt can be selected from at least one of lithium acetate, lithium nitrate, lithium sulfate, lithium fluoride, lithium hydroxide and lithium carbonate; the molar ratio of transition metal atoms in the oxide precursor to lithium in the lithium salt can be 1: 1-1.5; the temperature of the heat treatment can be 750-950 ℃, the time of the heat treatment can be 8-18 h, and the heating rate can be 1-10 ℃/min.
Specific examples are given below.
Example 1
Preparation of molecular formula Li1.2Mn0.54Co0.13Ni0.13O2Lithium-rich cathode material
57.5g of manganese sulfate monohydrate, 23.6g of cobalt sulfate heptahydrate and 22.0g of nickel sulfate hexahydrate are weighed according to the stoichiometric ratio (Mn: Co: Ni: 4: 1) and dissolved in 1L of deionized water to prepare a solution A with the concentration of 0.5 mol/L. 53g of sodium carbonate is weighed and dissolved in 1L of deionized water to prepare 0.5mol/L solution B. 1L of deionized water and 4g of sodium tartrate were added to the reaction vessel at a stirring speed of 500rpm and a temperature of 50 ℃. Solution A and solution B were added dropwise to the reaction vessel at a rate of 1mL/min by a peristaltic pump. And aging for 5 hours after the dropwise addition is finished, and filtering, washing and drying to obtain a carbonate precursor.
And placing the obtained carbonate precursor in a muffle furnace, and calcining for 5 hours at 500 ℃ to obtain an oxide precursor. After cooling, the oxide precursor was uniformly mixed with lithium hydroxide monohydrate (molar ratio of lithium ion to transition metal Li/TM 1.25), and the resulting mixture was calcined in a muffle furnace at 800 ℃ for 12 hours at a temperature rise rate of 10 ℃/min. Furnace cooling to obtain waxberry-shaped Li1.2Mn0.54Co0.13Ni0.13O2A lithium-rich cathode material.
Example 1 preparation of Li1.2Mn0.54Co0.13Ni0.13O2The XRD pattern of the lithium-rich cathode material is shown in FIG. 1, and Li prepared in example 11.2Mn0.54Co0.13Ni0.13O2A scanning electron micrograph of the lithium-rich cathode material is shown in figure 2. Li1.2Mn0.54Co0.13Ni0.13O2Transmission electron of lithium-rich cathode material after FIB slicingSee figure 3 for a sub-microscope. Li1.2Mn0.54Co0.13Ni0.13O2The rate capability of the lithium-rich cathode material is shown in fig. 4. Li1.2Mn0.54Co0.13Ni0.13O2The electrochemical performance of the lithium-rich cathode material at a current density of 1C (250 mA/g) is shown in fig. 5.
Example 2
Preparation of molecular formula Li1.2Mn0.6Ni0.2O2Lithium-rich cathode material
148.4g of manganese chloride tetrahydrate and 59.4g of nickel chloride hexahydrate are weighed according to the stoichiometric ratio (Mn: Ni ═ 3: 1) and dissolved in 500ml of deionized water to prepare a solution A with the concentration of 2 mol/L. 106g of sodium carbonate is weighed and dissolved in 500mL of deionized water to prepare 2mol/L solution B. 1L of deionized water and 4g of sodium tartrate were added to the reaction kettle, the stirring speed was 500rpm, and the temperature was set at 60 ℃. Solution A and solution B were added dropwise to the reaction vessel at a rate of 0.5mL/min by a peristaltic pump. And aging for 5 hours after the dropwise addition is finished, and filtering, washing and drying to obtain a carbonate precursor.
And placing the prepared carbonate precursor in a muffle furnace, and calcining for 5 hours at 500 ℃ to obtain an oxide precursor. After cooling, the oxide precursor was uniformly mixed with lithium carbonate (molar ratio of lithium ion to transition metal Li/TM 1.3). And placing the obtained mixture in a muffle furnace, calcining for 10h at 800 ℃, and raising the temperature at a rate of 10 ℃/min. Furnace cooling to obtain waxberry-shaped Li1.2Mn0.6Ni0.2O2A lithium-rich cathode material.
Firstly, preparing a transition metal carbonate precursor by adopting a coprecipitation method; the precursor is uniformly mixed with lithium salt according to a certain proportion after being calcined, and then the waxberry-shaped lithium-rich cathode material is prepared after calcination. The material is of a core-shell structure, wherein the interior of the material is a spherical core, and the exterior of the material is a shell layer consisting of radial rods. The lithium-rich cathode material synthesized by the invention is a secondary micron sphere with the diameter of about 12 microns, the inner core is a sphere consisting of primary nano particles, and the shell layer is formed by arranging radial micron rods. When the waxberry-shaped lithium-rich material is used as a lithium battery anode material, the material has excellent cycle and voltage stability and rate capability: the specific capacity can reach 250mAh/g when the current is circulated under the current density of 1C, the specific capacity can still be kept at 218mAh/g after 500 times of circulation, and the voltage retention rate is 89.6 percent after 500 cycles; the specific capacity of the material reaches 199mAh/g when the material is cycled at 5 ℃. The preparation method has the advantages of simple process, low cost and environmental friendliness, and is suitable for large-scale production. The specific capacity of 250mAh/g can be provided under the current density of 1C, and the specific capacity of 218mAh/g and 89% of voltage can be still maintained after 500 times of circulation. Under the current density of 5C, the specific capacity can reach 199mAh/g, and good cycle and voltage stability and rate capability are shown.
The foregoing is only a preferred embodiment of the present invention. It should be noted that those skilled in the art can make appropriate modifications without inventive step without departing from the scope of the present invention.
Claims (8)
1. A preparation method of a waxberry-shaped lithium-rich cathode material for a lithium battery is characterized by comprising the following steps of:
1) dissolving at least one of transition metal salts in deionized water to prepare a mixed salt solution A; the transition metal salt is selected from manganese salt, nickel salt, cobalt salt or other transition metal salts; the manganese salt is selected from at least one of manganese acetate, manganese nitrate, manganese sulfate and manganese chloride; the nickel salt is selected from at least one of nickel acetate, nickel nitrate, nickel sulfate and nickel chloride; the cobalt salt is at least one selected from cobalt acetate, cobalt sulfate, cobalt nitrate and cobalt chloride; the molar ratio of the manganese salt, the nickel salt and the cobalt salt is (2-4): 0-1); the molar concentration of the mixed salt solution A is 0.1-4 mol/L;
2) dissolving carbonate in deionized water to prepare a solution B;
3) adding a tartrate solution into a continuous stirring reaction kettle;
4) pumping the mixed salt solution A and the solution B into a reaction kettle for reaction;
5) collecting the product after the reaction is finished, filtering, washing and drying in vacuum to obtain a carbonate precursor;
6) placing the dried carbonate precursor into a muffle furnace for calcining to obtain an oxide precursor;
7) and mixing the oxide precursor with a lithium salt, and performing heat treatment to prepare the waxberry-shaped lithium-rich cathode material.
2. The method as claimed in claim 1, wherein in the step 2), the carbonate is selected from potassium carbonate and sodium carbonate; the amount of carbonate is 1-1.5 times of that of the transition metal salt, and the molar concentration of the solution B is 0.1-6 mol/L.
3. The method according to claim 1, wherein in the step 3), the tartrate solution has a molar concentration of 0.01 to 0.1 mol/L.
4. The method according to claim 1, wherein in step 4), the mixed salt solution A and the solution B are dropped into the reaction kettle at the same pumping speed; when the mixed salt solution A and the solution B are dripped into the reaction kettle, the flow rate of the peristaltic pump is controlled to be 0.1-1 mL/min, the reaction temperature is 40-80 ℃, the stirring speed is 300-600rpm, and inert gas is introduced for protection.
5. The method according to claim 1, wherein in the step 6), the calcination temperature is 350-550 ℃, the calcination time is 2-6 h, and the temperature increase rate is 1-10 ℃/min.
6. The method according to claim 1, wherein in step 7), the lithium salt is at least one selected from the group consisting of lithium acetate, lithium nitrate, lithium sulfate, lithium fluoride, lithium hydroxide, and lithium carbonate.
7. The method according to claim 1, wherein in step 7), the molar ratio of transition metal atoms in the oxide precursor to lithium atoms in the lithium salt is 1: 1-1.5.
8. The method according to claim 1, wherein in step 7), the heat treatment temperature is 750-950 ℃, the heat treatment time is 8-18 h, and the temperature rise rate is 1-10 ℃/min.
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| CN102881886A (en) * | 2012-09-24 | 2013-01-16 | 中国海洋石油总公司 | Method for preparing high-tap-density spherical lithium-rich manganese-based anode material |
| CN104241634A (en) * | 2014-09-29 | 2014-12-24 | 奇瑞汽车股份有限公司 | Lithium and manganese-rich cathode material of lithium ion battery and preparation method of cathode material |
| CN106711434A (en) * | 2015-08-05 | 2017-05-24 | 北京化工大学 | Urchin-like sodium-containing lithium-rich layered cathode material and preparation method thereof |
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| CN102881886A (en) * | 2012-09-24 | 2013-01-16 | 中国海洋石油总公司 | Method for preparing high-tap-density spherical lithium-rich manganese-based anode material |
| CN104241634A (en) * | 2014-09-29 | 2014-12-24 | 奇瑞汽车股份有限公司 | Lithium and manganese-rich cathode material of lithium ion battery and preparation method of cathode material |
| CN106711434A (en) * | 2015-08-05 | 2017-05-24 | 北京化工大学 | Urchin-like sodium-containing lithium-rich layered cathode material and preparation method thereof |
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