CN110642300A - Preparation method of micron-sized carbonate lithium ion battery cathode material - Google Patents
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Abstract
The invention discloses a preparation method of a micron-sized carbonate lithium ion battery cathode material, belonging to the field of preparation of lithium ion battery electrode materials. The invention aims to solve the technical problems of high cost, industrial payment and low reproducibility of actual production in the existing method. The method comprises the following steps: preparing a mixed solution of metal acetate and ammonium bicarbonate; carrying out solvent thermal reaction, and cooling to obtain a solid-phase substance; and centrifuging, removing impurities and drying the solvent hot product to obtain the micron-sized carbonate lithium ion battery cathode material. The product of the invention has spherical or ellipsoidal particle shape and particle size of 0.5-20 μm.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery cathode materials; in particular to a preparation method of a micron-sized carbonate lithium ion battery cathode material.
Background
The lithium ion battery has high energy density, is green and environment-friendly, has higher voltage, and can be well adapted to devices such as transistors, and the like, thereby being widely applied to equipment such as mobile phones, cameras and the like. Meanwhile, the lithium ion battery is beneficial to relieving crisis caused by fossil energy, and is widely applied to the field of electric automobiles at present.
The electrode material is the key point influencing the performance of the lithium ion battery, and the current commercially used cathode material is mainlyIs a graphite material, and the specific capacity of the graphite cathode material is 372mAh g-1In addition to affecting safety due to its tendency to generate lithium dendrites, graphite materials have difficulty meeting current needs under the dual requirements of current situation and policy. The transition metal oxide negative electrode material has high capacity and is not easy to generate lithium dendrite, but the preparation of the transition metal oxide negative electrode material usually needs to generate a precursor in advance and then obtain a final product through high-temperature calcination. The carbonate serving as a common precursor for preparing the oxide has the specific capacity equivalent to that of the oxide, and compared with an oxide material, the method has the advantages of one-step process reduction, easiness in preparation and cost reduction. When the cathode material is modified by carbon materials such as nano-materials and composite graphene, the cost is increased, and the tap density of the material is reduced, so that the further practicability of the material is hindered. In addition, the morphology of the past materials is changed by using a morphology control agent, so that the cost of raw materials is increased, the process is complicated, and the repeatability in the actual production is reduced.
Disclosure of Invention
The present invention has one of the objects: the carbonate cathode material is used as an active material, and the target of high capacity is reserved facing the oxide cathode material, so that the high-temperature complex process is eliminated;
the second object of the present invention is: the design of hollow or nano materials is not selected, the material is not suitable for compounding carbon materials such as graphene and the like, and the morphology directing agent is not suitable, so that the material has the advantages of saving cost under the condition of better tap density and still keeping higher capacity.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the micron-sized carbonate lithium ion battery cathode material is carried out according to the following steps:
step one, preparing a mixed solution taking metal acetate and ammonium bicarbonate as solutes;
secondly, carrying out solvothermal reaction;
and step three, centrifuging to remove impurities, and drying to finally obtain micron-sized carbonate powder.
Further, the concentration of the metal acetate in the mixed solution in the first step is 0.01mol/L to 0.05 mol/L.
Further, in the first step, the metal acetate is cobalt acetate, manganese acetate or nickel acetate.
Further, the concentration of ammonium bicarbonate in the mixed solution in the first step is 0.1 mol/L-0.8 mol/L.
Further, the mixed solution in the first step is prepared by using diethylene glycol ether, ethylene glycol or deionized water as a solvent.
Further limiting, stirring or ultrasonic process is needed to be assisted in the preparation process of the mixed solution in the step one, wherein the stirring speed is 300-1200 rpm, and the time is 5 min-3 h.
And further limiting, the solvothermal reaction in the step two is carried out in a reaction kettle with a Teflon liner, wherein the temperature of the solvothermal reaction is 150-220 ℃, the solvothermal reaction enters a furnace when the temperature is reached, and the solvothermal reaction is cooled along with the furnace after being heated for 6-15 hours.
Further limiting, the specific process of centrifugal impurity removal in the third step is as follows: and sequentially centrifuging the mixture three times by using deionized water and ethanol respectively, wherein the centrifugation rotating speed is 2000-10000 rpm each time, and the centrifugation time is 5-10 min each time.
And further limiting, the specific process of drying in the third step is to remove supernatant after the centrifugation is finished, and the remained solid-phase substance is dried at the temperature of 30-100 ℃ for 6-24 h.
The micron-sized carbonate cathode material prepared by the method has the particle size of 0.5-20 mu m, and does not form a hollow or other hierarchical structure.
The micron-sized carbonate cathode material prepared by the method has a spherical or ellipsoidal particle shape, and is modified without depending on carbon materials such as graphene and the like or other shape control.
The micron-sized carbonate cathode material prepared by the method has the advantages of simple and safe preparation process and low production cost, and is expected to be produced in a large scale.
The micron-sized carbonate cathode material prepared by the method is used as a cathode material of a lithium ion battery.
Drawings
FIG. 1 is an XRD spectrum of a micron-sized cobalt carbonate negative electrode material in examples 1-3;
FIG. 2 is an SEM photograph of the micron-sized cobalt carbonate negative electrode material of example 1, wherein a is 5 μm, b is 1 μm, c is 500nm, and d is 200 nm;
FIG. 3 is an SEM photograph of the micron-sized cobalt carbonate cathode material of example 2, a-5 μm, b-2 μm, c-500 nm, d-200 nm;
FIG. 4 is an SEM photograph of the micron-sized cobalt carbonate negative electrode material of example 3, wherein a is 20 μm, b is 10 μm, c is 5 μm, and d is 1 μm;
FIG. 5 is a TEM photograph of the micron-sized cobalt carbonate anode material in example 1, a-500 nm, b-200 nm;
FIG. 6 is a 0.2C cycle performance test curve of the micron-sized cobalt carbonate negative electrode material in examples 1-3;
FIG. 7 is a 1C cycle performance test curve of the micron-sized cobalt carbonate negative electrode material in examples 1-3;
FIG. 8 is a curve of the rate test of the micron cobalt carbonate negative electrode material in examples 1-3.
Detailed Description
Example 1, the present example is a method for preparing a micron-sized cobalt carbonate negative electrode material, which is performed according to the following steps:
step one, dissolving 1mmol of cobalt acetate and 10mmol of ammonium bicarbonate in 30ml of diethylene glycol ether, directly dissolving the cobalt acetate and the ammonium bicarbonate simultaneously, wherein the dissolution is slow, the dissolution process is accelerated by using a repeated ultrasonic and stirring method, the single stirring time or the ultrasonic time is 30min, the total time is 2h, and the stirring speed is 500rpm, and finally obtaining a red solution;
step two, performing solvothermal reaction on the mixed solution in the step one in a reaction kettle with a Teflon inner container of 50ml at the reaction temperature of 200 ℃, heating for 15 hours, stopping heating, cooling along with the furnace, and finally retaining pink solid-phase precipitate in the inner container;
and step three, centrifuging the solid-phase product obtained in the step two for three times by using deionized water, then centrifuging the solid-phase product for three times by using absolute ethyl alcohol, wherein the rotating speed of each centrifugation is 8000rpm to remove soluble impurities, removing supernatant after the centrifugation is finished, and drying the precipitate in a 60-DEG C forced air drying oven for 12 hours to obtain micron-sized cobalt carbonate particles.
step one, dissolving 1mmol of cobalt acetate and 10mmol of ammonium bicarbonate in 30ml of ethylene glycol, directly dissolving the cobalt acetate and the ammonium bicarbonate simultaneously, wherein the dissolution is slow, the dissolution process is accelerated by using a method of repeated ultrasound and stirring, the single stirring time or the ultrasound time is 15min, the total time is 1h, the stirring speed is 500rpm, and finally, a red solution is obtained;
step two, performing solvothermal reaction on the mixed solution in the step one in a reaction kettle with a Teflon inner container of 50ml at the reaction temperature of 200 ℃, heating for 15 hours, stopping heating, cooling along with the furnace, and finally retaining pink solid-phase precipitate in the inner container;
and step three, centrifuging the solid-phase product obtained in the step two for three times by using deionized water, then centrifuging the solid-phase product for three times by using absolute ethyl alcohol, wherein the rotating speed of each centrifugation is 8000rpm to remove soluble impurities, removing supernatant after the centrifugation is finished, and drying the precipitate in a 60-DEG C forced air drying oven for 12 hours to obtain micron-sized cobalt carbonate particles.
Embodiment 3, which is a method for preparing a micron-sized cobalt carbonate negative electrode material, is performed according to the following steps:
step one, dissolving 1mmol of cobalt acetate in 10ml of deionized water, and performing ultrasonic treatment for 5min to accelerate solid phase. Dissolving 10mmol ammonium bicarbonate in 20ml deionized water, and magnetically stirring at 300rpm for 5min to accelerate the dissolution process. Keeping the ammonium bicarbonate solution in a stirring state, and slowly dripping cobalt acetate solution into the ammonium bicarbonate solution at a constant speed for 5 min. After the dropwise addition is finished, stirring at the speed of 500rpm for 10 min;
step two, performing solvothermal reaction on the mixed solution in the step one in a reaction kettle with a Teflon inner container of 50ml at the reaction temperature of 200 ℃, heating for 15 hours, stopping heating, cooling along with the furnace, and finally retaining pink solid-phase precipitate in the inner container;
and step three, centrifuging the solid-phase product obtained in the step two for three times by using deionized water, then centrifuging the solid-phase product for three times by using absolute ethyl alcohol, wherein the rotating speed of each centrifugation is 8000rpm to remove soluble impurities, removing supernatant after the centrifugation is finished, and drying the precipitate in a 60-DEG C forced air drying oven for 12 hours to obtain micron-sized cobalt carbonate particles.
The XRD spectrogram of the micron-sized cobalt carbonate lithium ion battery cathode material prepared in the embodiments 1-3 is shown in figure 1, and it can be seen from figure 1 that the diffraction peak positions of the three products are completely consistent with a standard card (JCPDS card NO.11-0692), which indicates that the products obtained by the three preparation methods are pure-phase cobalt carbonate.
The SEM photograph of the micron-sized cobalt carbonate lithium ion battery negative electrode material prepared in example 1 is shown in fig. 2, and it can be seen from fig. 2 that the size of cobalt carbonate is about 1 μm, the particle dispersibility is good, and the cobalt carbonate is in the shape of an ellipsoid with a rough surface.
The SEM photograph of the micron-sized cobalt carbonate lithium ion battery negative electrode material prepared in example 2 is shown in fig. 3, and it can be seen from fig. 2 that the size of cobalt carbonate is about 1.5 μm, the particle dispersibility is good, and the shape is also an ellipsoid with a rough surface. From fig. 3c it can be seen that the surface roughness is slightly greater than in example 1.
An SEM photograph of the micron-sized cobalt carbonate lithium ion battery negative electrode material prepared in example 3 is shown in fig. 4, and it can be seen from fig. 2 that the size of cobalt carbonate is about 5 μm, the particle dispersibility is good, and the cobalt carbonate is in an ellipsoid shape with uneven surface. It is clearly perceived as a combination of smaller sized particles.
A TEM photograph of the micron-sized cobalt carbonate lithium ion battery negative electrode material prepared in example 1 is shown in fig. 5, wherein the cobalt carbonate particles have a substantially solid structure, the large particles are formed by combining smaller particles, and the material contains a certain amount of pores. It can be seen that the three particles have substantially similar particle structures.
Micron-sized cobalt carbonate lithium ion battery negative electrode material 0.1C (1C ═ 1000 mAg) prepared in examples 1-3-1) The cycle performance test curve is shown in FIG. 6, and the cobalt carbonate material of example 1 has 1023.2/1015.6mAh g at 20 charging and discharging cycles under low current density-1Has excellent discharge/charge specific capacityThe lithium storage capacity of the material is good. The specific discharge/charge capacities of the products of examples 2 and 3 at 20 circles are 873/864mAh g-1And 617.8/612.9mAh g-1. In addition, all three have higher coulombic efficiencies of 72.95%, 66.93% and 73.92%, respectively.
The 1C cycle performance test curve of the micron-sized cobalt carbonate lithium ion battery cathode material prepared in the embodiments 1-3 is shown in FIG. 7, and in the 1C high-current charge and discharge test process, the capacity of the material is kept stable when the material circulates for 200 circles, and the capacity reaches 824.6/820.8mAh g-1The discharge/charge specific capacity of the battery is high, and the battery has high large-current cycle performance. The specific discharge/charge capacities of the products of examples 2 and 3 at 200 cycles are 713.3/712.2mAh g respectively under the condition of 1C current density-1And 405.5/405.6mAh g-1。
The curve of the rate performance test curve of the micron-sized cobalt carbonate lithium ion battery negative electrode material prepared in the examples 1 to 3 is shown in fig. 8, and under the condition that the serving current density is gradually increased, the average specific capacities of the cobalt carbonate material in the example 1 are 1014, 841, 711, 595 and 476mAh g at 0.1, 0.2, 0.5, 1 and 2C respectively-1. When the temperature is recovered to 0.1C, the capacity is basically recovered, and then the circulation is carried out to 100 circles at 0.5C, and the capacity is 664.5/660mAh g-1The discharge/charge specific capacity of the lithium ion battery has better rate capability. The curves of examples 2 and 3 have the same tendency as example 1, and the specific capacity can be recovered to a higher level after the discharge of a large current.
Claims (9)
1. A preparation method of a micron-sized carbonate lithium ion battery cathode material is characterized by comprising the following steps:
step one, preparing a mixed solution taking metal acetate and ammonium bicarbonate as solutes;
secondly, carrying out solvothermal reaction;
and step three, centrifuging to remove impurities, and drying to finally obtain micron-sized carbonate powder.
2. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: the concentration of the metal acetate in the mixed solution in the first step is 0.01 mol/L-0.05 mol/L.
3. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: in the first step, the metal acetate is cobalt acetate, manganese acetate or nickel acetate.
4. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: and step one, the concentration of ammonium bicarbonate in the mixed solution is 0.1-0.8 mol/L.
5. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: the solvent for preparing the mixed solution in the first step is diethylene glycol ether, ethylene glycol or deionized water.
6. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: step one, the preparation process of the mixed solution needs to be assisted by stirring or ultrasonic process, wherein the stirring speed is 300 rpm-1200 rpm, and the time is 5 min-3 h.
7. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: and secondly, carrying out the solvothermal reaction in a reaction kettle with a Teflon liner, wherein the temperature of the solvothermal reaction is 150-220 ℃, entering the furnace after reaching the temperature, heating for 6-15 h, and cooling along with the furnace.
8. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: step three, the specific process of centrifugal impurity removal is as follows: and sequentially centrifuging the mixture for three times by using deionized water and absolute ethyl alcohol respectively, wherein the centrifugal rotating speed is 2000 rpm-10000 rpm each time, and the centrifugal time is 5 min-10 min each time.
9. The method for preparing the micron-sized carbonate lithium ion battery anode material according to claim 1, is characterized in that: the specific process of drying in the third step is that supernatant liquid after the centrifugation is finished is removed, and the remained solid-phase substance is dried at the temperature of 30-100 ℃ for 6-24 h.
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| CN112960702A (en) * | 2021-04-23 | 2021-06-15 | 华中科技大学 | Preparation method of cobaltosic oxide with thermochemical energy storage performance and product |
| CN113213558A (en) * | 2021-07-09 | 2021-08-06 | 金驰能源材料有限公司 | Large-particle spherical cobalt carbonate precursor, preparation method thereof and preparation method of cobaltosic oxide |
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| CN113213558A (en) * | 2021-07-09 | 2021-08-06 | 金驰能源材料有限公司 | Large-particle spherical cobalt carbonate precursor, preparation method thereof and preparation method of cobaltosic oxide |
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