CN109301185B - Ternary cathode material with high conductivity and preparation method thereof - Google Patents
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
A ternary positive electrode material with high conductivity is characterized in that: comprises a kernel and a shell coated on the outer surface of the kernel; has the following chemical formula: licNiaCobMn1‑a‑bO2Wherein a is more than or equal to 0 and less than or equal to 1, b is more than or equal to 0 and less than or equal to 1, and c is more than or equal to 0.4 and less than or equal to 1.5; the inner core is made of ternary materials of nickel, cobalt and manganese coated by lithium, and the shell is a film of a conductive polymer. In the invention, the thin film of the shell has higher conductivity, and the surface impedance of the ternary material can be reduced, so that the rate capability of the battery is improved. Meanwhile, the ternary cathode material can be better combined with a binder, so that impedance can be prevented from being increased to a certain extent in the charge and discharge processes, and the cycle performance of the material is improved.
Description
Technical Field
The invention relates to a lithium ion battery, in particular to a ternary cathode material with high conductivity of the lithium ion battery and a preparation method thereof.
Background
At present, fossil fuels remain the main power supply resource. However, with unreasonable exploitation and utilization of human beings, fossil energy is increasingly in tension, and environmental pollution is increasingly serious. Therefore, it is urgent to develop and utilize new clean resources and renewable energy sources such as solar energy, wind energy, tidal energy, etc. On the other hand, the normal operation of the power grid requires stable and continuous power generation, and solar energy, wind energy, tidal energy and the like are limited by factors such as weather, places, time and the like, so that the large-scale application and popularization of the power grid are greatly limited. In order to solve this problem, large-scale electricity storage technology has become an important research area. Among them, the secondary battery has high energy density and conversion efficiency, and is a priority for large-scale electricity storage, and the lithium ion battery having a long cycle life and the highest energy density is considered as the most promising secondary battery. Since the successful emergence of the lithium ion battery in the 90 th of the 20 th century, the lithium ion battery has been applied to electric automobiles, portable electronic equipment and the like on a considerable scale, but with the continuous progress and development of the lithium ion battery, a series of hidden dangers are gradually exposed to the visual field of people.
Under high pressure, the components in the electrolyte decompose to produce a large amount of gas that corrodes the positive electrode material, thereby dissolving the metal ions. Under the condition, the problem can be well solved by modifying the surface of the ternary material by using the metal oxide, and the cycle performance of the material can be improved, but the modification by using the metal oxide brings a new problem that the surface impedance of the ternary material can be improved, so that the first discharge specific capacity of the material is small.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a ternary cathode material with high conductivity and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a ternary cathode material with high conductivity comprises a core and a shell coated on the outer surface of the core; has the following chemical formula:
LicNiaCobMn1-a-bO2
wherein a is more than or equal to 0 and less than or equal to 1, b is more than or equal to 0 and less than or equal to 1, and c is more than or equal to 0.4 and less than or equal to 1.5;
the inner core is a ternary material of lithium-coated nickel, cobalt and manganese, and the shell is a film of a conductive polymer; the conductive polymer is obtained by carrying out polymerization reaction on acetylene, pyrrole, thiophene and derivatives thereof.
In the invention, a layer of film with very stable chemical property is formed on the surface of the inner core, and the layer of film is a non-metal film which does not influence the subject structure of the inner core and can simultaneously prevent the corrosion of gas generated by the decomposition of the electrolyte under high pressure to the inner core and protect the material structure; from the viewpoint of chemical reaction, decomposition of the electrolytic solution can be suppressed to some extent.
In the invention, the thin film of the shell has higher conductivity, and the surface impedance of the ternary material can be reduced, so that the conductivity of the anode is improved, and the rate capability of the battery is improved. Meanwhile, the conductive polymer coating can prevent impedance from increasing in the charging and discharging process, and the cycle performance of the material is improved. The cycle performance of a lithium battery is determined by one of the difference between the cycle performance of a positive electrode matched with an electrolyte and the cycle performance of a negative electrode matched with the electrolyte.
It is known that, the negative electrode of the lithium battery generally adopts a carbon-coated aluminum foil/copper foil, namely, the dispersed nano conductive graphite and carbon-coated particles are uniformly and finely coated on the aluminum foil/copper foil. The conductive material can provide excellent static conductivity, collect micro-current of active material, thereby greatly reducing contact resistance between positive/negative electrode material and current collection, improving adhesion between the positive/negative electrode material and the current collection, reducing the usage amount of binder, and further significantly improving the overall performance of the battery. The nano conductive graphite is an excellent conductor, and can reduce the internal resistance of the battery and inhibit the dynamic internal resistance amplification in the charge-discharge cycle process.
The conductive agent of the active material on the positive electrode of the lithium battery only accounts for about 3 percent of the weight of the positive electrode material, the dosage of the binder is more than that of the negative electrode, and the cycle performance of the positive electrode matched with the electrolyte is generally not as high as that of the positive electrode matched with the electrolyte; therefore, the improvement of the cycle performance of the matched anode and the electrolyte is actually to improve the cycle performance of the lithium battery.
The conductive polymer adopted by the shell is an organic material, has good thermal stability, can be kept for 1000 hours at 120 ℃, and has basically unchanged conductivity; polyvinylidene fluoride (PVDF) is generally adopted in industry as a binder of a lithium ion battery; the conductive polymer and the binder adopted by the shell can be combined more tightly, and the structure of the positive pole piece can be stabilized better. In the charge and discharge cycle process of some lithium ion batteries, the interior of the lithium ion battery can generate heat, the binder can expand and contract to a certain degree, the traditional ternary cathode materials are all metal ions, the expansion coefficient difference between the traditional ternary cathode materials and the binder is large, and the phenomenon that the ternary cathode materials are separated from the binder is easy to occur, so that the resistance between the active material and the binder is increased, and the internal resistance of the lithium ion battery is also increased. In the invention, the existence of the conductive polymer on the surface of the ternary cathode material can play a certain buffer role between the adhesive and the inner core, so that the ternary cathode material of the adhesive is tightly connected in the continuous expansion and contraction process, and the electronic contact between the active material and the current collector is ensured.
Preferably, the particle size of the core is 2-20 μm, and the thickness of the shell is 5-50 nm.
A preparation method of a ternary cathode material with high conductivity comprises the following steps of 1) preparing a multi-element mixed solution of nickel salt, cobalt salt and manganese salt with a preset proportion,
2) adding the multicomponent mixed solution obtained in the step 1), ammonia water and a sodium hydroxide solution into a reaction device containing a base solution in a concurrent flow manner, and carrying out a coprecipitation reaction to obtain a sodium hydroxide precursor; the whole process is carried out under the protection of inert gas atmosphere;
3) filtering the reaction product obtained in the step 2) to obtain a precipitate, and washing the precipitate with deionized water until the filtrate is neutral;
4) drying in a hot air circulation oven for 10-12h to obtain a ternary material precursor;
5) mixing the ternary precursor of the step 4) with Li2CO3Uniformly mixing and grinding the materials according to the stoichiometric ratio of 2:1.1, and then sintering to obtain an inner core; the D50 of the kernel granularity obtained by the invention is 10-12um, and the tap density is 1.8-2.5g/cm3Specific surface area of 4-7g/m2。
6) Immersing the kernel in the step 5) into a conductive polymer monomer solution, firstly mechanically stirring for 0.5-10h, and then ultrasonically dispersing for 0.5-72 h; the monomer solution comprises a monomer and absolute ethyl alcohol, and the molar ratio of the monomer to the absolute ethyl alcohol is 1:10-1: 1. The solid-liquid ratio of the inner core to the monomer solution is 40-60 g/L.
7) Drying the kernel obtained in the step 6) at room temperature to 70 ℃ for 30-360 min; when drying, the excessive monomer solution can be volatilized, so that the thickness of the coating of the shell is ensured.
8) Immersing the inner core in the step 7) in an oxidant, wherein the oxidant is one or more of iron p-toluenesulfonate, ammonium persulfate, sodium persulfate, ammonium sulfate and ferric chloride; the concentration of the oxidant solution is 10-70 wt%; after the impregnation with the oxidant, carrying out polymerization reaction in a polymerization oven, wherein the highest temperature of the reaction is 200 ℃, and the reaction time is 55-65 min;
9) washing the ternary cathode material obtained in the step 8) with ethanol, filtering, and drying at the temperature of 40-120 ℃ to obtain the product.
In the preparation method of the ternary cathode material with high conductivity, preferably, the low solution in the step 2) is a mixed solution of sodium hydroxide and ammonia water; the concentration of the sodium hydroxide solution in the base solution is 7.5-10mol/L, and the concentration of the ammonia water is 6-8 mol/L.
In the above preparation method of the ternary cathode material with high conductivity, preferably, in step 1), the nickel salt is at least one of nickel nitrate, nickel chloride, nickel acetate and nickel sulfate; the manganese salt is at least one of manganese nitrate, manganese chloride, manganese acetate and manganese sulfate; the cobalt salt is at least one of cobalt nitrate, cobalt chloride, cobalt acetate and cobalt sulfate.
In the method for preparing the ternary cathode material with high conductivity, the total ion concentration of the multi-element mixed solution obtained in the step 1) is preferably 1-1.5 mol/L, the concentration of the sodium hydroxide solution flowing in the step 2) is preferably 7.5-10mol/L, and the concentration of the ammonia water flowing in is preferably 6-8 mol/L.
In the preparation method of the ternary cathode material with high conductivity, preferably, the feeding speed of the mixed solution in the step 2) is 90-150ml/min, the feeding speed of the sodium hydroxide is 30-70ml/min, and the feeding speed of the ammonia water is 5-40 ml/min. The growth speed of the particles in the range is stable, and the sphericity is good.
In the preparation method of the ternary cathode material with high conductivity, preferably, the pH value of the coprecipitation reaction in the step 2) is 10-12, the ammonium ion concentration is 5-9g/L, the reaction temperature is 50-60 ℃, and the stirring speed is 200-400 r/min. The range is favorable for uniform growth of particles, the dispersibility is good, and the particles are prevented from agglomerating.
Preferably, the sintering in the step 5) is carried out in three steps, namely, the temperature rise rate is 4 ℃ min-1Heating to 400-; ② then heating up at a rate of 2 ℃ for min-1Heating to 580 ℃ and 600 ℃, and preserving heat for 3 h; thirdly, heating rate is 1 ℃ and min-1Heating to 750 ℃ and 900 ℃ and preserving the temperature for 15h to obtain the product.
In the above method for preparing a ternary cathode material with high conductivity, preferably, the conductive polymer monomer in step 6) includes acetylene, pyrrole, thiophene and derivatives thereof.
Preferably, in the step 8, the polymerization reaction is divided into two stages, wherein the first stage temperature is 60-65 ℃, the polymerization time is 25-30 min, and the second stage temperature is 165-170 ℃, and the polymerization time is 30-35 min.
In the invention, a layer of film with very stable chemical property is formed on the surface of the inner core, and the layer of film is a non-metal film which does not influence the subject structure of the inner core and can simultaneously prevent the corrosion of gas generated by the decomposition of the electrolyte under high pressure to the inner core and protect the material structure; from the viewpoint of chemical reaction, decomposition of the electrolytic solution can be suppressed to some extent.
In the invention, the thin film of the shell has higher conductivity, and the surface impedance of the ternary material can be reduced, so that the conductivity of the anode is improved, and the rate capability of the battery is improved. Meanwhile, the ternary cathode material can be better combined with a binder, so that impedance can be prevented from being increased to a certain extent in the charge and discharge processes, and the cycle performance of the material is improved.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
A preparation method of a ternary cathode material with high conductivity comprises the following steps of 1) preparing a multi-element mixed solution of nickel salt, cobalt salt and manganese salt, wherein the stoichiometric ratio of Ni in the mixed solution is as follows: co: mn is 5: 2: 3.
2) adding the multicomponent mixed solution obtained in the step 1), ammonia water and a sodium hydroxide solution into a reaction device containing a base solution in a concurrent flow manner, and carrying out a coprecipitation reaction to obtain a sodium hydroxide precursor; the whole process is carried out at N2Under the protection of the atmosphere;
3) filtering the reaction product obtained in the step 2) to obtain a precipitate, and washing the precipitate with deionized water until the filtrate is neutral;
4) drying in a hot air circulation oven for 10-12h to obtain Ni0.5Co0.2Mn0.3(OH)2A precursor;
5) mixing the ternary precursor of the step 4) with Li2CO3Mixing and grinding uniformly according to the stoichiometric ratio of 2:1.1, sintering, and obtaining LiNi0.5Co0.2Mn0.3A material, namely an inner core;
6) immersing the kernel obtained in the step 5) into a 3, 4-Ethylenedioxythiophene (EDOT) monomer solution, firstly mechanically stirring for 2 hours, and then ultrasonically dispersing for 5 hours; the monomer solution comprises a monomer and absolute ethyl alcohol, and the molar ratio of the monomer to the absolute ethyl alcohol is 1: 10. The solid-liquid ratio of the inner core to the monomer solution was 45 g/L.
7) Drying the inner core in the step 6) at room temperature for 360 min;
8) immersing the kernel in the step 7) in an oxidant, wherein the oxidant is ferric p-toluenesulfonate; the concentration of the oxidant solution is 35 wt%; after the impregnation with the oxidant, carrying out polymerization reaction in a polymerization oven, wherein the highest temperature of the reaction is 200 ℃, and the reaction time is 55-65 min; the polymerization reaction is divided into two stages, wherein the temperature of the first stage is 60-65 ℃, the polymerization is carried out for 25-30 min, and the temperature of the second stage is 165-170 ℃, and the polymerization is carried out for 30-35 min.
9) Washing the ternary positive electrode material obtained in the step 8) with ethanol, filtering, and drying at 120 ℃ to obtain the PEDOT-coated LiNi0.5Co0.2Mn0.3。
The LiNi obtained in the step 5) is subjected to0.5Co0.2Mn0.3Material (labeled as material 1) and PEDOT-coated LiNi obtained in step 9)0.5Co0.2Mn0.3The materials (labeled as material 2) were used as positive active materials to fabricate lithium ion batteries, respectively. Polyvinylidene fluoride (PVDF) is used as a binder on the positive electrode, N-methyl pyrrolidone (NMP) is used as a dispersing agent, artificial graphite is used as the negative electrode, solvents EC, DMC and EMC are used as electrolytes in a mass ratio of 1:1, the concentration of lithium salt of the electrolytes is 1.0M, the batteries with the nominal capacity of 20Ah are manufactured, 1C charge-discharge circulation is carried out within the voltage range of 2.7-4.5V, and the results are shown in the following table 1.
TABLE 1
| Material | First discharge efficiency | Number of cycles | Capacity retention (%) |
| 1 | 87.2 | 300 | 85.1 |
| 2 | 88.9 | 300 | 90.1 |
As can be seen from table 1, the lithium ion battery manufactured by using the ternary cathode material of the present invention has greatly improved first discharge efficiency and cycle performance.
Claims (9)
1. A preparation method of a ternary cathode material with high conductivity is characterized by comprising the following steps: comprises the following steps of 1) preparing a multi-element mixed solution of nickel salt, cobalt salt and manganese salt with a preset proportion,
2) adding the multicomponent mixed solution obtained in the step 1), ammonia water and a sodium hydroxide solution into a reaction device containing a base solution in a concurrent flow manner, and carrying out a coprecipitation reaction to obtain a sodium hydroxide precursor; the whole process is carried out under the protection of inert gas atmosphere;
3) filtering the reaction product obtained in the step 2) to obtain a precipitate, and washing the precipitate with deionized water until the filtrate is neutral;
4) drying in a hot air circulation oven for 10-12h to obtain a ternary material precursor;
5) mixing the ternary precursor of the step 4) with Li2CO3Uniformly mixing and grinding the materials according to the stoichiometric ratio of 2:1.1, and then sintering to obtain an inner core;
6) immersing the kernel in the step 5) into a conductive polymer monomer solution, firstly mechanically stirring for 0.5-10h, and then ultrasonically dispersing for 0.5-72 h;
7) drying the kernel obtained in the step 6) at room temperature to 70 ℃ for 30-360 min;
8) immersing the inner core in the step 7) in an oxidant, wherein the oxidant is one or more of iron p-toluenesulfonate, ammonium persulfate, sodium persulfate, ammonium sulfate and ferric chloride; the concentration of the oxidant solution is 10-70 wt%; carrying out polymerization reaction in a polymerization oven after impregnation with an oxidant, wherein the highest temperature of the reaction is 200 ℃, and the reaction time is 55-65 min;
9) washing the ternary cathode material obtained in the step 8) with ethanol, filtering, and drying at the temperature of 40-120 ℃ to obtain the product.
2. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: the low liquid in the step 2) is a mixed liquid of sodium hydroxide and ammonia water; the concentration of the sodium hydroxide solution in the base solution is 7.5-10mol/L, and the concentration of the ammonia water is 6-8 mol/L.
3. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: in the step 1), the nickel salt is at least one of nickel nitrate, nickel chloride, nickel acetate and nickel sulfate; the manganese salt is at least one of manganese nitrate, manganese chloride, manganese acetate and manganese sulfate; the cobalt salt is at least one of cobalt nitrate, cobalt chloride, cobalt acetate and cobalt sulfate.
4. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: the ion total concentration of the multi-element mixed solution obtained in the step 1) is 1-1.5 mol/L, the concentration of the sodium hydroxide solution flowing in the step 2) is 7.5-10mol/L, and the concentration of the ammonia water flowing in is 6-8 mol/L.
5. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: the feeding speed of the mixed solution in the step 2) is 90-150ml/min, the feeding speed of the sodium hydroxide is 30-70ml/min, and the feeding speed of the ammonia water is 5-40 ml/min.
6. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: the PH value of the coprecipitation reaction in the step 2) is 10-12, the ammonium ion concentration is 5-9g/L, the reaction temperature is 50-60 ℃, and the stirring speed is 200-400 r/min.
7. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: the sintering in the step 5) is carried out in three steps, namely, according to the temperature rise rate of 4 ℃ min-1Heating to 400-; ② then heating up at a rate of 2 ℃ for min-1Heating to 580 ℃ and 600 ℃, and preserving heat for 3 h; thirdly, heating rate is 1 ℃ and min-1Heating to 750 ℃ and 900 ℃ and preserving the temperature for 15h to obtain the product.
8. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: the conductive polymer monomer in the step 6) comprises acetylene, pyrrole, thiophene and derivatives thereof.
9. The method for preparing a ternary positive electrode material with high conductivity according to claim 1, wherein the method comprises the following steps: in the step 8), the polymerization reaction is divided into two stages, wherein the temperature of the first stage is 60-65 ℃, the polymerization is carried out for 25-30 min, and the temperature of the second stage is 165-170 ℃, and the polymerization is carried out for 30-35 min.
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