CN110182857B - High-activity petal-shaped nickel-cobalt-manganese ternary precursor and preparation method thereof - Google Patents
High-activity petal-shaped nickel-cobalt-manganese ternary precursor and preparation method thereof Download PDFInfo
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Abstract
A high-activity petal-shaped nickel-cobalt-manganese ternary precursor and a preparation method thereof are disclosed, wherein the chemical general formula of the nickel-cobalt-manganese ternary precursor is as follows: niaCobMnc(OH)2, wherein a + b + c =1, and 0.33. ltoreq. a.ltoreq.0.9, 0.05. ltoreq. b.ltoreq.0.33, 0.05. ltoreq. c.ltoreq.0.33,the specific surface area of the nickel-cobalt-manganese ternary precursor is 20-30m2Per g, and is petal-shaped; the invention also discloses a preparation method of the high-activity petal-shaped nickel-cobalt-manganese ternary precursor. The high-activity petal-shaped ternary precursor is petal-shaped, has a large specific surface area and is high in activity; the process is simple and convenient to operate, and the requirements on production equipment are not high.
Description
Technical Field
The invention relates to the technical field of manufacturing of nickel-cobalt-manganese ternary precursors, and particularly relates to a high-activity petal-shaped nickel-cobalt-manganese ternary precursor and a preparation method thereof.
Background
Lithium ion batteries were first commercialized in japan, and their use is also expanded from the 3C field to the fields of energy storage, power, and the like. The requirements of people on energy density, safety performance, use cost and cycle performance of power batteries are continuously improved. The positive electrode material is one of the key materials for manufacturing the lithium ion battery, and determines the energy density, the safety performance, the use cost, the cycle performance and the like of a battery core.
The lithium ion battery anode materials which are successfully industrialized at present comprise a layered ternary anode material, a spinel lithium manganate anode material and an olivine lithium iron phosphate anode material. Due to the defects of lithium iron phosphate and lithium manganate in energy density, the current ternary cathode material becomes the mainstream in the market.
The industrial synthesis of the ternary material mainly comprises a high-temperature solid phase method: the ternary precursor and lithium carbonate or lithium hydroxide are uniformly mixed and sintered, and the performance of the ternary precursor determines the performance of the ternary cathode material to a certain extent, so that the ternary precursor with excellent performance index must be prepared in order to prepare the ternary material with excellent performance; at present, the preparation process of hydroxide coprecipitation is generally adopted in industrialization, the preparation process is complex to operate and has high requirements on production equipment, and the prepared spherical ternary precursor is uneven in doping, smaller in specific surface area and lower in activity.
Disclosure of Invention
The invention aims to solve the technical problems that the defects in the prior art are overcome, and the high-activity petal-shaped nickel-cobalt-manganese ternary precursor and the preparation method thereof are provided, wherein the particle shape of the ternary precursor is petal-shaped, and the ternary precursor has a large specific surface area and high activity; the preparation process is simple and convenient to operate, and has low requirements on production equipment.
The technical scheme adopted by the invention for solving the technical problems is as follows: a high-activity petal nickel-cobalt-manganese ternary precursor has a chemical general formula as follows: niaCobMnc(OH)2, wherein a + b + c =1, and 0.33. ltoreq. a.ltoreq.0.9, 0.05. ltoreq. b.ltoreq.0.33, 0.05. ltoreq. c.ltoreq.0.33, the specific surface area of the nickel-cobalt-manganese ternary precursor being 20 to 30m2(ii)/g, and the shape of the particles is petal-shaped.
The preparation method of the high-activity petal-shaped nickel-cobalt-manganese ternary precursor comprises the following steps of: preparing a nickel-cobalt-manganese soluble salt aqueous solution, an ammonia aqueous solution, an alkali liquor and a reaction base solution; (2) adding a metal salt aqueous solution to the nickel-cobalt-manganese soluble salt aqueous solution to obtain a doped aqueous solution; (3) adding reaction bottom liquid into the reaction kettle, starting stirring, introducing inert gas, and then introducing the doped aqueous solution, the ammonia water solution and the alkali liquor by using a precise metering pump to react; (4) continuously stirring, and opening an overflow valve when the liquid level in the reaction kettle rises to be close to the cover of the reaction kettle, so that the reaction liquid flows into the aging kettle for aging; and (5) carrying out solid-liquid separation on the aged product, washing the obtained solid material, and then drying and sieving to obtain the petal-shaped nickel-cobalt-manganese ternary precursor doped with the metal elements.
Further, in the step (1), the concentration of the nickel-cobalt-manganese soluble salt aqueous solution is 1.0-3.5 mol/L, the concentration of the ammonia aqueous solution is 8-12 mol/L, the concentration of the alkali liquor is 5-13 mol/L, and the reaction bottom liquid is prepared from ammonia water, soluble ammonium salt and alkali liquor.
Further, in the step (1), the nickel-cobalt-manganese soluble salt aqueous solution is an aqueous solution of nickel salt, cobalt salt and manganese salt, wherein the molar ratio of nickel to cobalt to manganese is 1:1:1 to 9:0.5: 0.5.
Further, in the step (1), the reaction base solution is prepared from a soluble ammonium salt aqueous solution, ammonia water and alkali liquor, the ammonia concentration of the reaction base solution is 0.4 mol/L, the pH value is in the range of 11.2-11.5, and the ratio of the ammonia water to the soluble ammonium salt is 3: 1.
The preparation method of the reaction kettle bottom liquid comprises the steps of firstly preparing a soluble ammonium salt aqueous solution, then adding 12 mol/L ammonia water into the prepared soluble ammonium salt according to a proportion, and finally adding a proper amount of water and alkali liquor to ensure that the ammonia concentration of the bottom liquid is 0.4 mol/L and the pH value is within the range of 11.2-11.5, wherein the proportion of the ammonia water to the soluble ammonium salt is 3: 1.)
Further, in the step (1), the soluble ammonium salt is two or more of ammonium sulfate, ammonium carbonate, ammonium chloride, ammonium tartrate, ammonium oxalate and ammonium citrate, and the alkali liquor is an aqueous solution of sodium hydroxide.
Further, in the step (2), the aqueous solution of the metal salt is an aqueous solution of one or more sulfate salts of aluminum, magnesium, zirconium, titanium, yttrium, tungsten, molybdenum, calcium, niobium, lanthanum, indium, strontium and tantalum.
Further, in the step (3), the addition amount of the reaction bottom solution is 1/4-3/4 of the volume of the reaction kettle, and the usage amount of the metal salt aqueous solution is not more than 1% of the total amount of the nickel-cobalt-manganese soluble salt aqueous solution.
Further, in the step (3), the stirring speed is 300-700r/min, the reaction temperature is 50-65 ℃, the ammonia concentration is maintained to be 0.4-1.0 mol/L, and the pH value is 10.5-12.5.
Further, in the step (4), the reaction liquid overflowing in the first 20h is discharged as a defective product, the stirring speed of the aging kettle is adjusted to 150rpm, and the aging time is kept for 8h-10 h.
Further, in the step (5), filtering the aged product by using a filter, washing by using an alkali liquor, continuously washing by using deionized water until the pH value of the final washing water is 7-8, and finishing washing; the washed precipitate was dried at a temperature of 150 + -10 deg.C.
The invention has the beneficial effects that: 1) the nickel-cobalt-manganese ternary precursor has large specific surface area and high activity, and can be used for preparing a large single crystal ternary cathode material; 2) the preparation method is simple and convenient to operate, has low requirements on production equipment, and can selectively regulate and control the primary particle arrangement of the precursor by selectively regulating parameters such as the reaction bottom liquid amount, the reaction bottom liquid components, the addition amount of reactants, the addition speed, the stirring strength of a reaction kettle and the like in the coprecipitation reaction process; 3) through liquid phase doping, uniform precipitation of doping elements can be realized, the stability and the conductivity of a ternary material lattice prepared in the later stage are improved, the cycle performance of the anode material is improved, and the condition that the dry method doping is not uniform and the electrical property is poor is avoided.
Drawings
FIG. 1 is a schematic diagram of a Ni-Co-Mn ternary precursor of example 1 under a 5000-fold electron microscope;
FIG. 2 is a shape diagram of the Ni-Co-Mn ternary precursor of embodiment 1 under an electron microscope of 10000 times;
fig. 3 is an electron microscope topography of a nickel-cobalt-manganese ternary positive electrode material prepared by using the nickel-cobalt-manganese ternary precursor of embodiment 1 of the present invention;
fig. 4 is an electrical property diagram of the nickel-cobalt-manganese ternary positive electrode material prepared by using the nickel-cobalt-manganese ternary precursor in embodiment 1 of the present invention.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention:
the high-activity petal-shaped nickel-cobalt-manganese ternary precursor provided by the embodiment 1 of the invention has a chemical general formula as follows: niaCobMnc(OH)2, wherein a + b + c =1, and 0.33. ltoreq. a.ltoreq.0.9, 0.05. ltoreq. b.ltoreq.0.33, 0.05. ltoreq. c.ltoreq.0.33, the specific surface area of the ternary precursor being from 20 to 30m2(ii)/g; the particle morphology is shown in fig. 1 and fig. 2, and the particle shape is petal-shaped.
The preparation method of the high-activity petal-shaped ternary precursor disclosed by the invention, in the embodiment 1, comprises the following steps of:
(1) preparing 2 mol/L of nickel-cobalt-manganese soluble salt aqueous solution, 11 mol/L of sodium hydroxide solution, 12 mol/L of ammonia aqueous solution and reaction base solution with the pH value of 11.2 and the ammonia concentration of 0.4 mol/L of sodium hydroxide, ammonia aqueous solution and ammonium sulfate according to the mol ratio of Ni to Co to Mn =6 to 2, wherein the use amounts of the ammonia aqueous solution and the ammonium sulfate in the base solution are 3: 1;
(2) adding a metal salt aqueous solution into the nickel-cobalt-manganese soluble salt aqueous solution to obtain a doped aqueous solution, wherein the metal salt aqueous solution is a mixed solution of zirconium sulfate and titanium sulfate with the concentration of 0.8 g/L;
(3) adding 1/4 reaction base solution with the volume of the reaction kettle into the reaction kettle, starting stirring at the stirring speed of 700rpm, keeping the temperature at 55 ℃, introducing inert gas, and introducing the doped aqueous solution, the ammonia aqueous solution and the alkali liquor by using a precise metering pump to react, wherein the temperature of the reaction kettle system is kept at 54 +/-2 ℃, the pH value is 11.1 +/-0.1, and the ammonia concentration is 0.5 +/-0.1 mol/L during the reaction;
(4) continuously stirring, opening an overflow valve when the liquid level in the reaction kettle rises to be close to the cover of the reaction kettle, allowing the reaction liquid to flow into an aging kettle for aging, adjusting the stirring speed to 150rpm in the aging process, and keeping the aging time for 8 hours;
(5) performing solid-liquid separation on the aged product, washing the obtained solid material, drying and sieving to obtain the product with the specific surface area of 20-25m2The shape of the petal-shaped zirconium and titanium doped nickel-cobalt-manganese ternary precursor is shown in figures 1 and 2.
Weighing 5g of the nickel-cobalt-manganese ternary precursor and 2.3g of lithium hydroxide monohydrate, putting the mixture into a ball mill for mixing, carrying out ball milling for 20 hours by the ball mill to ensure that the nickel-cobalt-manganese ternary precursor and the lithium hydroxide monohydrate are fully and uniformly mixed, and putting the mixture into a tube furnace for sintering after uniform mixing; then in a tubular furnace, firstly performing heat treatment at 450 ℃ for 3h, then performing heat treatment at 700 ℃ for 5h, and finally performing heat treatment at 900-930 ℃ for 12h, keeping an oxygen atmosphere in the whole process, dissociating and screening the obtained product to finally obtain the zirconium-titanium co-doped ternary cathode material, wherein the morphology is shown in FIG. 3, and the measured electrical property is shown in FIG. 4: in the voltage range of 3.0-4.3V, the discharge capacity of the obtained ternary cathode material 1C is up to 163.2mAh/g, and after 50 cycles, the capacity retention rate is up to 97.3%.
The preparation method of the high-activity petal-shaped nickel-cobalt-manganese ternary precursor disclosed by the invention, in the embodiment 2, comprises the following steps of:
(1) preparing 2 mol/L of a nickel-cobalt-manganese soluble salt aqueous solution, 11 mol/L of a sodium hydroxide solution, 12 mol/L of an ammonia aqueous solution according to a molar ratio of Ni to Co to Mn =65 to 15 to 20, and preparing a reaction base solution with a pH value of 11.2 and an ammonia concentration of 0.4 mol/L of sodium hydroxide, ammonia and ammonium sulfate, wherein the use amounts of the ammonia water and the ammonium sulfate in the base solution are 3: 1;
(2) adding a metal salt aqueous solution into the nickel-cobalt-manganese soluble salt aqueous solution to obtain a doped aqueous solution, wherein the metal salt aqueous solution is a mixed solution of zirconium sulfate and aluminum sulfate with the concentration of 0.8 g/L;
(3) adding 1/2 reaction base solution with the volume of the reaction kettle into the reaction kettle, then starting stirring at the stirring speed of 600rpm, keeping the temperature at 60 ℃, introducing inert gas, and then introducing the doped aqueous solution, the ammonia aqueous solution and the alkali liquor by using a precise metering pump to react, wherein the temperature of the reaction kettle system is kept at 57-63 ℃, the pH value is 11.1-11.5, and the ammonia concentration is 0.4-0.6 mol/L during the reaction;
(4) continuously stirring, opening an overflow valve when the liquid level in the reaction kettle rises to be close to the cover of the reaction kettle, allowing the reaction liquid to flow into an aging kettle for aging, adjusting the stirring speed to 150rpm in the aging process, and keeping the aging time for 8 hours;
(5) performing solid-liquid separation on the aged substance, washing the obtained solid material, drying and sieving to obtain the product with the specific surface area of 20-25m2The nickel-cobalt-manganese ternary precursor is characterized by comprising a petal-shaped zirconium and aluminum doped nickel-cobalt-manganese ternary precursor.
Weighing 5g of the nickel-cobalt-manganese ternary precursor and 2.3g of lithium hydroxide monohydrate, putting the mixture into a ball mill for mixing, carrying out ball milling for 20 hours by the ball mill to ensure that the nickel-cobalt-manganese ternary precursor and the lithium hydroxide monohydrate are fully and uniformly mixed, and putting the mixture into a tube furnace for sintering after uniform mixing; and then carrying out heat treatment for 3h at 450 ℃, then carrying out heat treatment for 5h at 700 ℃ and finally carrying out heat treatment for 12h at 930 ℃ in a tubular furnace, keeping the oxygen atmosphere in the whole process, dissociating and screening the obtained product, and finally obtaining the zirconium-aluminum co-doped ternary cathode material. The electrical properties were measured as follows: in the voltage range of 3.0-4.3V, the discharge capacity of the obtained ternary cathode material 1C is as high as 168.5mAh/g, and after 50 cycles, the capacity retention rate is as high as 97.25%.
The preparation method of the high-activity petal-shaped ternary precursor disclosed by the invention, in the embodiment 3, comprises the following steps of:
(1) preparing 2 mol/L of nickel-cobalt-manganese soluble salt aqueous solution, 11 mol/L of sodium hydroxide solution, 12 mol/L of ammonia aqueous solution and sodium hydroxide, ammonia aqueous solution and ammonium sulfate into reaction base solution with the pH value of 11.5 and the ammonia concentration of 0.4 mol/L according to the mol ratio of Ni to Co to Mn =83 to 11 to 6, wherein the use amounts of the ammonia aqueous solution and the ammonium sulfate in the base solution are 3: 1;
(2) adding a metal salt aqueous solution into the nickel-cobalt-manganese soluble salt aqueous solution to obtain a doped aqueous solution, wherein the metal salt aqueous solution is a mixed solution of zirconium sulfate and titanium sulfate with the concentration of 0.8 g/L;
(3) adding 1/4 reaction base solution with the volume of the reaction kettle into the reaction kettle, then starting stirring at the stirring speed of 500rpm, keeping the temperature at 60 ℃, introducing inert gas, and then introducing the doped aqueous solution, the ammonia aqueous solution and the alkali liquor by using a precise metering pump to react, wherein the temperature of the reaction kettle system is kept at 60 +/-2 ℃, the pH value is 12 +/-0.3, and the ammonia concentration is 0.8 +/-0.1 mol/L during the reaction;
(4) continuously stirring, opening an overflow valve when the liquid level in the reaction kettle rises to be close to the cover of the reaction kettle, allowing the reaction liquid to flow into an aging kettle for aging, adjusting the stirring speed to 150rpm in the aging process, and keeping the aging time for 8 hours;
(5) performing solid-liquid separation on the aged substance, washing the obtained solid material, drying and sieving to obtain the product with the specific surface area of 20-30m2The petal-shaped nickel-cobalt-manganese ternary precursor doped with zirconium and titanium.
Weighing 5g of the nickel-cobalt-manganese ternary precursor and 2.3g of lithium hydroxide monohydrate, putting the mixture into a ball mill for mixing, carrying out ball milling for 20 hours by the ball mill to ensure that the nickel-cobalt-manganese ternary precursor and the lithium hydroxide monohydrate are fully and uniformly mixed, and putting the mixture into a tube furnace for sintering after uniform mixing; and then carrying out heat treatment for 3h at 450 ℃, then carrying out heat treatment for 5h at 700 ℃ and finally carrying out heat treatment for 12h at 900-930 ℃ in a tubular furnace, keeping the oxygen atmosphere in the whole process, dissociating and screening the obtained product, and finally obtaining the zirconium and titanium co-doped nickel-cobalt-manganese ternary cathode material. The electrical properties were measured as follows: in the voltage range of 3.0-4.3V, the discharge capacity of the obtained ternary cathode material 1C is up to 178.51mAh/g, and after 50 cycles, the capacity retention rate is up to 96.56%.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as being within the protection scope of the present invention.
Claims (8)
1. A preparation method of a high-activity petal-shaped nickel-cobalt-manganese ternary precursor doped with metal elements is characterized by comprising the following steps:
(1) preparing a nickel-cobalt-manganese soluble salt aqueous solution, an ammonia aqueous solution, an alkali liquor and a reaction base solution;
(2) adding a metal salt aqueous solution into the nickel-cobalt-manganese soluble salt aqueous solution to obtain a doped aqueous solution;
(3) adding reaction base liquid into the reaction kettle, starting stirring, introducing inert gas, and then introducing the doped aqueous solution, the ammonia water solution and the alkali liquor by using a precise metering pump to react;
(4) continuously stirring, and opening an overflow valve when the liquid level in the reaction kettle rises to be close to the cover of the reaction kettle, so that the reaction liquid flows into the aging kettle for aging;
(5) carrying out solid-liquid separation on the aged product, washing the obtained solid material, and then drying and sieving to obtain a petal-shaped nickel-cobalt-manganese ternary precursor doped with metal elements;
in the step (1), the reaction bottom liquid is prepared from an ammonia water solution, a soluble ammonium salt and an alkali liquor;
in the step (1), the nickel-cobalt-manganese soluble salt aqueous solution is an aqueous solution of nickel salt, cobalt salt and manganese salt, wherein the molar ratio of nickel to cobalt to manganese is 1:1:1 to 9:0.5: 0.5;
in the step (2), the metal salt aqueous solution is one or more sulfate aqueous solutions of aluminum, magnesium, zirconium, titanium, yttrium, tungsten, molybdenum, calcium, niobium, lanthanum, indium, strontium and tantalum;
in the step (3), the addition amount of the reaction bottom liquid is 1/4-3/4 of the volume of the reaction kettle, and the usage amount of the metal salt aqueous solution is not more than 1% of the total amount of the nickel-cobalt-manganese soluble salt aqueous solution;
in the step (3), the stirring speed is 300-700r/min, the reaction temperature is 50-65 ℃, the ammonia concentration is maintained to be 0.4-1.0 mol/L, and the pH = 10.5-12.5;
the alkali liquor is sodium hydroxide aqueous solution; the specific surface area of the obtained ternary precursor is 20-30m2(ii)/g, and the shape of the particles is petal-shaped.
2. The method for preparing the high-activity petal-shaped metallic element doped nickel-cobalt-manganese ternary precursor as claimed in claim 1, wherein in the step (1), the concentration of the nickel-cobalt-manganese soluble salt aqueous solution is 1.0-3.5 mol/L, the concentration of the ammonia aqueous solution is 8-12 mol/L, and the concentration of the alkali liquor is 5-13 mol/L.
3. The method for preparing the petal-shaped high-activity ternary precursor of nickel, cobalt and manganese doped with metal elements according to claim 1 or 2, wherein the soluble ammonium salt is two or more of ammonium sulfate, ammonium carbonate, ammonium chloride, ammonium tartrate, ammonium oxalate and ammonium citrate.
4. The method for preparing the petal-shaped metallic element doped nickel-cobalt-manganese ternary precursor as claimed in claim 1 or 2, wherein in step (4), the reaction solution overflowing in the first 20h is discharged as a rejected product, the stirring speed of the aging kettle is adjusted to 150rpm, and the aging time is kept for 8h-10 h.
5. The method for preparing the high-activity petal-shaped metallic element doped nickel-cobalt-manganese ternary precursor as claimed in claim 3, wherein in the step (4), the reaction solution overflowing in the first 20h is discharged as a rejected product, the stirring speed of the aging kettle is adjusted to 150rpm, and the aging time is kept for 8h-10 h.
6. The method for preparing the high-activity petal-shaped metallic element doped nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein in the step (5), the aged product is filtered by a filter, washed by alkali liquor and then by deionized water until the pH value of the final washing water is 7-8, and the washing is finished; the washed precipitate was dried at a temperature of 150 + -10 deg.C.
7. The method for preparing the high-activity petal-shaped metallic element doped nickel-cobalt-manganese ternary precursor as claimed in claim 3, wherein in the step (5), the aging product is filtered by a filter, washed by alkaline solution and then by deionized water until the final pH value of the washing water is 7-8, and the washing is finished; the washed precipitate was dried at a temperature of 150 + -10 deg.C.
8. The method for preparing the high-activity petal-shaped metallic element doped nickel-cobalt-manganese ternary precursor according to claim 4, wherein in the step (5), the aged product is filtered by a filter, washed by alkaline solution and then by deionized water until the pH value of the final washing water is 7-8, and the washing is finished; the washed precipitate was dried at a temperature of 150 + -10 deg.C.
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