CN107482210A - A kind of magnesia@nickel cobalt lithium aluminate cathode materials and preparation method and application - Google Patents
A kind of magnesia@nickel cobalt lithium aluminate cathode materials and preparation method and application Download PDFInfo
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- CN107482210A CN107482210A CN201710573390.5A CN201710573390A CN107482210A CN 107482210 A CN107482210 A CN 107482210A CN 201710573390 A CN201710573390 A CN 201710573390A CN 107482210 A CN107482210 A CN 107482210A
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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Abstract
The present invention discloses a kind of magnesia@nickel cobalt lithium aluminate cathode materials and preparation method and application.This method is that nickel salt, cobalt salt, aluminium salt and lithium salts are dissolved in into deionized water, stir under an inert gas, it is 9~13 to instill alkali lye and control solution ph, nickel cobalt lithium aluminate cathode material presoma is made, add sonic oscillation after appropriate magnesium salts mixes and carry out ball milling after uniformly mixing, then gained nickel cobalt lithium aluminate positive pole presoma/magnesium salts composite is calcined at 450 DEG C~900 DEG C, obtains magnesia@nickel cobalt lithium aluminate cathode materials.This method technique is simple, can be sufficiently mixed raw material using high-energy ball milling, and under 2.8V~4.3V, 0.1C, first discharge specific capacity 201.3mAh/g, 0.2C 100 capability retentions of circulation are up to 98%.The problems such as heat endurance that solves nickel cobalt lithium aluminate is poor, poor circulation and storage performance be not good enough.
Description
Technical field
The invention belongs to lithium battery material technical field, more particularly, to a kind of magnesia@nickel cobalts lithium aluminate positive pole material
Material and preparation method and application.
Background technology
Nearly two during the last ten years, and lithium ion battery is because its energy density is high, self discharge degree is low, memory-less effect and environment
It is the advantages that friendly, ripe to be applied to the minitype motivation lithium battery such as 3C electronic products and electric tool, electric automobile market,
It is chemical energy storage power supply most with prospects at present.And core material of the positive electrode as four big material of lithium-ion-power cell
Material, serves critical to the final performance of battery, and the overall performance of lithium ion battery, which optimizes, often to be risen certainly in positive electrode
Technological break-through, therefore develop high performance positive electrode and be imminent.
Nickel cobalt lithium aluminate (NCA) as most well-known, the most ripe positive electrode after nickle cobalt lithium manganate (NCM) it
One, have the following advantages that:Discharge voltage is high, and specific capacity is high, energy density height etc..Unavoidably, although NCA is to be commercialized at present
Middle specific capacity highest positive electrode, but its heat endurance is poor, poor circulation and storage performance be not good enough.
The content of the invention
In order to solve above-mentioned the shortcomings of the prior art, there is provided a kind of magnesia@nickel cobalts lithium aluminate positive pole material
The preparation method of material, this method combination high-energy ball milling method and high temperature solid-state method carry out magnesia cladding to nickel cobalt aluminium positive electrode,
Its advantage is short preparation period, and technique is simple, and powder granule soilless sticking, product electrical property homogeneity are good, are a kind of having for row
The lithium ion tertiary cathode material of effect prepares and method of modifying this method, solve poor NCA heat endurances, poor circulation,
Not the problems such as storage performance is not good enough.
Another object of the present invention is to provide the magnesia@nickel cobalt lithium aluminate cathode materials of above method preparation.The oxygen
Changing magnesium@nickel cobalt lithium aluminate cathode materials has excellent heat endurance, cycle performance and storage performance.
It is still another object of the present invention to provide the application of above-mentioned magnesia@nickel cobalt lithium aluminate cathode materials.
The purpose of the present invention is realized by following technical proposals:
A kind of preparation method of magnesia@nickel cobalt lithium aluminate cathode materials, including step in detail below:
S1. nickel salt, cobalt salt, aluminium salt and lithium salts are dissolved in deionized water, stir wiring solution-forming, under an inert atmosphere
Continuously stir, it is 9~13 that alkali lye, which is added dropwise, and controls the pH value of solution, and nickel cobalt lithium aluminate cathode material presoma is made;
S2. by the nickel cobalt lithium aluminate cathode material presoma that step S1 is obtained and magnesium salts mixing sonic oscillation, after ball milling
Nickel cobalt lithium aluminate positive pole presoma/magnesium salts composite is made;
S3. nickel cobalt lithium aluminate positive pole presoma/magnesium salts composite obtained by step S2 is calcined under an inert atmosphere,
Obtain magnesia@nickel cobalt lithium aluminate composite positive poles.
Preferably, alkali lye described in step S1 is 0.1~10mol/L ammoniacal liquor and 0.1~10mol/L sodium hydrate aqueous solutions
Mixed liquor, the volume ratio of the sodium hydrate aqueous solution and ammoniacal liquor is (1~5):(1~5).
Preferably, the mol ratio of nickel salt described in step S1, cobalt salt, aluminium salt and lithium salts is 80:15:5:(1~1.05), institute
The molal volume ratio of the total moles and deionized water of stating nickel salt, cobalt salt, aluminium salt and lithium salts is 9:(50~500) mol/L.
Preferably, the nickel salt is one or more of nickel acetate or nickel sulfate, and described cobalt salt is cobalt acetate or sulfuric acid
One or more of cobalt, described aluminium salt are one or more of aluminium acetate or aluminum sulfate, and described lithium salts is lithium acetate or sulphur
One or more of sour lithium.
Preferably, inert atmosphere described in step S1 and S3 is nitrogen or argon gas.
Preferably, magnesium salts described in step S2 is one kind in magnesium nitrate, magnesium sulfate, magnesium phosphate, magnesium chloride or magnesium acetate
More than, the mass ratio of the magnesium salts and nickel cobalt lithium aluminate cathode material presoma is (0.03~0.4):1;The rotating speed of the ball milling
For 200~1000rpm, the time of the ball milling is 0.5~10h, and the time of the sonic oscillation is 0.5~10h.
Preferably, the specific procedure calcined described in step S3 is:Heating rate is 3~8 DEG C/min, calcining heat 450
~600 DEG C, 4~10h of soaking time, then 750~900 DEG C are warming up to, 4~10h of soaking time.
A kind of magnesia@nickel cobalt lithium aluminate cathode materials are made by above-mentioned method, the magnesia@nickel cobalt aluminic acids
The chemical molecular formula of lithium anode material is LiβNi1-x-y-αCox+αAlyO2, wherein, 0<X≤0.1,0<Y≤0.05,0<ɑ≤0.05,
0<β≤1.2。
Application of the magnesia@nickel cobalt lithium aluminate cathode materials in field of lithium ion battery material.
Compared with prior art, the invention has the advantages that:
1. the short preparation period of the present invention, technique is simple, and the particle of magnesia@nickel cobalt lithium aluminate cathode materials is without group
It is poly-, product electrical property homogeneity is good.
2. magnesia@nickel cobalt lithium aluminate cathode materials produced by the present invention have cyclical stability, in 2.8V~4.3V,
Under 0.1C, the first discharge specific capacity of battery is 201.3mAh/g.Battery circulates 100 capability retentions in 0.2C and is up to
98%.The problems such as heat endurance that solves nickel cobalt lithium aluminate is poor, poor circulation and storage performance be not good enough.
Brief description of the drawings
Fig. 1 is the first charge and discharge curve map of the magnesia nickel cobalt aluminic acid lithium battery of embodiment 1.
Fig. 2 is the capacity circulating conservation rate of 50 discharge and recharges of the magnesia nickel cobalt aluminic acid lithium battery of embodiment 1.
Embodiment
Present disclosure is further illustrated with reference to specific embodiment, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagent, method and apparatus.
Embodiment 1
1. measure 1mol/L nickel acetates, cobalt acetate, aluminium acetate and lithium acetate 0.8L, 0.15L, 0.05L, 1.2L respectively to mix
Close, stir wiring solution-forming, in continuous stirred tank reactor of the injection full of nitrogen, is then slowly dropped into 0.1mol/L sodium hydroxide
Volume ratio (the V of the aqueous solution and 0.1mol/L ammoniacal liquorNaOH:VNH3·H2O) it is 1:5, it is 11 to control solution ph, obtains kernel material
Expect nickel cobalt lithium aluminate cathode material presoma Li1.2Ni0.8Co0.15Al0.05(OH)2。
2. the nickel cobalt lithium aluminate cathode material presoma that step 1 is obtained and quality are nickel cobalt lithium aluminate cathode material forerunner
The magnesium nitrate that 0.05 times of body is placed in ultrasonator, sonic oscillation 1h, is then moved to and is placed in high energy ball mill, and control ball milling turns
Speed is 300rpm, Ball-milling Time 6h, and nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material is made.
3. step 2 gained nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material is placed in high-temperature calcination stove in nitrogen
Calcined under gas, it is 5 DEG C/min to control heating rate, is warming up to 450 DEG C, soaking time 8h, then is warming up to 800 DEG C, soaking time
4h, room temperature is then annealed to 4 DEG C/min, obtains magnesia@nickel cobalt lithium aluminate composite positive poles, its chemical molecular formula is
Li1.2Ni0.8Co0.15Al0.05O2。
Fig. 1 be the present embodiment magnesia nickel cobalt aluminic acid lithium battery head charge and discharge curve maps, as shown in Figure 1 2.8V~
Under 4.3V, 0.1C, the first discharge specific capacity of battery is 201.3mAh/g.Fig. 2 is magnesia@nickel cobalt aluminium made from the present embodiment
The capacity circulating conservation rate of 50 discharge and recharges of acid lithium battery.As can be known from Fig. 2, battery circulates 100 capacity in 0.2C and kept
Rate is up to 98%, illustrates that it possesses excellent cyclical stability.
Embodiment 2
1. 3mol/L nickel sulfates, cobaltous sulfate, aluminum sulfate and lithium sulfate 0.8L, 0.15L, 0.05L, 1L mixing are measured respectively,
Stir wiring solution-forming, and in continuous stirred tank reactor of the injection full of argon gas, the sodium hydroxide for being then slowly dropped into 10mol/L is water-soluble
Volume ratio (the V of liquid and 10mol/L ammoniacal liquorNaOH:VNH3·H2O) it is 5:1 control solution ph be 12, obtain inner nuclear material nickel cobalt
Lithium aluminate cathode material presoma LiNi0.8Co0.15Al0.05(OH)2。
2. the nickel cobalt lithium aluminate cathode material presoma that step 1 is obtained and quality are nickel cobalt lithium aluminate cathode material forerunner
The magnesium nitrate that 0.1 times of body is placed in ultrasonator, sonic oscillation 2h, is then moved in high energy ball mill, controls the rotational speed of ball-mill to be
400rpm, Ball-milling Time 12h, nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material is made.
3. step 2 gained nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material is placed in high-temperature calcination stove in argon
Calcined under gas, it is 3 DEG C/min to control heating rate, is warming up to 500 DEG C, soaking time 4h, then is warming up to 750 DEG C, soaking time
8h, room temperature is then annealed to 6 DEG C/min, obtains magnesia@nickel cobalt lithium aluminate composite positive poles, its chemical molecular formula is
LiNi0.8Co0.15Al0.05O2。
Embodiment 3
1. measure 5mol/L nickel acetates, cobaltous sulfate, aluminium acetate and lithium sulfate 0.8L, 0.15L, 0.05L, 1.2L respectively to mix
Close, stir, wiring solution-forming, injection is full of in the continuous stirred tank reactor of nitrogen, is then slowly dropped into 0.1mol/L hydroxide
Volume ratio (the V of sodium water solution and 5mol/L ammoniacal liquorNaOH:VNH3·H2O) it is 3:1 control solution ph be 13, obtain inner nuclear material
Nickel cobalt lithium aluminate cathode material presoma Li1.2Ni0.8Co0.15Al0.05(OH)2。
2. the nickel cobalt lithium aluminate cathode material presoma that step 1 is obtained and quality are nickel cobalt lithium aluminate cathode material forerunner
The magnesium nitrate that 0.2 times of body is placed in ultrasonator, sonic oscillation 1h, is placed in high energy ball mill, controls the rotational speed of ball-mill to be
600rpm, Ball-milling Time 18h, nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material is made.
3. nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material that step 2 obtains is placed in high-temperature calcination stove in nitrogen
Calcined in gas, it is 5 DEG C/min to control heating rate, is warming up to 550 DEG C, soaking time 8h, then is warming up to 900 DEG C, soaking time
10h, room temperature is then annealed to 8 DEG C/min, obtains magnesia@nickel cobalt lithium aluminate composite positive poles, its chemical molecular formula is
Li1.2Ni0.8Co0.15Al0.05O2。
Embodiment 4
1. measure 7mol/L nickel sulfates, cobalt acetate, aluminum sulfate and lithium acetate 0.85L, 0.1L, 0.05L, 1.2L respectively to mix
Close, stir wiring solution-forming, in continuous stirred tank reactor of the injection full of argon gas, is then slowly dropped into 10mol/L sodium hydroxide
Volume ratio (the V of the aqueous solution and 0.1mol/L ammoniacal liquorNaOH:VNH3·H2O) it is 1:5 control solution ph be 12, obtain inner nuclear material
Nickel cobalt lithium aluminate positive pole material drives body Li1.2Ni0.85Co0.1Al0.05(OH)2。
2. the nickel cobalt lithium aluminate cathode material presoma that step 1 is obtained and quality are nickel cobalt lithium aluminate cathode material forerunner
The magnesium nitrate that 0.3 times of body is placed in ultrasonator, sonic oscillation 2h, is placed in high energy ball mill, controls the rotational speed of ball-mill to be
800rpm, Ball-milling Time 6h, obtain nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material.
3. nickel cobalt lithium aluminate positive pole presoma/nitric acid magnesium base composite material that step 2 obtains is placed in high-temperature calcination stove in argon
Calcined in gas, it is 8 DEG C/min to control heating rate, is warming up to 600 DEG C, soaking time 10h, then is warming up to 850 DEG C, soaking time
4h, room temperature is then annealed to 5 DEG C/min, obtains magnesia@nickel cobalt lithium aluminate composite positive poles, its chemical molecular formula is
Li1.2Ni0.85Co0.1Al0.05O2。
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine and simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of magnesia@nickel cobalt lithium aluminate cathode materials, it is characterised in that including step in detail below:
S1. nickel salt, cobalt salt, aluminium salt and lithium salts are dissolved in deionized water, stir wiring solution-forming, under an inert atmosphere continuously
Stirring, it is 9~13 that alkali lye, which is added dropwise, and controls the pH value of solution, and nickel cobalt lithium aluminate cathode material presoma is made;
S2. by the nickel cobalt lithium aluminate cathode material presoma that step S1 is obtained and magnesium salts mixing sonic oscillation, it is made after ball milling
Nickel cobalt lithium aluminate positive pole presoma/magnesium salts composite;
S3. nickel cobalt lithium aluminate positive pole presoma/magnesium salts composite obtained by step S2 is calcined under an inert atmosphere, obtained
Magnesia@nickel cobalt lithium aluminate composite positive poles.
2. the preparation method of magnesia@nickel cobalts lithium aluminate cathode material according to claim 1, it is characterised in that step S1
Described in alkali lye be 0.1~10mol/L ammoniacal liquor and 0.1~10mol/L sodium hydrate aqueous solutions mixed liquor, the sodium hydroxide
The volume ratio of the aqueous solution and ammoniacal liquor is (1~5):(1~5).
3. the preparation method of magnesia@nickel cobalts lithium aluminate cathode material according to claim 1, it is characterised in that step S1
Described in nickel salt, cobalt salt, the mol ratio of aluminium salt and lithium salts be 80:15:5:(1~1.05), the nickel salt, cobalt salt, aluminium salt and lithium
The total moles of salt and the molal volume ratio of deionized water are 9:(50~500) mol/L.
4. the preparation method of magnesia@nickel cobalts lithium aluminate cathode material according to claim 3, it is characterised in that the nickel
Salt is one or more of nickel acetate or nickel sulfate, and described cobalt salt is one or more of cobalt acetate or cobaltous sulfate, described
Aluminium salt is one or more of aluminium acetate or aluminum sulfate, and described lithium salts is one or more of lithium acetate or lithium sulfate.
5. the preparation method of magnesia@nickel cobalts lithium aluminate cathode material according to claim 1, it is characterised in that step S1
It is nitrogen or argon gas with inert atmosphere described in S3.
6. the preparation method of magnesia@nickel cobalts lithium aluminate cathode material according to claim 1, it is characterised in that step S2
Described in magnesium salts be one or more of magnesium nitrate, magnesium sulfate, magnesium phosphate, magnesium chloride or magnesium acetate, the magnesium salts and nickel cobalt aluminium
The mass ratio of sour lithium anode material presoma is (0.03~0.4):1;The rotating speed of the ball milling is 200~1000rpm, the ball
The time of mill is 0.5~10h, and the time of the sonic oscillation is 0.5~10h.
7. the preparation method of magnesia@nickel cobalts lithium aluminate cathode material according to claim 1, it is characterised in that step S3
Described in the specific procedure calcined be:Heating rate is 3~8 DEG C/min, 450~600 DEG C of calcining heat, soaking time 4~
10h, then 750~900 DEG C are warming up to, 4~10h of soaking time.
A kind of 8. magnesia@nickel cobalt lithium aluminate cathode materials, it is characterised in that the magnesia@nickel cobalt lithium aluminate cathode materials
It is to be made by the method described in claim any one of 1-7.
9. magnesia@nickel cobalt lithium aluminate cathode materials according to claim 8, it is characterised in that the magnesia@nickel cobalts
The chemical molecular formula of lithium aluminate cathode material is LiβNi1-x-y-αCox+αAlyO2, wherein, 0<X≤0.1,0<Y≤0.05,0<ɑ≤
0.05,0<β≤1.2.
10. application of the magnesia@nickel cobalt lithium aluminate cathode materials of claim 8 or 9 in field of lithium ion battery material.
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CN110364710A (en) * | 2019-07-02 | 2019-10-22 | 华南理工大学 | High-performance manganese-based zinc ion battery positive electrode material and preparation method and application thereof |
CN112079399A (en) * | 2020-09-07 | 2020-12-15 | 隆能科技(南通)有限公司 | Preparation method of low-cost high-performance nickel-cobalt lithium aluminate composite cathode material |
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CN108574100B (en) * | 2018-03-23 | 2022-03-15 | 深圳市德方纳米科技股份有限公司 | Ternary cathode material, preparation method and lithium ion battery |
CN109167051A (en) * | 2018-09-30 | 2019-01-08 | 东莞市三臻科技发展有限公司 | A kind of ternary material and high-capacity battery of nickelic system |
CN110364710A (en) * | 2019-07-02 | 2019-10-22 | 华南理工大学 | High-performance manganese-based zinc ion battery positive electrode material and preparation method and application thereof |
CN112079399A (en) * | 2020-09-07 | 2020-12-15 | 隆能科技(南通)有限公司 | Preparation method of low-cost high-performance nickel-cobalt lithium aluminate composite cathode material |
CN112079399B (en) * | 2020-09-07 | 2023-08-22 | 隆能科技(南通)有限公司 | Preparation method of low-cost high-performance nickel cobalt lithium aluminate composite positive electrode material |
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Application publication date: 20171215 |
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