CN104868122A - Preparation method of single-crystal Li(NiCoMn)O2 ternary cathode material - Google Patents
Preparation method of single-crystal Li(NiCoMn)O2 ternary cathode material Download PDFInfo
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Abstract
The invention relates to a preparation method of a single-crystal Li(NiCoMn)O2 ternary cathode material, and belongs to the technical field of a manufacturing process for chemical electrode materials. The preparation method comprises the following steps: firstly, nickel salt, cobalt salt and manganese salt are dissolved in a deionized water and ethylene glycol mixed solution, the mixture is uniformly stirred, a surfactant is added, the mixed solution is clarified, a precipitant is added, the mixture is uniformly stirred and poured into a reactor, the reactor is arranged in a drying oven for a reaction, and then an obtained precursor and lithium salt are mixed, presintered and calcined to obtain a target product. The preparation method is simple and convenient to operate, the controllability of preparation parameters is high, the prepared ternary cathode material is a single-crystal material, particle sizes are concentrated at the submicron dimension, a fast conveying channel with the short path is provided for lithium ions, and contact of the material with an electrolyte is increased. The ternary cathode material has high specific capacity, high rate capability and high cycling stability, and meets the requirements of electronic products with high volume energy density.
Description
Technical field
The present invention relates to a kind of preparation method of monocrystalline nickle cobalt lithium manganate tertiary cathode material, belong to chemical industry electrode material manufacturing process technology field.
Background technology
Along with the continuous progress of society, the scarcity of ecological deterioration and fossil type non-renewable resources, the demand of people to new forms of energy is more and more urgent instantly.As a kind of lithium ion battery of green energy resource, since the beginning of the nineties in last century successfully develops, just high with its specific energy, operating voltage is high, temperature limit is wide, self-discharge rate is low, have extended cycle life, the unique advantage such as pollution-free and receiving much attention, extensive use in the small-sized portable electronic products such as mobile phone, digital camera, notebook computer, and become one of topmost candidate's electrical source of power of electric automobile gradually.Along with the increasingly serious of environmental problem and to while the high-technicalization of military equipment, miniature requirement, have higher requirement to the energy density of lithium ion battery, security reliability and cycle life, be wherein the emphasis of research as the exploitation of the function admirable positive electrode of one of the key factor improving performance of lithium ion battery always.
Current commercial anode material for lithium-ion batteries is mainly cobalt acid lithium, LiFePO 4 and nickle cobalt lithium manganate etc.Wherein, cobalt acid lithium is commercial anode material for lithium-ion batteries the earliest, but cobalt price is higher, also produces harmful effect to environment, and its fail safe in electric automobile and large-scale redundant electrical power need to improve.Owing to self there is the defects such as electronic conductivity is low, lithium ion diffusion velocity is slow, volume energy density is little in LiFePO 4, and its theoretical capacity is lower, limits its application on high specific energy lithium ion battery.Nickle cobalt lithium manganate tertiary cathode material, owing to combining the advantage of cobalt acid lithium, LiMn2O4 and lithium nickelate three, presents good chemical property, has high specific capacity and cycle performance, reduce the cost of material simultaneously, day by day receive the concern of people.But it is being applied to room for promotion very large in addition in high energy lithium ion cell.
Current hydrothermal synthesis method has been widely used in the synthesis preparation of lithium ion battery plus-negative plate material, and it has, and particle purity is high, good dispersion, crystal formation are good and can control, the features such as production cost is low.Old build (201410512794.X) discloses employing water heat transfer LiNi
xco
ymn
zo
2positive electrode, under this material charge-discharge performance 0.5C, specific discharge capacity is up to 177.3mAh/g, but the resorcinol used in the method and formaldehyde poisonous, there is excitant, and under 10C, specific discharge capacity only has 141.7mAh/g.
Summary of the invention
The object of the invention is the nickle cobalt lithium manganate tertiary cathode material cannot producing monocrystalline primary particle in order to solve prior art, a kind of preparation method of monocrystalline nickle cobalt lithium manganate tertiary cathode material is provided.The feature that the method has universality, process is easy to control.
The object of the invention is to be achieved through the following technical solutions.
The preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material of the present invention, concrete steps are:
Step one, divalent nickel salt, divalent cobalt and manganous salt are dissolved in glycol water; The mol ratio of divalent nickel salt, divalent cobalt and manganous salt is a:b:c; Add surfactant after divalent nickel salt, divalent cobalt and manganous salt dissolve completely, the mol ratio of surfactant and divalent nickel salt, divalent cobalt and manganous salt mixture is (0.01 ~ 0.8): 1; After surfactant dissolves completely, add precipitation reagent, the mol ratio of precipitation reagent and divalent nickel salt, divalent cobalt and manganous salt mixture is (1 ~ 1.15): 1; Mixture is obtained after stirring;
Step 2, be transferred in reactor by step one gained mixture, sealing is placed in air dry oven reacts; After reaction terminates, take out reactor and be cooled to room temperature, after centrifugal, drying, obtain presoma;
Step 3, by pre-burning in air atmosphere after step 2 gained precursor and lithium salts Homogeneous phase mixing, the mol ratio of described lithium salts and divalent nickel salt, divalent cobalt and manganous salt mixture is (1 ~ 1.15): 1; The temperature of pre-burning is 400 ~ 480 DEG C, and the time of pre-burning is 3 ~ 10h; Be cooled to room temperature after pre-burning, obtain oxide; High temperature sintering under oxygen atmosphere again, oxide, from room temperature to 500 DEG C, sinters 3 ~ 10h at this temperature, and heating rate is 1 ~ 10 DEG C/min; And then be warming up to 700 DEG C, sinter 3 ~ 10h at this temperature, heating rate is 1 ~ 10 DEG C/min; Finally be warming up to 750 DEG C ~ 950 DEG C again, sinter 8 ~ 24h at this temperature, heating rate is 1 ~ 10 DEG C/min; Be down to room temperature, obtain monocrystalline nickle cobalt lithium manganate tertiary cathode material LiNi
aco
bmn
co
2(0.4≤a≤0.9,0.1≤b≤0.5,0.1≤c≤0.5, a+b+c=1).
In described step one, surfactant comprises: softex kw (CTAB), imidazoline.
In described step one, precipitation reagent comprises: oxalic acid, oxalic acid two formicester.
In described step one, divalent nickel salt is nickel acetate, nickelous carbonate or the mixture of the two.In described step one, divalent cobalt is cobalt acetate, cobalt carbonate or the mixture of the two; In described step one, manganous salt is manganese acetate, manganese carbonate or the mixture of the two.
The temperature of reacting in described step 2 is 120 ~ 220 DEG C, and the time of this reaction is 6 ~ 48h.
In described step 3, lithium salts is one or more any mixture in lithium nitrate, lithium acetate, lithium oxalate, lithium chloride, lithium carbonate, lithium hydroxide.
Beneficial effect
1, the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material of the present invention, the method has universality, and preparation technology is simple, and process is easy to the features such as control, is easy to industrialization promotion.The LiNi prepared
aco
bmn
co
2tertiary cathode material has the layer structure of standard, and primary particle is monocrystalline sub-micrometer scale granularity.
2, the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material of the present invention, the material of synthesis has the layer structure of standard, improve its high rate performance and cycle performance, its under 10C multiplying power specific discharge capacity up to 153.6mAh/g, after circulation 100 circle, capability retention reaches 80.5%, improves the energy density (10C assigns 1017Wh/L) of material.
Accompanying drawing explanation
Fig. 1 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2eSEM shape appearance figure before tertiary cathode material calcining;
Fig. 2 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2eSEM shape appearance figure after tertiary cathode material calcining;
Fig. 3 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2the X ray diffracting spectrum of tertiary cathode material;
Fig. 4 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2the transmission electron microscope shape appearance figure of tertiary cathode material;
Fig. 5 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2the electronic diffraction spectrogram of A is chosen in the transmission electron microscope shape appearance figure 4 of tertiary cathode material;
Fig. 6 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2the electronic diffraction spectrogram of B is chosen in the transmission electron microscope shape appearance figure 4 of tertiary cathode material;
Fig. 7 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2the electronic diffraction spectrogram of C is chosen in the transmission electron microscope shape appearance figure 4 of tertiary cathode material;
Fig. 8 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2the electronic diffraction spectrogram of D is chosen in the transmission electron microscope shape appearance figure 4 of tertiary cathode material;
Fig. 9 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2the first run discharge curve of tertiary cathode material under different multiplying;
Figure 10 is LiNi prepared by embodiment 1
0.6co
0.2mn
0.2o
2tertiary cathode material charges in 0.2C multiplying power, the cycle performance figure that the circulation under 0.2C, 0.5C, 1C, 2C, 5C, 10C discharge-rate is 100 times.
Embodiment
For further setting forth the present invention for the taked technological means that accomplishes the end in view, below in conjunction with drawings and Examples, to according to the present invention propose a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material preparation method and specifically implement means, step and effect thereof, be described in detail as follows.
Embodiment 1
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
1) by 2.98g Ni (CH
3cOO)
24H
2o, 1.00g Co (CH
3cOO)
24H
2o and 0.98g Mn (CH
3cOO)
24H
2o, is dissolved into (volume ratio 1:1) in the mixed solution of 80mL deionized water and ethylene glycol, stirs, add 1.5g CTAB after it dissolves completely, add 2.65g oxalic acid, be stirred to and mix completely after it dissolves completely.
2) by step 1) homogeneous mixture that obtains is transferred in stainless steel cauldron, and sealing is placed in air dry oven, under 200 DEG C of conditions, react 10h;
3), after reaction terminates, take out reactor and be cooled to room temperature, by the precursor liquid in reactor through centrifuge 5 times, be then placed in air dry oven, under 80 DEG C of conditions, dry 24h, obtains presoma, and its SEM shape appearance figure as shown in Figure 1;
4) by the LiNO of 0.81g
3join step 3) in 2g presoma in, after abundant mixing to be ground, be placed on pre-burning in the pre-burning stove of air atmosphere, heating rate 5 DEG C/min rises to calcined temperature 450 DEG C, and constant temperature pre-burning 5h, is cooled to room temperature, obtains oxide.Then oxide is placed in calciner high-temperature calcination, heating rate 3 DEG C/min is warming up to 500 DEG C, after constant temperature 3h, be warming up to 700 DEG C with 3 DEG C/min, constant temperature 3h, be warming up to calcining heat 850 DEG C with 3 DEG C/min thereafter, calcining 12h, is cooled to room temperature with 3 DEG C/min, thus obtains LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material, quality is about 1.9g, and its SEM shape appearance figure as shown in Figure 2.
By the LiNi obtained
0.6co
0.2mn
0.2o
2tertiary cathode material carries out X-ray diffraction test, and as shown in Figure 3, the diffraction pattern obtained and standard spectrogram contrast and illustrate that synthetic material is without dephasign without assorted peak result, and the comparatively sharp-pointed illustrative material crystallinity of diffraction maximum is better; LiNi will be obtained
0.6co
0.2mn
0.2o
2tertiary cathode material carries out transmission electron microscope and electronics chooses diffraction test, and result is as shown in Fig. 4-Fig. 8, and result illustrative material has a set of electronic diffraction speckle, illustrates that this material is a kind of single crystal grain.
The tertiary cathode material obtained is directly applied to lithium ion battery and carries out charging and discharging capacity test: LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material is as work electrode, and metal lithium sheet is to electrode, the LiF of 1mol/L
6/ EC+DMC+EMC (volume ratio 1: 1:1) is electrolyte, in argon gas atmosphere glove box, be assembled into simulated battery.Carry out charge-discharge test to simulated battery, voltage range is 2.8 ~ 4.3V (vs.Li
+/ Li).
Test result: LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material at the first run specific discharge capacity under different multiplying as shown in Figure 5, its first discharge specific capacity is 183.7mAh/g (0.2C) respectively, 172.7mAh/g (0.5C), 169.3mAh/g (1C), 165.7mAh/g (2C), 157.4mAh/g (5C), and 153.6mAh/g (10C); This material circulate under 0.2C, 0.5C, 1C, 2C, 5C and 10C multiplying power 100 times cycle performance as shown in Figure 6, as can be seen from the figure, charge under 0.2C multiplying power, the specific discharge capacity after 100 times that circulates under 0.2C, 0.5C, 1C, 2C, 5C and 10C discharge-rate is respectively 165.2mAh/g, 161.5mAh/g, 153.2mAh/g, 149.1mAh/g, 128.8mAh/g and 123.6mAh/g, capability retention is respectively 89.9%, and 93.5%, 90.5%, 90.0%, 81.8%, 80.5%.
Embodiment 2
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
Step is identical with the step in embodiment 1, difference be step 4) in by the LiNO of 0.81g
3join step 3) in 2g presoma in, after abundant mixing to be ground, be placed on pre-burning in the pre-burning stove of air atmosphere, heating rate 5 DEG C/min rises to calcined temperature 450 DEG C, and constant temperature pre-burning 10h, is cooled to room temperature, obtains oxide.Then oxide is placed in calciner high-temperature calcination, heating rate 10 DEG C/min is warming up to 500 DEG C, after constant temperature 10h, be warming up to 700 DEG C with 10 DEG C/min, constant temperature 10h, be warming up to calcining heat 950 DEG C with 10 DEG C/min thereafter, calcining 24h, is cooled to room temperature with 10 DEG C/min, thus obtains LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material, quality is about 1.9g.
By the LiNi obtained
0.6co
0.2mn
0.2o
2tertiary cathode material carries out X-ray diffraction test, and result shows that the diffraction pattern that obtains and standard spectrogram contrast without assorted peak, illustrates that synthetic material is without dephasign, and comparatively sharply illustrative material crystallinity is better for diffraction maximum; LiNi will be obtained
0.6co
0.2mn
0.2o
2tertiary cathode material carries out transmission electron microscope and electronics chooses diffraction test, and result illustrative material has a set of electronic diffraction speckle, illustrates that this material is a kind of single crystal grain.
The tertiary cathode material obtained is directly applied to lithium ion battery and carries out charging and discharging capacity test: LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material is as work electrode, and metal lithium sheet is to electrode, the LiF of 1mol/L
6/ EC+DMC+EMC (volume ratio 1: 1:1) is electrolyte, in argon gas atmosphere glove box, be assembled into simulated battery.Carry out charge-discharge test to simulated battery, voltage range is 2.8 ~ 4.3V (vs.Li
+/ Li).
Test result: LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material is 172.7mAh/g (0.2C) in first discharge specific capacity under different multiplying respectively, 165.7mAh/g (0.5C), 160.3mAh/g (1C), 155.7mAh/g (2C), 150.1mAh/g (5C), and 143.8mAh/g (10C); This material charges under 0.2C multiplying power, the specific discharge capacity after 100 times that circulates under 0.2C, 0.5C, 1C, 2C, 5C and 10C discharge-rate is respectively 151.3mAh/g, 149.3mAh/g, 140.3mAh/g, 135.3mAh/g, 124.1mAh/g and 115.5mAh/g, capability retention is respectively 87.6%, and 90.1%, 87.5%, 86.9%, 82.7%, 80.3%.
Embodiment 3
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
1) by 1.23g NiCO
3, 0.41g CoCO
3and 0.40g MnCO
3, be dissolved into (volume ratio 1:2) in the mixed solution of 80mL deionized water and ethylene glycol, stir, after it dissolves completely, add 1.5gCTAB, after it dissolves completely, add 2.65g oxalic acid, be stirred to and mix completely.
2) by step 1) homogeneous mixture that obtains is transferred in stainless steel cauldron, and sealing is placed in air dry oven, under 220 DEG C of conditions, react 6h;
3), after reaction terminates, take out reactor and be cooled to room temperature, by the precursor liquid in reactor through centrifuge 5 times, be then placed in air dry oven, under 80 DEG C of conditions, dry 24h, obtains presoma;
4) by the LiNO of 0.81g
3join step 3) in 2g presoma in, after abundant mixing to be ground, be placed on pre-burning in the pre-burning stove of air atmosphere, heating rate 8 DEG C/min rises to calcined temperature 400 DEG C, and constant temperature pre-burning 6h, is cooled to room temperature, obtains oxide.Then oxide is placed in calciner high-temperature calcination, heating rate 1 DEG C/min is warming up to 500 DEG C, after constant temperature 6h, be warming up to 700 DEG C with 1 DEG C/min, constant temperature 6h, be warming up to calcining heat 750 DEG C with 1 DEG C/min thereafter, calcining 16h, is cooled to room temperature with 1 DEG C/min, thus obtains LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material, quality is about 1.9g.
Carry out constant current charge-discharge performance test according to method of testing described in embodiment 1, under 0.2C multiplying power, first discharge specific capacity is 175.2mAh/g, and the capability retention after 100 times that circulates is 87.3%.
Embodiment 4
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
1) by 1.23g NiCO
3, 1.00g Co (CH
3cOO)
24H
2o and 0.98g Mn (CH
3cOO)
24H
2o, is dissolved into (volume ratio 2:1) in the mixed solution of 80mL deionized water and ethylene glycol, stirs, add 5.8g CTAB after it dissolves completely, add 2.90g oxalic acid, be stirred to and mix completely after it dissolves completely.
2) by step 1) homogeneous mixture that obtains is transferred in stainless steel cauldron, and sealing is placed in air dry oven, under 120 DEG C of conditions, react 48h;
3), after reaction terminates, take out reactor and be cooled to room temperature, by the precursor liquid in reactor through centrifuge 5 times, be then placed in air dry oven, under 80 DEG C of conditions, dry 24h, obtains presoma;
4) by the LiNO of 0.81g
3join step 3) in 2g presoma in, after abundant mixing to be ground, be placed on pre-burning in the pre-burning stove of air atmosphere, heating rate 5 DEG C/min rises to calcined temperature 450 DEG C, and constant temperature pre-burning 5h, is cooled to room temperature, obtains oxide.Then oxide is placed in calciner high-temperature calcination, heating rate 3 DEG C/min is warming up to 500 DEG C, after constant temperature 3h, be warming up to 700 DEG C with 3 DEG C/min, constant temperature 3h, be warming up to calcining heat 850 DEG C with 3 DEG C/min thereafter, calcining 12h, is cooled to room temperature with 3 DEG C/min, thus obtains LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material, quality is about 1.9g.
Carry out constant current charge-discharge performance test according to method of testing described in embodiment 1, under 0.2C multiplying power, first discharge specific capacity is 174.5mAh/g, and the capability retention after 100 times that circulates is 86.4%.
Embodiment 5
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
1) by 1.23g NiCO
3, 1.00g Co (CH
3cOO)
24H
2o and 0.40g MnCO
3, be dissolved into (volume ratio 1:5) in the mixed solution of 80mL deionized water and ethylene glycol, stir, after it dissolves completely, add 1.15g imidazoline, after it dissolves completely, add 2.52g oxalic acid, be stirred to and mix completely.
2) by step 1) homogeneous mixture that obtains is transferred in stainless steel cauldron, and sealing is placed in air dry oven, under 180 DEG C of conditions, react 12h;
3), after reaction terminates, take out reactor and be cooled to room temperature, by the precursor liquid in reactor through centrifuge 5 times, be then placed in air dry oven, under 80 DEG C of conditions, dry 24h, obtains presoma;
4) by 0.49g LiOHH
2o joins step 3) in 2g presoma in, after abundant mixing to be ground, be placed on pre-burning in the pre-burning stove of air atmosphere, heating rate 5 DEG C/min rises to calcined temperature 450 DEG C, and constant temperature pre-burning 5h, is cooled to room temperature, obtains oxide.Then oxide is placed in calciner high-temperature calcination, heating rate 3 DEG C/min is warming up to 500 DEG C, after constant temperature 3h, be warming up to 700 DEG C with 3 DEG C/min, constant temperature 3h, be warming up to calcining heat 850 DEG C with 3 DEG C/min thereafter, calcining 12h, is cooled to room temperature with 3 DEG C/min, thus obtains LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material, quality is about 1.9g.
Carry out constant current charge-discharge performance test according to method of testing described in embodiment 1, under 0.2C multiplying power, first discharge specific capacity is 177.6mAh/g, and the capability retention after 100 times that circulates is 87.1%.
Embodiment 6
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
1) by 1.23g NiCO
3, 1.00g Co (CH
3cOO)
24H
2o and 0.40g MnCO
3, be dissolved into (volume ratio 2:5) in the mixed solution of 80mL deionized water and ethylene glycol, stir, after it dissolves completely, add 1.15g imidazoline, after it dissolves completely, add 2.48g oxalic acid two formicester, be stirred to and mix completely.
2) by step 1) homogeneous mixture that obtains is transferred in stainless steel cauldron, and sealing is placed in air dry oven, under 200 DEG C of conditions, react 10h;
3), after reaction terminates, take out reactor and be cooled to room temperature, by the precursor liquid in reactor through centrifuge 5 times, be then placed in air dry oven, under 80 DEG C of conditions, dry 24h, obtains presoma;
4) by 0.49g LiOHH
2o joins step 3) in 2g presoma in, after abundant mixing to be ground, be placed on pre-burning in the pre-burning stove of air atmosphere, heating rate 5 DEG C/min rises to calcined temperature 450 DEG C, and constant temperature pre-burning 5h, is cooled to room temperature, obtains oxide.Then oxide is placed in calciner high-temperature calcination, heating rate 3 DEG C/min is warming up to 500 DEG C, after constant temperature 3h, be warming up to 700 DEG C with 3 DEG C/min, constant temperature 3h, be warming up to calcining heat 850 DEG C with 3 DEG C/min thereafter, calcining 12h, is cooled to room temperature with 3 DEG C/min, thus obtains LiNi
0.6co
0.2mn
0.2o
2tertiary cathode material, quality is about 1.9g.
Carry out constant current charge-discharge performance test according to method of testing described in embodiment 1, under 0.2C multiplying power, first discharge specific capacity is 168.6mAh/g, and the capability retention after 100 times that circulates is 93.1%.
Embodiment 7
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
Step is identical with the step in embodiment 1, and difference is step 4) in add the Li of 0.72g
2cO
3.Carry out constant current charge-discharge performance test according to method of testing described in embodiment 1, under 0.2C multiplying power, first discharge specific capacity is 175.6mAh/g, and the capability retention after 100 times that circulates is 88.2%.
Embodiment 8
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
Step is identical with the step in embodiment 1, difference be step 1) in add 5.8g CTAB.Carry out constant current charge-discharge performance test according to method of testing described in embodiment 1, under 0.2C multiplying power, first discharge specific capacity is 178.6mAh/g, and the capability retention after 100 times that circulates is 89.5%.
Embodiment 9
A preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, concrete steps are:
Step is identical with the step in embodiment 1, and difference is step 4) in naturally cool to room temperature after high-temperature calcination.Carry out constant current charge-discharge performance test according to method of testing described in embodiment 1, under 0.2C multiplying power, first discharge specific capacity is 179.6mAh/g, and the capability retention after 100 times that circulates is 90.2%.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned elaboration can be utilized or partly modify the Equivalent embodiments being considered as equivalent variations, in every case be the content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (8)
1. a preparation method for monocrystalline nickle cobalt lithium manganate tertiary cathode material, is characterized in that: concrete steps are as follows,
Step one, divalent nickel salt, divalent cobalt and manganous salt are dissolved in glycol water; The mol ratio of divalent nickel salt, divalent cobalt and manganous salt is a:b:c; Add surfactant after divalent nickel salt, divalent cobalt and manganous salt dissolve completely, the mol ratio of surfactant and divalent nickel salt, divalent cobalt and manganous salt mixture is 0.01 ~ 0.8:1; After surfactant dissolves completely, add precipitation reagent, the mol ratio of precipitation reagent and divalent nickel salt, divalent cobalt and manganous salt mixture is 1 ~ 1.15:1; Mixture is obtained after stirring;
Step 2, be transferred in reactor by step one gained mixture, sealing is placed in air dry oven reacts; After reaction terminates, take out reactor and be cooled to room temperature, after centrifugal, drying, obtain presoma;
Step 3, by pre-burning in air atmosphere after step 2 gained precursor and lithium salts Homogeneous phase mixing, the mol ratio of described lithium salts and divalent nickel salt, divalent cobalt and manganous salt mixture is (1 ~ 1.15): 1; The temperature of pre-burning is 400 ~ 480 DEG C, and the time of pre-burning is 3 ~ 10h; Be cooled to room temperature after pre-burning, obtain oxide; High temperature sintering under oxygen atmosphere again, oxide, from room temperature to 500 DEG C, sinters 3 ~ 10h at this temperature, and heating rate is 1 ~ 10 DEG C/min; And then be warming up to 700 DEG C, sinter 3 ~ 10h at this temperature, heating rate is 1 ~ 10 DEG C/min; Finally be warming up to 750 DEG C ~ 950 DEG C again, sinter 8 ~ 24h at this temperature, heating rate is 1 ~ 10 DEG C/min; Be down to room temperature, obtain monocrystalline nickle cobalt lithium manganate tertiary cathode material LiNi
aco
bmn
co
2, wherein 0.4≤a≤0.9,0.1≤b≤0.5,0.1≤c≤0.5, a+b+c=1.
2. the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material as claimed in claim 1, is characterized in that: in described step one, surfactant comprises: softex kw CTAB, imidazoline.
3. the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material as claimed in claim 1, is characterized in that: in described step one, precipitation reagent comprises: oxalic acid, oxalic acid two formicester.
4. the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material as claimed in claim 1, is characterized in that: in described step one, divalent nickel salt is nickel acetate, nickelous carbonate or the mixture of the two.
5. the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material as claimed in claim 1, is characterized in that: in described step one, divalent cobalt is cobalt acetate, cobalt carbonate or the mixture of the two.
6. the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material as claimed in claim 1, is characterized in that: in described step one, manganous salt is manganese acetate, manganese carbonate or the mixture of the two.
7. the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material as claimed in claim 1, is characterized in that: the temperature of reacting in described step 2 is 120 ~ 220 DEG C, and the time of this reaction is 6 ~ 48h.
8. the preparation method of a kind of monocrystalline nickle cobalt lithium manganate tertiary cathode material as claimed in claim 1, is characterized in that: in described step 3, lithium salts is one or more any mixture in lithium nitrate, lithium acetate, lithium oxalate, lithium chloride, lithium carbonate, lithium hydroxide.
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