CN103259008B - Ternary composite positive electrode material of lithium ion battery and preparation method thereof - Google Patents

Ternary composite positive electrode material of lithium ion battery and preparation method thereof Download PDF

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CN103259008B
CN103259008B CN201310126591.2A CN201310126591A CN103259008B CN 103259008 B CN103259008 B CN 103259008B CN 201310126591 A CN201310126591 A CN 201310126591A CN 103259008 B CN103259008 B CN 103259008B
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preparation
manganese
nickel
lithium
salt
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CN103259008A (en
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崔萍
梁英
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Xiangyang Huahong tech new material Co. Ltd.
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Hubei University of Arts and Science
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a ternary composite positive electrode material of a lithium ion battery and a preparation method thereof. The preparation method comprises the following steps: mixing a nickel salt, a manganese salt, a vanadium salt and citric acid, adding water or ethanol which is to be used as a ball milling solvent, carrying out drying after ball milling and carrying out calcining in a muffle furnace so as to obtain an intermediate product; and subjecting the intermediate product and a lithium salt to ball milling and batch mixing, putting an obtained mixture into the muffle furnace and carrying out heating and calcining again in an air atmosphere so as to obtain the ternary composite positive electrode material LiNi0.5Mn0.25V0.25O2. According to the invention, vanadium is used to substitute cobalt to prepare the ternary composite positive electrode material, so production cost for the lithium ion battery and environmental pollution are reduced. The prepared ternary composite positive electrode material has high specific capacity and good cycle performance and safety performance.

Description

A kind of ternary composite cathode material of lithium ion battery and preparation method thereof
Technical field
The invention belongs to lithium ion secondary battery anode material field, be specifically related to the preparation method of a kind of ternary composite cathode material and this material.
Background technology
Lithium ion battery is since the commercialization nineties of 20th century, development rapidly, because of its have that specific energy is high, battery operating voltage is high, operating temperature range is wide, have extended cycle life, the feature such as memory-less effect and environmental sound, be widely used in military and civilian compact electric apparatus, as mobile phone, notebook computer, camera, microcam, electric tool etc.
Positive electrode is one of important component part of lithium ion battery.LiCoO 2as commercial positive electrode is still most widely used the earliest, LiCoO 2good cycle, production technology are ripe, product is stablized, but actual capacity is not high, there is potential safety hazard, so all substitute LiCoO in searching in recent years 2positive electrode: LiNiO 2capacity is high, but its synthesis condition is harsh, is difficult to realize industrialization; LiMn 2o 4security performance is good, low price, but specific capacity is low, and high temperature cyclic performance is poor.Tertiary cathode material LiCo 1/3ni 1/3mn 1/3o 2combine LiCoO 2good cycle performance, LiNiO 2height ratio capacity, LiMn 2o 4high safety performance and low-cost advantage, be the high performance lithium ion battery anode material with Ni, Co, Mn tri-kinds of element cooperative effects, but cobalt resource is deficient, expensive and cobalt is poisonous, limit its large-scale application.
Current lithium cobalt nickel manganese oxide positive electrode mainly adopts coprecipitation to prepare: after obtained cobalt, nickel, manganese composite hydroxide precursor, precursor is joined lithium salts sintering.Although coprecipitation improves being uniformly distributed of ion to a certain extent, also there are some defects: co-precipitation preparation method cost is high, complex process, process control is difficult, produces a large amount of waste water in production process, big for environment pollution.
In transition metal, the price of vanadium is lower, aboundresources, has multiple valence state, can form many oxide, as VO 2, V 2o 5, V 3o 7, V 4o 9and V 6o 13deng, also can form Li with lithium in addition 1+xv 3o 8.Therefore the oxide of vanadium is very potential as anode material for lithium-ion batteries, has the advantages such as specific capacity is high, aboundresources.If replace cobalt formation nickel, manganese, vanadium ternary composite cathode material can reduce the cost of lithium ion battery with vanadium, reduce the pollution to environment.
Summary of the invention
In order to overcome the deficiency that lithium cobalt nickel manganese oxide positive electrode exists, the present invention seeks under the prerequisite not affecting specific capacity, replace cobalt to form nickel, manganese, vanadium ternary composite cathode material with vanadium, provide that a kind of cost is lower, the anode material for lithium-ion batteries of more environmental protection and preparation method thereof.The method technique is simple, production is easy to control, cost is low, and obtained product has the characteristic that specific capacity is high, good cycle, security performance are good.
The present invention can take following technical scheme to implement: a kind of preparation method of ternary composite cathode material of lithium ion battery, is characterized in that: preparation method comprises the following steps:
(1) nickel salt, manganese salt, vanadic salts and citric acid are mixed, under medium, ball milling obtains pastes gels body in 2 ~ 5 hours.Wherein the molar ratio of nickel salt, manganese salt, vanadic salts, citric acid is 1:0.5:0.5:1;
(2) dried in air dry oven by pastes gels body, bake out temperature is 80 ~ 120 DEG C, and drying time is 10 ~ 15 hours, obtains dry gelinite;
(3) gelinite of drying is put into Muffle furnace to calcine, calcining heat is 400 ~ 500 DEG C, and calcination time is 15 ~ 20 hours, obtains the composite oxides of nickel, manganese, vanadium;
(4) by naturally cool to the nickel after normal temperature, manganese, vanadium composite oxides mix with lithium salts, then in grinding in ball grinder 0.5 ~ 2 hour, batch mixing after grinding is put into Muffle furnace in 700 ~ 850 DEG C of calcining at constant temperature 25 ~ 35 hours, namely obtaining chemical molecular formula after naturally cooling to normal temperature is LiNi 0.5mn 0.25v 0.25o 2finished product ternary composite cathode material powder.
Nickel salt in step (1) is nickel nitrate or nickel acetate, and manganese salt is manganese acetate or manganese nitrate, and vanadic salts is ammonium metavanadate.
Medium in step (1) is ethanol or water, and the mass ratio of compound and medium is 1:0.9 ~ 1.1.Adopt ethanol or water mainly to allow various raw material mix as medium, select ethanol favourable post-order process medium can better be allowed to volatilize, during enforcement, the ethanol of various purity, selects that water is favourable to be reduced costs.
Ball milling speed in step (1) and step (4) is 200 ~ 400 revs/min.
Lithium salts in step (4) is lithium hydroxide or lithium carbonate.
The molar ratio of nickel, manganese, vanadium oxides composite and lithium salts in step (4) is 1:1.
The present invention has following advantage and effect: the composite oxides of the present invention's nickel that adopted Rheological Phase Method to prepare, manganese, vanadium, and the application of ball grinding technique improves the reactivity of material and the uniformity of batch mixing; The pastes gels body obtained directly is dried rear sintering to obtain intermediate product by the preparation technology of Rheological Phase Method, and compared with preparing tertiary cathode material with coprecipitation, can not produce a large amount of waste water because of washing of precipitate, production technology is simplified; The present invention replaces expensive and poisonous cobalt to prepare ternary composite cathode material with aboundresources, cheap vanadium, reduces the production cost of lithium ion battery, decreases the pollution to environment; The material specific capacity that the present invention obtains is high, cycle performance and security performance good.
Accompanying drawing explanation
Fig. 1 is tertiary cathode material LiNi prepared by the embodiment of the present invention 1 0.5mn 0.25v 0.25o 2xRD figure.
Fig. 2 is tertiary cathode material LiNi prepared by the embodiment of the present invention 1 0.5mn 0.25v 0.25o 2cycle performance curve chart.
In Fig. 1, tertiary cathode material LiNi 0.5mn 0.25v 0.25o 2there is α-NaFeO 2layer structure.
In Fig. 2, charging/discharging voltage scope 2.5V ~ 4.8V, discharge-rate 0.1C.LiNi 0.5mn 0.25v 0.25o 2the discharge capacity first of positive electrode is 154mAh/g, and after 20 circulations, discharge capacity is 142.3mAh/g, and inducing capacity fading is only 7.6%.
Embodiment
Embodiment 1: produce ternary composite cathode material LiNi 0.5mn 0.25v 0.25o 2powder 5g.Concrete steps are as follows:
(1) 4.75g nickel nitrate, 2.25g manganese acetate, 1.52g ammonium metavanadate and 5g citric acid are mixed, wherein the molar ratio of nickel salt, manganese salt, vanadic salts, citric acid is 1:0.5:0.5:1.The zirconium ball being 1:4 with ratio of grinding media to material together adds in ball grinder, adds 15ml water as ball milling solvent (mass ratio of compound and solvent is 1:1.1), after sealing on planetary ball mill with the speed ball mill mixing 3 hours of 300rpm.
(2) the pastes gels body obtained is placed in air dry oven to dry, bake out temperature is 110 DEG C, and drying time is 12 hours.
(3) the desiccant gel body that step (2) produces is put in Muffle furnace, is warmed up to 450 DEG C with the speed of 5 DEG C/min, be incubated 15 hours, be cooled to normal temperature with stove.
(4) the composite oxides intermediate product obtained is mixed with 1.25g lithium hydroxide ((Ni+Mn+V): Li=1:1), with the speed ball milling 1.5 hours of 250rpm on planetary ball mill, discharging loads corundum crucible and is placed in Muffle furnace, under air atmosphere condition, 850 DEG C are warmed up to the speed of 5 DEG C/min, be incubated 30 hours, after being cooled to normal temperature with stove, namely obtain finished product positive electrode.Fig. 1 is shown in by its XRD collection of illustrative plates.
The chemical property of gained sample measures as follows: positive electrode active material powder, conductive agent acetylene black, binding agent Kynoar in mass ratio 85:8:7 mix.Take 2.25g trielement composite material LiNi 0.5mn 0.25v 0.25o 2positive pole powder, add 0.21g acetylene black as conductive agent, add 0.19gPVDF again as adhesive, solvent is made with 1-METHYLPYRROLIDONE NMP, speed ball milling with 280rpm on planetary ball mill after sealing mixes 2 hours, the slurry obtained evenly is coated on aluminium collector, and at 80 DEG C, vacuum drying 10 hours, obtains positive plate.Take metal lithium sheet as the LiPF of negative pole, 1.0mol/L 6/ EC+DMC (1:1) is electrolyte, Celgard2320 film is barrier film, in the glove box being full of argon gas, be assembled into battery, under 0.1C multiplying power, carry out constant current charge-discharge test, voltage range 2.5V ~ 4.8V, the charge/discharge capacity of test positive electrode and cycle performance.Its cycle performance curve chart is shown in Fig. 2.
Embodiment 2: produce ternary composite cathode material LiNi 0.5mn 0.25v 0.25o 2powder 9.5g.Concrete steps are as follows:
(1) manganese nitrate solution of 8.84g nickel acetate, 8.95g50%, 2.92g ammonium metavanadate and 9.6g citric acid are mixed, wherein the molar ratio of nickel salt, manganese salt, vanadic salts, citric acid is 1:0.5:0.5:1.The zirconium ball being 1:4 with ratio of grinding media to material together adds in ball grinder, adds 27ml water as ball milling solvent (mass ratio of compound and solvent is 1:0.9), after sealing on planetary ball mill with the speed ball mill mixing 2 hours of 200rpm.
(2) the pastes gels body obtained is placed in air dry oven to dry, bake out temperature is 120 DEG C, and drying time is 10 hours.
(3) the desiccant gel body that step (2) produces is put in Muffle furnace, is warmed up to 400 DEG C with the speed of 5 DEG C/min, be incubated 18 hours, be cooled to normal temperature with stove.
(4) the composite oxides intermediate product obtained is mixed with 3.7g lithium carbonate ((Ni+Mn+V): Li=1:1), with the speed ball milling 0.5 hour of 200rpm on planetary ball mill, discharging loads corundum crucible and is placed in Muffle furnace, under air atmosphere condition, 750 DEG C are warmed up to the speed of 5 DEG C/min, be incubated 25 hours, after being cooled to normal temperature with stove, namely obtain finished product positive electrode.
Detection method is with embodiment 1.
Embodiment 3: produce ternary composite cathode material LiNi 0.5mn 0.25v 0.25o 2powder 49.3g.Concrete steps are as follows:
(1) 45.94g nickel acetate, 22.5g manganese acetate, 15.2g ammonium metavanadate and 49.96g citric acid are mixed, wherein the molar ratio of nickel salt, manganese salt, vanadic salts, citric acid is 1:0.5:0.5:1.The zirconium ball being 1:4 with ratio of grinding media to material together adds in ball grinder, adds 169ml ethanol as ball milling solvent (mass ratio of compound and solvent is 1:1), after sealing on planetary ball mill with the speed ball mill mixing 5 hours of 400rpm.
(2) the pastes gels body obtained is placed in air dry oven to dry, bake out temperature is 80 DEG C, and drying time is 15 hours.
(3) the desiccant gel body that step (2) produces is put in Muffle furnace, is warmed up to 500 DEG C with the speed of 5 DEG C/min, be incubated 20 hours, be cooled to normal temperature with stove.
(4) the composite oxides intermediate product obtained is mixed with 19.2g lithium carbonate ((Ni+Mn+V): Li=1:1), with the speed ball milling 2 hours of 400rpm on planetary ball mill, discharging loads corundum crucible and is placed in Muffle furnace, under air atmosphere condition, 700 DEG C are warmed up to the speed of 5 DEG C/min, be incubated 35 hours, after being cooled to normal temperature with stove, namely obtain finished product positive electrode.
Detection method is with embodiment 1.
Embodiment 4: produce ternary composite cathode material LiNi 0.5mn 0.25v 0.25o 2powder 94.8g.Concrete steps are as follows:
(1) manganese nitrate solution of 91.4g nickel nitrate, 89.5g50%, 29.3g ammonium metavanadate and 96g citric acid are mixed, wherein the molar ratio of nickel salt, manganese salt, vanadic salts, citric acid is 1:0.5:0.5:1.The zirconium ball being 1:4 with ratio of grinding media to material together adds in ball grinder, adds 368ml ethanol as ball milling solvent (mass ratio of compound and solvent is 1:0.95), after sealing on planetary ball mill with the speed ball mill mixing 5 hours of 400rpm.
(2) the pastes gels body obtained is placed in air dry oven to dry, bake out temperature is 100 DEG C, and drying time is 15 hours.
(3) the desiccant gel body that step (2) produces is put in Muffle furnace, is warmed up to 450 DEG C with the speed of 5 DEG C/min, be incubated 20 hours, be cooled to normal temperature with stove.
(4) the composite oxides intermediate product obtained is mixed with 23.95g lithium hydroxide ((Ni+Mn+V): Li=1:1), with the speed ball milling 2 hours of 400rpm on planetary ball mill, discharging loads corundum crucible and is placed in Muffle furnace, under air atmosphere condition, 850 DEG C are warmed up to the speed of 5 DEG C/min, be incubated 30 hours, after being cooled to normal temperature with stove, namely obtain finished product positive electrode.
Detection method is with embodiment 1.

Claims (6)

1. a preparation method for ternary composite cathode material of lithium ion battery, is characterized in that: preparation method comprises the following steps:
(1) nickel salt, manganese salt, vanadic salts and citric acid are mixed, under medium, ball milling obtains pastes gels body in 2 ~ 5 hours, and wherein the molar ratio of nickel salt, manganese salt, vanadic salts, citric acid is 1:0.5:0.5:1;
(2) dried in air dry oven by pastes gels body, bake out temperature is 80 ~ 120 DEG C, and drying time is 10 ~ 15 hours, obtains dry gelinite;
(3) gelinite of drying is put into Muffle furnace to calcine, calcining heat is 400 ~ 500 DEG C, and calcination time is 15 ~ 20 hours, obtains the composite oxides of nickel, manganese, vanadium;
(4) mix with lithium salts after the composite oxides that step (3) produces being naturally cooled to normal temperature, then in grinding in ball grinder 0.5 ~ 2 hour, batch mixing after grinding is put into Muffle furnace in 700 ~ 850 DEG C of calcining at constant temperature 25 ~ 35 hours, namely obtaining chemical molecular formula after naturally cooling to normal temperature is LiNi 0.5mn 0.25v 0.25o 2finished product ternary composite cathode material powder.
2. preparation method according to claim 1, is characterized in that: the nickel salt in step (1) is nickel nitrate or nickel acetate, and manganese salt is manganese acetate or manganese nitrate, and vanadic salts is ammonium metavanadate.
3. preparation method according to claim 1, is characterized in that: the medium in step (1) is ethanol or water, and the mass ratio of compound and medium is 1:0.9 ~ 1.1.
4. preparation method according to claim 1, is characterized in that: the ball milling speed in step (1) and step (4) is 200 ~ 400 revs/min.
5. preparation method according to claim 1, is characterized in that: the lithium salts in step (4) is lithium hydroxide or lithium carbonate.
6. preparation method according to claim 1, is characterized in that: in the nickel in step (4), manganese, vanadium oxides composite, the mole sum of nickel, manganese, vanadium and the mole of lithium in lithium salts are than being 1:1.
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CN104409723B (en) * 2014-12-25 2016-09-28 芜湖华欣诺电化学科技有限公司 A kind of electrochemical preparation method of tertiary cathode material
CN110061319B (en) * 2018-12-31 2021-05-14 圣戈莱（北京）科技有限公司 Method for recycling ternary positive electrode material of waste power lithium ion battery
CN110085835B (en) * 2019-04-30 2021-09-21 河南固锂电技术有限公司 Preparation method of positive electrode composite material for high-energy-density all-solid-state lithium ion battery
CN112447968A (en) 2019-09-02 2021-03-05 宁德时代新能源科技股份有限公司 Positive electrode active material, positive electrode plate and lithium ion secondary battery
CN112062166B (en) * 2020-08-29 2023-03-31 渤海大学 Ternary composite electrode material for hybrid capacitor and application thereof

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