CN102386381B - Preparation method of nano positive material for lithium ion battery - Google Patents

Preparation method of nano positive material for lithium ion battery Download PDF

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CN102386381B
CN102386381B CN201010266326.0A CN201010266326A CN102386381B CN 102386381 B CN102386381 B CN 102386381B CN 201010266326 A CN201010266326 A CN 201010266326A CN 102386381 B CN102386381 B CN 102386381B
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lithium
salt
nickel
manganese
cobalt
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CN201010266326.0A
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CN102386381A (en
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王萌
陈蕴博
陈林
左玲立
谷亦杰
牟锐
张钊
李青海
林道勇
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机械科学研究总院先进制造技术研究中心
江苏绿科能源有限公司
山东润锋新能源科技有限公司
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention belongs to the field of preparation techniques of nanophase materials and green energy resources, and relates to a preparation method of a nano positive material LiNi1/3Mn1/3Co1/3O2 applied to a lithium ion battery. By using the method, the defects that the calcining temperature needed by a current synthetic material is high, the calcining time is long, the particle sizes of a product are not uniform, and the like, are mainly solved. The preparation method comprises the following steps: adding a certain amount of template agent in a mixed aqueous solution of a nickel salt, a manganese salt and a cobalt salt, and then, dripping a precipitant and a complexing agent into the obtained mixture to form a precipitate; subjecting the precipitate and the mixed aqueous solution to a high-pressure thermal reaction in a hydrothermal kettle, cleaning and baking the obtained product to be dry, so as to obtain a nickel manganese cobalt oxide; and finally, uniformly mixing the nickel manganese cobalt oxide with the lithium salt to prepare a final product by calcining and cooling. By using the preparation method, the product with favorable electrochemical performance can be obtained within a shorter calcining time; the energy consumption is decreased; and the preparation method has obvious economic benefit in the large-scale application of industrial synthesis.

Description

A kind of preparation method of nano positive material for lithium ion battery

Technical field

The invention belongs to nano material technology of preparing and green energy resource field, relate to a kind of nanoscale positive electrode LiNi that is applied to lithium ion battery 1/3mn 1/3co 1/3o 2preparation method.

Background technology

The two main tasks of Study on Li-ion batteries using is improve performance (being mainly high energy density and power density, long-life, fail safe) and reduce costs.And positive electrode is the key that improves performance of lithium ion battery, it determines the main performance index of lithium ion battery.With regard to positive electrode in power lithium-ion rechargeable battery, cobalt acid lithium (LiCoO 2) there is the problems such as thermal runaway the risk and cost height of large battery; LiMn2O4 (LiMn 2o 4) there is the advantages such as low cost, environmental friendliness, fail safe height, but its energy density is low, cycle performance is poor, Mn dissolution problems outstanding; LiFePO4 (LiFePO 4) system has the advantages such as low cost, high charge stability and safety, but the problems such as energy density is low, electron conduction rate variance, complicated process of preparation.And the development of the new stratiform embedding lithium ternary system Li-Ni-Mn-Co-O composite oxides that rise is in recent years rapid, its representative is nickel manganese cobalt acid lithium (LiNi 1/3mn 1/3co 1/3o 2).This type of material electrochemical performance is stable, discharge capacity and discharge-rate is high, Heat stability is good, fail safe are good, and its combination property is better than any one-component compound, is a kind of novel anode material that is expected to substituting cobalt acid lithium.

Although LiNi 1/3mn 1/3co 1/3o 2material has vast potential for future development, but its complicated process of preparation is not suitable for industrial production, has limited its practical application.Conventional solid phase method synthetic method operating procedure is simple, but the material component inequality that energy consumption is large, the reaction time is long, synthetic is once inadequate; Although the liquid phase method such as sol-gal process, the precipitation method can synthesize the product of component homogeneous, heat treated calcining heat very high (over 900 ℃), calcination time are long, and the energy consumption that makes to prepare material is large.Meanwhile, the low conductivity of positive electrode has had a strong impact on its chemical property under large electric current.And nano level powder particle is a kind of effective way that improves positive electrode large-current electric chemical property: can shorten the evolving path, the increase material specific area of lithium ion, increase the contact area of active material and electrolyte, thereby improve ionic conductivity.

The people such as Kobayashi (Kobayashi H, Arachi Y, Emura S, et al. Investigation on lithium de-intercalation mechanism for Li1-yNi1/3Mn1/3Co1/3O2[J]. Journal of Power Sources, 2005,146:640-644.) adopt hydroxide precipitation method to calcine at 1000 ℃ and within 24 hours, just obtain the LiNi that discharge capacity is 160 mAh/g 1/3mn 1/3co 1/3o 2.And the present invention can obtain the product that chemical property is good in shorter calcination time (2 ~ 12 hours), with low cost, be easy to industrialization; Adopt water as solvent, environmental protection; The interpolation of template makes product pattern rule, size homogeneous, difficult reunion, and high rate charge-discharge performance is splendid, compares with the method for other document patent report, has outstanding novelty and advance.

Summary of the invention

The object of this invention is to provide and a kind ofly can in shorter calcination time, prepare the nano-scale lithium ion battery anode material LiNi that chemical property is good 1/3mn 1/3co 1/3o 2method.

Nanoscale positive electrode LiNi of the present invention 1/3mn 1/3co 1/3o 2preparation method, its concrete steps are as follows:

(1) adopting nickel salt, manganese salt, the cobalt salt of solubility is raw material, presses positive electrode LiNi 1/3mn 1/3co 1/3o 2nickel, manganese, cobalt ratio in component, be mixed with the mixed aqueous solution of nickel salt, manganese salt, cobalt salt, and wherein tenor is 2 mol/L;

(2) in the solution in step (1), add a certain amount of template, template quality and target product mass ratio are 0.1 ~ 3, with 800 ~ 1200 revs/min, stir 0.2 ~ 1.5 hour;

(3) at N 2under atmosphere, in the solution of step (2), drip precipitation reagent and complexing agent simultaneously, simultaneously with 800 ~ 1200 revs/min of stirrings, keep 40 ~ 70 ℃ of reaction temperatures, keep the pH value 9 ~ 13 of reaction system.Precipitation has formed rear continuation and has kept stirring 1 ~ 3 hour;

(4) precipitation and the solution that in step (3), form are transferred in water heating kettle, compactedness is 60 ~ 90 %, and under 100 ~ 280 ℃ of thermal and hydric environments, hot high pressure reaction is 6 ~ 40 hours;

(5) sedimentation and filtration in step (4) is cleaned, filter cake is dried to obtain oxidation of precursor nickel manganese cobalt; Press positive electrode component ratio, presoma and lithium compound are mixed in batch mixer; At 200 ~ 400 ℃, preheating is 2 ~ 12 hours, is warming up to 600 ~ 1000 ℃ of calcinings 2 ~ 15 hours, obtains the LiNi of nanoscale stratiform structure after cooling grinding 1/3mn 1/3co 1/3o 2.

Nickel salt used is nickel acetate, nickel nitrate or nickel oxalate.

Manganese salt used is manganese acetate, manganese nitrate or manganese oxalate.

Cobalt salt used is cobalt acetate, cobalt nitrate or cobalt oxalate.

Lithium salts used is lithium acetate, lithium nitrate, lithium oxalate, lithium formate, lithium nitrite or lithium citrate.

Template used is active carbon powder, activated carbon fiber, carbon nano-tube, sawdust, wood powder, bamboo carbon powder, cornstalk, cellulose, peanut shell, carbon aerogels, starch, sucrose, ethyl phosphonic acid ester, polypropylene glycol, polyacrylamide, polypropylene ether, polystyrene, polyvinylether, Merlon or polymethyl methacrylate.

Complexing agent used is urea or ammoniacal liquor.

Precipitation reagent used is lithium hydroxide or NaOH, and itself and the total mol ratio of nickel ion+manganese ion+cobalt ions are 2 ~ 4.The mol ratio of complexing agent and precipitation reagent is 0.1 ~ 2.

Nanoscale positive electrode LiNi of the present invention 1/3mn 1/3co 1/3o 2preparation method, be characterized in: by changing template and regulating calcination time and temperature, can prepare average crystal grain at the nanoscale LiNi of 15 nm ~ 200 nm 1/3mn 1/3co 1/3o 2composite oxides, tap density is 1.8 ~ 2.8 g/m 3.At 0.2 C, discharge and recharge under condition, its discharge capacity is more than 178 mAh/g.

The invention has the advantages that:

1, heat treatment time is short, less energy consumption;

2, technique is simple, is easy to industrialization and amplifies, prepared ternary system LiNi 1/3mn 1/3co 1/3o 2particle size distribution is even, and pattern rule is difficult for reuniting, and composition is easily controlled;

3, in precursor synthesis process, adopt water as solvent, environmental protection;

4, prepared ternary system LiNi 1/3mn 1/3co 1/3o 2charge-discharge performance is outstanding, and 0.2 C discharges and recharges under condition, and its Reversible lithium insertion capacity is more than 178 mAh/g, and 1.0 C discharge and recharge capability retention that condition circulates 40 weeks in 98 % left and right, and good cycle, is the desirable positive electrode of power-type lithium ion secondary cell.

Accompanying drawing explanation

Fig. 1 is the prepared ternary system LiNi of embodiment 1 1/3mn 1/3co 1/3o 2the stereoscan photograph of composite material, multiplication factor is 20,000 times;

Fig. 2 is the prepared ternary system LiNi of embodiment 2 1/3mn 1/3co 1/3o 2initial charge/discharge curve, voltage range is 2.8-4.5 V, electrolyte is 1mol/L LiPF 6/ EC-DMC(1:1), charging and discharging currents density is 0.2 C;

Fig. 3 is the prepared ternary system LiNi of embodiment 1 1/3mn 1/3co 1/3o 2cycle performance curve, voltage range is 2.8-4.5V, electrolyte is 1mol/L LiPF 6/ EC-DMC(1:1), charging and discharging currents density is 1.0 C.

Embodiment

Embodiment 1: get 11.63 g nickel nitrates, 7.158 g manganese nitrates and 11.64 g cobalt nitrates, be dissolved in deionized water solution, the concentration of metal ion is 2 mol/L, adds 0.5 g polypropylene glycol simultaneously, with 800 revs/min, stirs 0.5 hour.At N 2under atmosphere, in above-mentioned solution, drip containing the aqueous solution of lithium hydroxide 0.08 mol and the aqueous solution of urea of 0.08 mol simultaneously, and with 800 revs/min of stirrings, keep 45 ℃ of reaction temperatures, keep the pH value 10 of reaction system.Precipitation has formed rear continuation and has kept stirring 2 hours.The precipitation of formation and solution are transferred in water heating kettle, and compactedness is 70 %, takes out precipitation after reacting 12 hours under 160 ℃ of thermal and hydric environments, filters and cleans, and filter cake is dried to obtain oxidation of precursor nickel manganese cobalt.Presoma and 2.76 g lithium nitrates are mixed in batch mixer, 400 ℃ of the pre-heat treatment 4 hours, be warming up to 800 ℃ of calcinings 4 hours, after cooling grinding, obtain the LiNi of nanoscale stratiform structure 1/3mn 1/3co 1/3o 2.Its average crystal grain, at 100 nm, discharges and recharges under condition at 0.2 C, and its discharge capacity is at 178.7 mAh/g, and 1.0 C discharge and recharge capability retention that condition circulates 40 weeks at 97.9 %.

Embodiment 2: get 9.95 g nickel acetates, 9.80 g manganese acetates and 9.96 g cobalt acetates and be dissolved in deionized water solution, the concentration of metal ion is 2 mol/L, adds 1.5 g carbon nano-tube simultaneously, with 1000 revs/min, stir 0.6 hour.At N 2under atmosphere, in above-mentioned solution, drip containing the aqueous solution of NaOH 0.12 mol and the aqueous solution of urea of 0.05 mol simultaneously, and with 1200 revs/min of stirrings, keep 40 ℃ of reaction temperatures, keep the pH value 11 of reaction system.Precipitation has formed rear continuation and has kept stirring 2 hours.The precipitation of formation and solution are transferred in water heating kettle, and compactedness is 70 %, takes out precipitation after reacting 16 hours under 150 ℃ of thermal and hydric environments, filters and cleans, and filter cake is dried to obtain oxidation of precursor nickel manganese cobalt.Presoma and 4.08 g lithium acetates are mixed in batch mixer; At 350 ℃, the pre-heat treatment is 3.5 hours, is warming up to 850 ℃ of calcinings 6 hours, obtains the LiNi of nanoscale stratiform structure after cooling grinding 1/3mn 1/3co 1/3o 2.Its average crystal grain, at 120 nm, discharges and recharges under condition at 0.2 C, and its discharge capacity is at 187.7 mAh/g, and 1.0 C discharge and recharge capability retention that condition circulates 40 weeks at 98.7 %.

Embodiment 3: get 17.06g nickel oxalate, 19.06g manganese oxalate, 19.59g cobalt oxalate and be dissolved in deionized water solution, the concentration of metal ion is 2 mol/L, adds 0.7 g cornstalk simultaneously, with 1000 revs/min, stir 1 hour.At N 2under atmosphere, in above-mentioned solution, drip containing the aqueous solution of lithium hydroxide 0.16 mol and the aqueous solution of urea of 0.05 mol simultaneously, and with 1100 revs/min of stirrings, keep 45 ℃ of reaction temperatures, keep the pH value 12 of reaction system.Precipitation has formed rear continuation and has kept stirring 2 hours.The precipitation of formation and solution are transferred in water heating kettle, and compactedness is 85 %, takes out precipitation after reacting 12 hours under 200 ℃ of thermal and hydric environments, filters and cleans, and filter cake is dried to obtain oxidation of precursor nickel manganese cobalt.Presoma and 4.08 g lithium oxalates are mixed in batch mixer; At 450 ℃, the pre-heat treatment is 4 hours, is warming up to 900 ℃ of calcinings 5 hours, obtains the LiNi of nanoscale stratiform structure after cooling grinding 1/3mn 1/3co 1/3o 2.Its average crystal grain is at 150 nm.At 0.2 C, discharge and recharge under condition, its discharge capacity is at 192.3 mAh/g, and 1.0 C discharge and recharge capability retention that condition circulates 40 weeks at 99.2 %.

Embodiment 4: get 11.63 g nickel nitrates, 7.158 g manganese nitrates and 11.64 g cobalt nitrates and be dissolved in deionized water solution, the concentration of metal ion is 2 mol/L, adds 1.0 g bamboo charcoal powder simultaneously, with 1000 revs/min, stir 0.5 hour.At N 2under atmosphere, in above-mentioned solution, drip containing the aqueous solution of lithium hydroxide 0.2 mol and the aqueous solution of urea of 0.04 mol simultaneously, and with 1000 revs/min of stirrings, keep 40 ℃ of reaction temperatures, keep the pH value 13 of reaction system.Precipitation has formed rear continuation and has kept stirring 1 hour.The precipitation of formation and solution are transferred in water heating kettle, and compactedness is 85 %, takes out precipitation after reacting 20 hours under 180 ℃ of thermal and hydric environments, filters and cleans, and filter cake is dried to obtain oxidation of precursor nickel manganese cobalt.Presoma and 11.28 g lithium citrates are mixed in batch mixer; At 400 ℃, the pre-heat treatment is 4 hours, is warming up to 800 ℃ of calcinings 7 hours, obtains the LiNi of nanoscale stratiform structure after cooling grinding 1/3mn 1/3co 1/3o 2.Its average crystal grain is at 130 nm.At 0.2 C, discharge and recharge under condition, its discharge capacity is at 200.3 mAh/g, and 1.0 C discharge and recharge capability retention that condition circulates 40 weeks at 99.5 %.

Claims (7)

1. a nano positive material for lithium ion battery LiNi 1/3mn 1/3co 1/3o 2preparation method, it is characterized in that comprising the following steps:
(1) adopting nickel salt, manganese salt, the cobalt salt of solubility is raw material, presses positive electrode LiNi 1/3mn 1/3co 1/3o 2nickel, manganese, cobalt ratio in component, be mixed with the mixed solution of nickel salt, manganese salt, cobalt salt, and wherein tenor is 2 mol/L;
(2) in the solution in step (1), add a certain amount of template, template quality and target product mass ratio are 0.1 ~ 3, with 800 ~ 1200 revs/min of stirrings 0.2 ~ 1.5 hour, described template was active carbon powder, activated carbon fiber, carbon nano-tube, sawdust, wood powder, bamboo carbon powder, cornstalk, cellulose, peanut shell, carbon aerogels, starch, sucrose, ethyl phosphonic acid ester, polypropylene glycol, polyacrylamide, polypropylene ether, polystyrene, polyvinylether, Merlon or polymethyl methacrylate;
(3) at N 2under atmosphere, in the solution of step (2), drip precipitation reagent and complexing agent simultaneously, simultaneously with 800 ~ 1200 revs/min of stirrings, keep 40 ~ 70 ℃ of reaction temperatures, keep the pH value 9 ~ 13 of reaction system, precipitation has formed rear continuation and has kept stirring 1 ~ 3 hour;
(4) precipitation and the solution that in step (3), form are transferred in water heating kettle, compactedness is 60 ~ 90 %, and under 100 ~ 280 ℃ of thermal and hydric environments, hot high pressure reaction is 6 ~ 40 hours;
(5) sedimentation and filtration in step (4) is cleaned, filter cake is dried to obtain oxidation of precursor nickel manganese cobalt; Press positive electrode component ratio, presoma and lithium salts are mixed in batch mixer; At 200 ~ 400 ℃, preheating is 2 ~ 12 hours, is warming up to 600 ~ 1000 ℃ of calcinings 2 ~ 15 hours, obtains the LiNi of nanoscale stratiform structure after cooling grinding 1/3mn 1/3co 1/3o 2.
2. preparation method as claimed in claim 1, is characterized in that, nickel salt used is nickel acetate, nickel nitrate or nickel oxalate.
3. preparation method as claimed in claim 1, is characterized in that, manganese salt used is manganese acetate, manganese nitrate or manganese oxalate.
4. preparation method as claimed in claim 1, is characterized in that, cobalt salt used is cobalt acetate, cobalt nitrate or cobalt oxalate.
5. preparation method as claimed in claim 1, is characterized in that, lithium salts used is lithium acetate, lithium nitrate, lithium oxalate, lithium formate, lithium nitrite or lithium citrate.
6. preparation method as claimed in claim 1, is characterized in that, complexing agent used is urea or ammoniacal liquor.
7. preparation method as claimed in claim 1, is characterized in that, precipitation reagent used is lithium hydroxide or NaOH, and itself and the total mol ratio of nickel ion+manganese ion+cobalt ions are 2 ~ 4, and the mol ratio of complexing agent and precipitation reagent is 0.1 ~ 2.
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