CN1194430C - Prepn of high-rate lithium ion battery cathode material - Google Patents

Prepn of high-rate lithium ion battery cathode material Download PDF

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Publication number
CN1194430C
CN1194430C CNB021491771A CN02149177A CN1194430C CN 1194430 C CN1194430 C CN 1194430C CN B021491771 A CNB021491771 A CN B021491771A CN 02149177 A CN02149177 A CN 02149177A CN 1194430 C CN1194430 C CN 1194430C
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cathode material
lithium ion
ion battery
battery
lithium
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Expired - Fee Related
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CNB021491771A
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CN1417874A (en
Inventor
邱新平
陈海龙
朱文涛
何志奇
梁宏莹
陈立泉
诸学农
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SHIJI BONA ENERGY SOURCE TECHNOLOGY Co Ltd BEIJING CITY
Tsinghua University
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SHIJI BONA ENERGY SOURCE TECHNOLOGY Co Ltd BEIJING CITY
Tsinghua University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The present invention discloses a preparation method for the cathode material of a lithium ion battery with high rate, which belongs to the preparation technology of battery materials. The organic polar solvent of various kinds of soluble lithium salt, soluble cobalt salt, soluble nickel salt and the like is used, and the organic solvent of solution and hydroxide is dried and ground in a coprecipitation way, so that nanoscale cathode material granules are obtained. After the granules are mixed with black carbon and polyvinylidene fluoride proportionally, the solvent is added, and flaky cathode material is prepared by casting technology and is filled in a battery. Cycle discharging characteristic tests indicate that the cathode material maintains the main advantages of high voltage and high capacity of a lithium battery, has the obvious characteristics of long cycle life and good safety performance, and has extensive application prospects and tremendous potential economic benefits on multiple aspects, such as portable electronic equipment, electric automobiles, space technology, national defence industry, etc. The granules can be multitudinously and quickly synthesized into various nanoscale cathode materials with low cost. A lithium ion battery can be charged and discharged at super high speed through the novel cathode material. The cathode material has great significance to the application of the lithium ion battery in devices with large power.

Description

A kind of two-forty cathode material for lithium ion battery preparation method
Technical field
The invention belongs to the battery material technology of preparing, particularly a kind of two-forty cathode material for lithium ion battery preparation method of energy quickly synthesizing nano grade particles.
Background technology
In the lithium ion battery industry, the high power electrokinetic cell of developing means of transportations such as can be used for electric automobile and large electric appliances is a focus always, and how to improve the lithium ion battery charge-discharge velocity and keep certain cycle life and capacity, be key issue wherein.The anode material that has outstanding two-forty performance at present is not rarely seen, and the research of the cathode material of two-forty does not also have phasic results, and this is the restraining factors that improve entire lithium ion battery system charge-discharge velocity.
Summary of the invention
The purpose of this invention is to provide a kind of two-forty cathode material for lithium ion battery preparation method, it is characterized in that described cathode material for lithium ion battery is with lithium salts, hydroxide and solvent, obtain with non-aqueous system co-precipitation synthetic method, its preparation process is:
1. soluble lithium salt or other ease of solubility salt are dissolved in and obtain solution A in the polar organic solvent;
2. with NaOH, be dissolved in the organic solvent, obtain solution B;
3. then solution B is splashed in the solution A under intense mechanical stirring and supersonic oscillations, obtain viscous mixture, after 10～24 hours leave standstill, use supercentrifuge that sediment is separated;
4. through 120 ℃, 24 hours is 10 in vacuum degree -1To 10 -2Torr grinds after drying down, obtains brown loose reacting precursor;
5. precursor carries out calcining in 2～24 hours and obtains the black solid product under the different temperatures in muffle furnace;
6. with product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, 120 ℃, grind behind the vacuum drying, finally obtain the lithium ion battery cathode nano-particle material.
Described soluble lithium salt comprises LiNO 3, LiCl, LiClO 4
Co salt, Ni salt, Mn salt, its Co, Ni that described other ease of solubility salt are ease of solubility are nitrate, and Mn is a chloride.
Described polar organic solvent comprises alcohols such as ethanol, ethylene glycol, propyl alcohol, isopropyl alcohol and oxolane (THF), methyl-sulfoxide (DMSO) and carbonic ester.
Beneficial effect of the present invention 1. uses organic polar solvent, lithium salts and hydroxide, utilizes non-aqueous system co-precipitation synthetic method to obtain the cathode material of multiple nano particle, as LiCoO 2, LiNiO 2, LiMn 2O 4, LiMnO 2, LiFePO 4, V 2O 5, LiM xN 1-xO 2(M=Al, Mg, Ti etc., N=Ni, Co, Mn), Li (Ni xMn yCo z) O 2Or the like, use growing up of strong mechanical agitation and supersonic oscillations control particle in the course of reaction, obtain the grain shape homogeneous, narrow diameter distribution, all below 100nm, phase constituent is single, and degree of crystallinity is good; 2. the material firing temperature is compared with conventional method also with the time and is reduced significantly.3. through systematically testing its two-forty cycle charge discharge electrical property, its performance is better than the conventional cathode material greatly.LiCoO 2High charge speed be 50 times of present common lithium ion battery.Its circulation volume is also than higher, and high discharge capacity reaches 160mA.h/g.Use the lithium ion battery of this cathode material, can realize discharging and recharging at a high speed, as in 5 minutes, being full of capacity or in 1 minute, being full of 80% capacity.And electric automobile, space flight device, fields such as ultracapacitor might be applied in the future.
Description of drawings
Fig. 1 is the X light powder diffraction spectrogram of embodiment 1 product;
Fig. 2 is the two-forty cycle charge-discharge test curve of the lithium ion battery of use the inventive method gained cathode material.
Embodiment
Embodiment one:
Accurate weighing 0.1mol LiNO 3, 0.1mol Co (NO 3) 2, be dissolved in the 100ml absolute ethyl alcohol and obtain solution A; In addition accurate weighing 0.3molNaOH is dissolved in the 100ml absolute ethyl alcohol, obtains solution B, then solution B is splashed in the solution A under intense mechanical stirring and supersonic oscillations, obtains viscous mixture.After 24 hours leave standstill, use supercentrifuge that precipitate and separate is come out, through 120 ℃, behind 24 hours vacuum dryings, grind, obtain brown loose reacting precursor.Precursor obtains the black solid product 400 ℃ of calcinings in following 10 hours in muffle furnace.With product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, 120 ℃ is 10 in vacuum degree -2Grind behind the vacuum drying under the torr, obtain end product LiCoO 2Its particle is through transmission electron microscope, and ESEM, XRD analysis, particle diameter are the sheet-like particle of shape homogeneous less than 80nm, and phase constituent is single.Its XRD (X light powder diffraction) spectrum as shown in Figure 1.
Embodiment two
With embodiment one obtain brown loose reacting precursor in atmosphere sintering furnace 600 ℃ of temperature, carry out calcining in 5 hours under the oxygen atmosphere and obtain the black solid product.With product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, 120 ℃ is 10 in vacuum degree -2Grind behind the vacuum drying under the torr, obtain end product LiNiO 2The product particle is through transmission electron microscope, and ESEM and XRD analysis, its particle diameter are the square particle of shape homogeneous less than 30nm.
Embodiment three
Obtaining brown loose reacting precursor with embodiment one carries out calcining in 10 hours and obtains the black solid product under 500 ℃ of temperature in muffle furnace.With product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, 120 ℃ is 10 in vacuum degree -2Grind behind the vacuum drying under the torr, obtain end product.Its particle is through transmission electron microscope, and ESEM, XRD analysis, particle diameter are the sheet-like particle of shape homogeneous less than 80nm, and phase constituent is single.
According to mass ratio ratio weighing in 6: 3: 1 product powder and carbon black, Kynoar (PVDF), PVDF is dissolved in a certain amount of N-methyl pyrrolidone (NMP), then the product powder is mixed the back in carbon black and add, stir (600 rev/mins) through 24 hours high speed machines and obtain uniform sizing material.Adopt The tape casting to be coated on the metal aluminum foil surface of cleaning in slurry, edge of a knife control wet-film thickness is less than 1mm.Wet film 140 ℃ of oven dry, through the pressurization of stainless steel roll, is obtained dry film then.With the dry film dicing, through behind 180 ℃ of vacuum dryings in the argon gas atmosphere glove box and metal lithium sheet, electrolyte and barrier film are assembled into battery.Battery is carried out two-forty cycle charge discharge electrical testing on the comprehensive electrochemical test of Solartron1287.Test result as shown in Figure 2
Embodiment four
Obtain brown loose reacting precursor in muffle furnace with embodiment one, under 600 ℃ of temperature, carry out calcining in 10 hours and obtain the black solid product.With product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, 120 ℃ is 10 in vacuum degree -2Grind behind the vacuum drying under the torr, obtain end product LiCoO 2According to mass ratio ratio weighing in 6: 3: 1 product powder and carbon black, Kynoar (PVDF), PVDF is dissolved in a certain amount of N-first class pyrrolidones (NMP), then the product powder is mixed the back in carbon black and add, stir (600 rev/mins) through 24 hours high speed machines and obtain uniform sizing material.Adopt The tape casting to be coated on the metal aluminum foil surface of cleaning in slurry, edge of a knife control wet-film thickness is less than 1mm.Wet film 140 ℃ of oven dry, through the pressurization of stainless steel roll, is obtained dry film then.With the dry film dicing, through behind 180 ℃ of vacuum dryings in the argon gas atmosphere glove box and metal lithium sheet, electrolyte and barrier film are assembled into battery.Battery is carried out two-forty cycle charge discharge electrical testing on the comprehensive electrochemical test of solartran1287, test result as shown in Figure 2
Embodiment five
Obtaining brown loose reacting precursor with embodiment one carries out calcining in 10 hours and obtains the black solid product under 600 ℃ of temperature in muffle furnace.With product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, weighing product powder and carbon black, Kynoar (PVDF), PVDF is dissolved in a certain amount of N-first class pyrrolidones (NMP), then the product powder is mixed the back in carbon black and add, stir (600 rev/mins) through 24 hours high speed machines and obtain uniform sizing material.Adopt The tape casting to be coated on the metal aluminum foil surface of cleaning in slurry, edge of a knife control wet-film thickness is less than 1mm.Wet film 140 ℃ of oven dry, through the pressurization of stainless steel roll, is obtained dry film then.With the dry film dicing,, be 10 in vacuum degree through 180 ℃ -2Under the torr behind the vacuum drying in the argon gas atmosphere glove box and metal lithium sheet, electrolyte and barrier film are assembled into battery.Battery is carried out two-forty cycle charge discharge electrical testing on the comprehensive electrochemical test of solartran1287, test result as shown in Figure 2.
Embodiment six
Accurate weighing 0.3mol LiNO 3, 0.1mol Ni (NO 3) 2, 0.1mol MnCl 2, 0.1molCo (NO 3) 2, be dissolved in the 200ml absolute ethyl alcohol and obtain solution A.In addition accurate weighing 0.9molNaOH is dissolved in the 200ml absolute ethyl alcohol, obtains solution B. and then solution B is splashed in the solution A under intense mechanical stirring and supersonic oscillations, obtain viscous mixture.After a period of time leaves standstill, use supercentrifuge that precipitate and separate is come out, through 120 ℃, behind 24 hours vacuum dryings, grind, obtain brown loose reacting precursor.Precursor carries out calcining in 5 hours and obtains the black solid product under 600 ℃ of temperature in muffle furnace.With product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, 120 ℃ is 10 in vacuum degree -2Grind behind the vacuum drying under the torr, obtain end product Li (Ni 1/3Co 1/3Mn1/ 3) O 2According to mass ratio ratio weighing in 6: 3: 1 product powder and carbon black, Kynoar (PVDF), PVDF is dissolved in a certain amount of N-first class pyrrolidones (NMP), then the product powder is mixed the back in carbon black and add, stir (600 rev/mins) through 24 hours high speed machines and obtain uniform sizing material.Adopt The tape casting to be coated on the metal aluminum foil surface of cleaning in slurry, edge of a knife control wet-film thickness is less than 1mm.Wet film 140 ℃ of oven dry, through the pressurization of stainless steel roll, is obtained dry film then.With the dry film dicing,, be 10 in vacuum degree through 180 ℃ -2Under the torr behind the vacuum drying in the argon gas atmosphere glove box and metal lithium sheet, electrolyte and barrier film are assembled into battery.Battery is carried out two-forty cycle charge discharge electrical testing on the comprehensive electrochemical test of solartran1287, test result as shown in Figure 2.
Comparative example:
Weighing 0.1molCo 2O 3, 0.1mol LiOH.H 2O mixes the back and grinds, and with mixture 750 ℃ of temperature lower calcinations 24 hours in muffle furnace, grind product cooling back, and 750 ℃ of calcinings are 10 hours once more.Grind once more.According to mass ratio ratio weighing in 6: 3: 1 product powder and carbon black, Kynoar (PVDF), PVDF is dissolved in a certain amount of N-first class pyrrolidones (NMP), then the product powder is mixed the back in carbon black and add, stir (600 rev/mins) through 24 hours high speed machines and obtain uniform sizing material.Adopt The tape casting to be coated on the metal aluminum foil surface of cleaning in slurry, edge of a knife control wet-film thickness is less than 1mm.Wet film 140 ℃ of oven dry, through the pressurization of stainless steel roll, is obtained dry film then.With the dry film dicing,, be 10 in vacuum degree through 180 ℃ -2Under the torr behind the vacuum drying in the argon gas atmosphere glove box and metal lithium sheet, electrolyte and barrier film are assembled into battery.Battery is carried out two-forty cycle charge discharge electrical testing on the comprehensive electrochemical test of solartran1287.Its test result as shown in Figure 2.
Figure 2 shows that different materials, the two-forty cycle charge discharge electrical testing comparison curves of the lithium ion battery of the cathode material of different disposal parameter gained is best with embodiment three, and discharge capacity height, cycle period are long, stable performance.

Claims (2)

1. a two-forty cathode material for lithium ion battery preparation method is characterized in that described cathode material for lithium ion battery is with lithium salts, hydroxide and solvent, obtains with non-aqueous system co-precipitation synthetic method, and its preparation process is:
1. with lithium salts LiNO 3, LiCl or LiClO 4And in the chloride of the nitrate of Co, Ni, Mn one or more are dissolved in and obtain solution A in the organic solvent;
2. with NaOH, be dissolved in the organic solvent, obtain solution B;
3. then solution B is splashed in the solution A under intense mechanical stirring and supersonic oscillations, obtain viscous mixture, after 10～24 hours leave standstill, use supercentrifuge that sediment is separated;
4. through 120 ℃, 24 hours, 10 -1To 10 -2After the oven dry, grind in the torr vacuum, obtain brown loose reacting precursor;
5. precursor carries out calcining in 2～24 hours respectively and obtains the black solid product under 400 ℃, 500 ℃ or 600 ℃ of temperature in muffle furnace;
6. with product with washed with de-ionized water to PH=8, use the ethanol cleaning and dewatering again, 120 ℃, grind behind the vacuum drying, finally obtain the lithium ion battery cathode nano-particle material.
2. according to the described two-forty cathode material for lithium ion battery of claim 1 preparation method, it is characterized in that: described organic solvent is selected from ethanol, ethylene glycol, propyl alcohol, isopropyl alcohol, oxolane, methyl-sulfoxide or carbonic ester.
CNB021491771A 2002-11-28 2002-11-28 Prepn of high-rate lithium ion battery cathode material Expired - Fee Related CN1194430C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8377509B2 (en) * 2006-02-28 2013-02-19 Primet Precision Materials, Inc. Lithium-based compound nanoparticle compositions and methods of forming the same
CN104157830A (en) * 2014-07-06 2014-11-19 魏斌 Novel LiCo(1-x)AlxO2 electrode material and preparation method thereof
CN104167539A (en) * 2014-07-06 2014-11-26 魏斌 A novel LiCo<1-x>Sn<x>O2 electrode material and a preparing method thereof
CN104362337A (en) * 2014-09-17 2015-02-18 陈虹 LiCo1-xZnxO2 electrode material and preparation method thereof
CN104362338A (en) * 2014-09-17 2015-02-18 陈虹 Fe-doped lithium ion cathode material and preparation method thereof
CN104319382A (en) * 2014-09-18 2015-01-28 陈虹 Multicomponent alloy LiCo1-xTixO2 electrode material and preparation method thereof
CN104269518A (en) * 2014-09-20 2015-01-07 陈虹 Multicomponent transition metal oxide composite electrode material and preparation method thereof
CN104269519A (en) * 2014-09-20 2015-01-07 陈虹 Cu doped LiCo(1-x)CuxO2 electrode material and preparation method thereof

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