CN105024065A - Lithium ion battery cathode material and preparation method thereof - Google Patents

Lithium ion battery cathode material and preparation method thereof Download PDF

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Publication number
CN105024065A
CN105024065A CN201510378734.8A CN201510378734A CN105024065A CN 105024065 A CN105024065 A CN 105024065A CN 201510378734 A CN201510378734 A CN 201510378734A CN 105024065 A CN105024065 A CN 105024065A
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lithium
raw material
cobalt
nickel
preparation
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刘兴泉
熊伟强
赵红远
陈炳
张峥
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University of Electronic Science and Technology of China
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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
    • H01M4/36—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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention belongs to the field of a lithium ion battery, and provides a doped and modified layered lithium ion battery cathode material LiNi<1-x-y>CoxAlyO2 and a preparation method thereof, wherein x is more than 0 and less than or equal to 0.2, y is more than or equal to 0 and less than or equal to 0.1, and (x+y) is more than 0 and less than or equal to 0.3. The lithium ion battery cathode material LiNi<1-x-y>CoxAlyO2 is obtained by simultaneously doping trivalent elemental aluminum and divalent element cobalt to replace elemental nickel in the cathode material. The cathode material is endowed with high discharging specific capacity and excellent cyclic stability performance, and the high-rate charging and discharging demand can be met; parallel flow and co-precipitation of four solutions combined with a solid-phase synthesis method are used for preparing the cathode material; and by the method, the defects of long preparation time, difficulty in controlling stoichiometric proportion, non-uniform distribution of product grain sizes, poor electrochemical property and the like of the solid-phase synthesis method are overcome, the prepared product is high in purity and high in crystalline quality, high and uniformly-distributed product grain density is achieved, electrochemical property is excellent, and manufacturing cost is low.

Description

A kind of anode material for lithium-ion batteries and preparation method thereof
Technical field
The invention belongs to field of lithium ion battery, relate to anode material for lithium-ion batteries and preparation method thereof, be specially anode material for lithium-ion batteries LiNi 1-x-yco xal yo 2, wherein 0<x≤0.2,0≤y≤0.1,0<x+y≤0.3; And the preparation method of this positive electrode.
Background technology
Along with going from bad to worse and the exhaustion of the resource such as oil of global environment, the research and development of energy-saving and emission-reduction and green energy resource are extremely urgent, all pay much attention to the development & application about new forms of energy and renewable and clean energy resource both at home and abroad.Lithium ion battery is the energy of wherein a kind of more promising novel environmental protection.Owing to having, energy density is high, quickly-chargeable, self discharge are little, can the advantage such as long-time storage, cycle performance is superior, memory-less effect, working temperature are wide, lightweight, lithium ion battery has been widely used on various portable electric appts, is also expected to the power source being applied to electric automobile and hybrid vehicle soon.
The positive electrode being applied to lithium ion battery at present in batches mainly contains cobalt acid lithium (LiCoO 2), lithium nickelate (LiNiO 2), LiFePO4 (LiFePO 4), nickle cobalt lithium manganate and spinel lithium manganate (LiMn 2o 4).Wherein, cobalt acid lithium realizes commercial applications the earliest, have ripe large-scale production technology, and be widely used on lower powered mobile electronic products, but cobalt resource is deficient, expensive, and toxicity is comparatively large not environmentally; The aboundresources of lithium manganate battery manganese, cheap, environmentally safe, deintercalation current potential is high, and power density is comparatively large, but low capacity and unstable cycle performance limit its application; Lithium iron phosphate positive material environment-protecting asepsis, rich in mineral resources, low raw-material cost, temperature tolerance is splendid, stable circulation performance is superior, but its conductivity is poor, and density is little, volume is large, and energy density is low and cryogenic property is not good enough, and its application and development is all restricted.
Lithium nickelate (LiNiO 2) positive electrode and cobalt acid lithium (LiCoO 2) positive electrode is all the material with layer structure, its specific discharge capacity is very high ~ 210mAh/g (LiCoO 2~ 140mAh/g), power density and energy density are large, good electric conductivity, relatively cheap price and lower toxicity, make lithium nickelate positive electrode get a good chance of replace lithium cobaltate cathode material, especially electric automobile and mixed power electric car application prospect better.But lithium nickelate preparation condition is harsh, the not easily product of obtained ideal stoichiometric ratio, electrochemistry cycle performance is poor, thermal stability is poor and have the safety problem of precipitation of oxygen in charging process, limits the process that it is practical.LiNi 1-x-yco xal yo 2it is LiCoO that positive electrode can look at 2, LiNiO 2, LiAlO 2the solid solution of three, it has had LiCoO concurrently 2circulation high stability and the long-life, LiNiO 2height ratio capacity and low cost, LiAlO 2high thermal stability and high security.Three's combination creates this positive electrode and is particularly suitable for manufacturing energy density lithium ion power battery, electric automobile uses and effectively significantly can promote course continuation mileage.
Summary of the invention
The object of the invention is to for lithium ion battery anode material nickel acid lithium (LiNiO 2) shortcoming of electrochemistry cycle performance difference, a kind of layered lithium ion battery positive electrode LiNi of doping vario-property is provided 1-x-yco xal yo 2(0<x≤0.2,0≤y≤0.1,0<x+y≤0.3) and preparation method thereof.This modification lithium-ion battery anode material LiNi 1-x-yco xal yo 2there is very high specific discharge capacity and excellent stable circulation performance, high rate charge-discharge demand can be met, its preparation method overcomes solid-phase synthesis preparation time length, is difficult to control stoichiometric proportion, the shortcomings such as particle size skewness and chemical property difference, the product purity of preparation is high, crystalline quality is high, product grain density is large and be evenly distributed, electrochemical performance and low cost of manufacture.
For achieving the above object, the technical solution used in the present invention is: a kind of anode material for lithium-ion batteries, is characterized in that, the molecular structure expression formula of described positive electrode is: LiNi 1-x-yco xal yo 2, wherein, 0<x≤0.2,0≤y≤0.1,0<x+y≤0.3.
Further, the molecular structure expression formula of described positive electrode is LiNi 0.8co 0.15al 0.05o 2or LiNi 0.75co 0.20al 0.05o 2.
The preparation method of described anode material for lithium-ion batteries, comprises the following steps:
Step 1. is according to mol ratio nickel source and aluminium source raw material are dissolved in appropriate amount of deionized water, join to obtain solution A, wherein, 0<x≤0.2,0≤y≤0.1,0<x+y≤0.3;
Step 2. is according to mol ratio cobalt source and aluminium source raw material are dissolved in appropriate amount of deionized water, join to obtain solution B;
NaOH is dissolved in appropriate amount of deionized water by step 3., joins to obtain solution C, and the solution concentration of NaOH is 4mol/L;
Step 4. by concentrated ammonia liquor by volume 1: 1 ratio be dissolved in appropriate amount of deionized water, join to obtain solution D, wherein, concentrated ammonia liquor consumption is mol ratio NH 3: (Ni+Co+Al)=2.47:1;
Step 5. by solution A, B, C, D stream add N 2protection also carries out co-precipitation in the reactor constantly stirred, and controls solution flow rate and four kinds of solution are added simultaneously, and control reactor temperature at 50-80 DEG C; The pH value adding rear adjustment reactive tank material is 11.0;
Step 6. by the still aging 12h of step 5 gained co-precipitation liquid, by ageing liquid filter and repeatedly washing after, vacuumize 24h at 105 DEG C;
Dry for step 6 gained presoma fully mixes with lithium source by step 7., and compressing, and wherein, the mol ratio of lithium source raw material, nickel source raw material, cobalt source raw material and aluminium source raw material is (1.05 ~ 1.15): (1-x-y): x: y;
Step 8. by compressing for step 7 gained material pre-burning 4h ~ 8h at 450 ~ 550 DEG C, then sinters 16h ~ 24h under oxygen flow, and sintering temperature is 690 DEG C ~ 820 DEG C, namely obtains target product LiNi 1-x-yco xal yo 2, wherein, 0<x≤0.2,0≤y≤0.1,0<x+y≤0.3.
In the present invention, in described step 5, mixing speed is 600rpm; In step 8, oxygen flow flow velocity is 200mL/min.
In the present invention, described lithium source raw material is at least one in lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate, lithium citrate, lithium oxalate;
Described nickel source raw material is at least one in nickel nitrate, nickelous sulfate, nickel oxide, nickel chloride, nickel hydroxide, nickel acetate;
Described cobalt source raw material is at least one in cobalt nitrate, cobaltous sulfate, cobalt oxide, cobalt chloride, cobalt hydroxide, cobalt acetate;
Described aluminium source raw material is at least one in aluminum nitrate, aluminium oxide, aluminum sulfate, aluminium chloride, aluminum trifluoride, aluminum phosphate.
The present invention obtains anode material for lithium-ion batteries LiNi by the elemental nickel (Ni) that doping triad aluminium (Al) and diad cobalt (Co) replace in positive electrode simultaneously 1-x-yco xal yo 2(0<x≤0.2,0≤y≤0.1,0<x+y≤0.3) is especially LiNi 0.8co 0.15al 0.05o 2and LiNi 0.75co 0.20al 0.05o 2.Aluminium is III Main Group Metal Elements, and its valence state is+3 valencys, and the trivalent aluminium ion nickel element replaced in positive electrode can improve the thermal stability of positive electrode; Cobalt is the transition metal close with nickel, its valence state is+divalent, and the introducing of cobalt ions can improve the structure of nickel system layered cathode material and reduce the difficulty of preparation, improves the structural stability of nickel system positive electrode, improve conductivity, increase the cycle life of positive electrode.
The present invention adopts four kinds of solution co-precipitations to prepare anode material for lithium-ion batteries LiNi in conjunction with solid-phase synthesis 1-x-yco xal yo 2(0<x≤0.2,0≤y≤0.1,0<x+y≤0.3), compared with pure solid-phase synthesis, four kinds of solution co-precipitations are simple in conjunction with the preparation technology of solid-phase synthesis, the time of sintering significantly shortens, the temperature of sintering obviously reduces, and therefore energy consumption significantly reduces, and product has good spherical morphology, easy to use and processing applies, and is convenient to suitability for industrialized production application.
In sum, invention effect of the present invention is:
1, the present invention adopts four kinds of solution co-precipitation methods, Ni in the process of reaction 2+, Co 2+, Al 3+at the uniform velocity co-precipitation is there is, Ni in precipitation process with aqueous slkali 2+, Co 2+, Al 3+solubility remain constant; Only need after four kinds of solution all add simultaneously, Ni 2+, Co 2+, Al 3+solubility just gradually uniform descent until precipitation completely; The speed of precipitation is controlled by ammoniacal liquor complexing agent, Ni in reaction raw materials in coprecipitation process 2+, Co 2+, Al 3+ion fully precipitates, and overcomes the shortcoming of conventional solid synthetic method and conventional coprecipitation method, the product crystalline quality of preparation is excellent, chemical composition close to theoretical value, product phase purity is high, layer structure is excellent.
2, the layered lithium ion battery positive electrode LiNi for preparing of the present invention 1-x-yco xal yo 2in (0<x≤0.2,0≤y≤0.1,0<x+y≤0.3), doping+divalent metallic cobalt element ,+3 valency aluminium elements, fully by means of the advantage of each doped chemical, can improve the combination property of positive electrode; There is very high specific discharge capacity and more excellent stable circulation performance, be applicable to the demand of electric automobile high-energy-density, high power discharge; Especially anode material for lithium-ion batteries LiNi 0.8co 0.15al 0.05o 2under room temperature environment, when constant current charge-discharge multiplying power is 0.2C, when voltage range is 2.75-4.3V, the first discharge specific capacity of this lithium ion battery positive electrode material in layer structure can reach 217.5mAh/g, circulate after 30 times, specific discharge capacity still can reach 194.5mAh/g, and capability retention is 90%.
3, in technique of the present invention, reaction raw material used are all general chemical products, and comparatively horn of plenty of originating, relative low price, manufacturing cost is lower.
4, in technique of the present invention, device therefor is simple, produces, both met environmental protection concept in preparation process without poisonous and harmful substance, is easy to again to realize large-scale industrial and produces.
Accompanying drawing explanation
Fig. 1 is that the present invention prepares anode material for lithium-ion batteries LiNi 0.8co 0.15al 0.05o 2process chart.
Fig. 2 is that the present invention prepares anode material for lithium-ion batteries LiNi 0.8co 0.15al 0.05o 2xRD figure.
Fig. 3 is that the present invention prepares precursor of lithium ionic cell positive material Ni 0.8co 0.15al 0.05(OH) 2+ δsEM figure.
Fig. 4 is that the present invention prepares anode material for lithium-ion batteries LiNi 0.8co 0.15al 0.05o 2first charge-discharge curve chart under 0.2C multiplying power.
Fig. 5 is that the present invention prepares anode material for lithium-ion batteries LiNi 0.8co 0.15al 0.05o 2cycle performance curve chart under 0.2C multiplying power.
Fig. 6 is that the present invention prepares anode material for lithium-ion batteries LiNi 0.8co 0.15al 0.05o 2coulombic efficiency curve chart under 0.2C multiplying power.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the present invention is described in further detail.
Embodiment
The nickelous sulfate of proportional quantities (0.8mol) and (0.025mol) aluminum nitrate are dissolved in 500mL deionized water, make it dissolve completely and obtain solution A; The cobaltous sulfate of proportional quantities (0.15mol) and (0.025mol) aluminum nitrate are dissolved in 250mL deionized water, make it dissolve completely and obtain solution B; The NaOH of proportional quantities (2.0mol) is dissolved in 500mL fresh deionized water, makes it dissolve completely and obtain solution C; 150ml concentrated ammonia liquor is dissolved in 150mL fresh deionized water, makes it dissolve completely and obtain solution D;
By solution A, B, C, D with certain speed and stream add strong stirring and have N 2carry out co-precipitation in the reactor of protection, control solution flow rate and make four kinds of solution add simultaneously and control reactor temperature at 50-80 DEG C; NaOH solution concentration is 4mol/L, and the pH value adding rear adjustment reactive tank material is about 11.0; Mixing speed is 600rpm; Then the coprecipitate at room temperature ageing 12h will obtained, then filters, with 50 DEG C of deionized water washing multipass, until the Na that can not detect +and SO 4 2-till; Then filter cake is placed in air dry oven 105 DEG C of drying 12 ~ 24h;
By dried presoma with excessive 5 ~ 15% lithium hydroxide (being used as lithium source) to mix with mortar and to grind evenly, compressing by powder compressing machine, then be positioned in tube furnace at 450-550 DEG C of low temperature presintering 4h-8h, finally in oxygen flow, sinter 16-24h at (200mL/min) 690-820 DEG C of temperature, the lithium ion battery target positive electrode LiNi that layer structure is excellent can be obtained 0.8co 0.15al 0.05o 2.
Adopt same method can obtain the excellent lithium ion battery target positive electrode LiNi of layer structure 0.75co 0.20al 0.05o 2.
To the lithium ion battery target positive electrode LiNi of preparation 0.8co 0.15al 0.05o 2carry out constant current charge-discharge test, can find out that this positive electrode has very high specific discharge capacity and comparatively excellent stable circulation performance from test result; Under room temperature environment, when constant current charge-discharge multiplying power is 0.2C, when voltage range is 2.75-4.3V, the first discharge specific capacity of this lithium ion battery positive electrode material in layer structure can reach 217.5mAh/g, circulate after 30 times, specific discharge capacity still can reach 194.5mAh/g, and capability retention is 90%.
The above, be only the specific embodiment of the present invention, arbitrary feature disclosed in this specification, unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object; Step in disclosed all features or all methods or process, except mutually exclusive feature and/or step, all can be combined in any way.

Claims (7)

1. an anode material for lithium-ion batteries, is characterized in that, the molecular structure expression formula of described positive electrode is: LiNi 1-x-yco xal yo 2, wherein, 0<x≤0.2,0≤y≤0.1,0<x+y≤0.3.
2., by anode material for lithium-ion batteries described in claim 1, it is characterized in that, the molecular structure expression formula of described positive electrode is LiNi 0.8co 0.15al 0.05o 2or LiNi 0.75co 0.20al 0.05o 2.
3., by the preparation method of anode material for lithium-ion batteries described in claim 1, comprise the following steps:
Step 1. is according to mol ratio nickel source and aluminium source raw material are dissolved in appropriate amount of deionized water, join to obtain solution A, wherein, 0<x≤0.2,0≤y≤0.1,0<x+y≤0.3;
Step 2. is according to mol ratio cobalt source and aluminium source raw material are dissolved in appropriate amount of deionized water, join to obtain solution B;
NaOH is dissolved in appropriate amount of deionized water by step 3., joins to obtain solution C, and the solution concentration of NaOH is 4mol/L;
Step 4. by concentrated ammonia liquor by volume 1: 1 ratio be dissolved in appropriate amount of deionized water, join to obtain solution D, wherein, concentrated ammonia liquor consumption is mol ratio NH 3: (Ni+Co+Al)=2.47:1;
Step 5. by solution A, B, C, D stream add N 2protection also carries out co-precipitation in the reactor constantly stirred, and controls solution flow rate and four kinds of solution are added simultaneously, and control reactor temperature at 50-80 DEG C; The pH value adding rear adjustment reactive tank material is 11.0;
Step 6. by the still aging 12h of step 5 gained co-precipitation liquid, by ageing liquid filter and repeatedly washing after, vacuumize 24h at 105 DEG C;
Dry for step 6 gained presoma fully mixes with lithium source by step 7., and compressing, and wherein, the mol ratio of lithium source raw material, nickel source raw material, cobalt source raw material and aluminium source raw material is (1.05 ~ 1.15): (1-x-y): x: y;
Step 8. by compressing for step 7 gained material pre-burning 4h ~ 8h at 450 ~ 550 DEG C, then sinters 16h ~ 24h under oxygen flow, and sintering temperature is 690 DEG C ~ 820 DEG C, namely obtains target product LiNi 1-x-yco xal yo 2, wherein, 0<x≤0.2,0≤y≤0.1,0<x+y≤0.3.
4., by the preparation method of anode material for lithium-ion batteries described in claim 3, it is characterized in that, described lithium source raw material is at least one in lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate, lithium citrate, lithium oxalate.
5., by the preparation method of anode material for lithium-ion batteries described in claim 3, it is characterized in that, described nickel source raw material is at least one in nickel nitrate, nickelous sulfate, nickel oxide, nickel chloride, nickel hydroxide, nickel acetate.
6., by the preparation method of anode material for lithium-ion batteries described in claim 3, it is characterized in that, described cobalt source raw material is at least one in cobalt nitrate, cobaltous sulfate, cobalt oxide, cobalt chloride, cobalt hydroxide, cobalt acetate.
7., by the preparation method of anode material for lithium-ion batteries described in claim 3, it is characterized in that, described aluminium source raw material is at least one in aluminum nitrate, aluminium oxide, aluminum sulfate, aluminium chloride, aluminum trifluoride, aluminum phosphate.
CN201510378734.8A 2015-07-02 2015-07-02 Lithium ion battery cathode material and preparation method thereof Pending CN105024065A (en)

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CN105514373A (en) * 2016-01-18 2016-04-20 四川富骅新能源科技有限公司 Positive electrode material of high-capacity lithium ion battery and preparation method of positive electrode material
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CN105336944A (en) * 2015-12-09 2016-02-17 四川富骅新能源科技有限公司 High-capacity cathode material for lithium ion batteries and preparation method thereof
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Application publication date: 20151104