CN104362338A - Fe-doped lithium ion cathode material and preparation method thereof - Google Patents

Fe-doped lithium ion cathode material and preparation method thereof Download PDF

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Publication number
CN104362338A
CN104362338A CN201410474023.6A CN201410474023A CN104362338A CN 104362338 A CN104362338 A CN 104362338A CN 201410474023 A CN201410474023 A CN 201410474023A CN 104362338 A CN104362338 A CN 104362338A
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preparation
lithium ion
solution
doped
precipitation
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不公告发明人
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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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • 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
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/582—Halogenides
    • 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 invention discloses a Fe-doped lithium ion cathode material and its preparation method. By a coprecipitation method, LiNO3, Co(NO3)2 and FeCl2 which are used as raw materials at the mole ratio of 1:(1-x):x are solved in an ethanol solution; the solution is then added drop by drop into a NaOH ethanol solution at the speed of one drip/second, and filtration is carried out to isolate a precipitate when a reaction is fully carried out and no precipitate is generated; the isolated precipitate spreads out and is dried at 80 DEG C for 10h, and the dried precipitate is calcined at 400-800 DEG C in the air; and finally, the calcined precipitate is ground to obtain the final product. The preparation method has advantages as follows: quantity ratio can accurately be controlled; purity of the product is high; calcinations temperature is low; constituents of the synthetic product are uniform; conditions are easy to control; and operation is simple.

Description

Lithium ion anode material of a kind of doped F e and preparation method thereof
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries and preparation method thereof, particularly the cell positive material and preparation method thereof of doped F e.
Background technology
At occurring in nature, elemental lithium is the lightest metal, and its atomic weight is 6.94g/mol, ρ=0.53g/cm 3, electrochemical equivalent is minimum, is 0.26 gAh -1standard electrode potential is the most negative, for-3.045 V, it is a kind of material with very high-energy-density that these features of elemental lithium determine it, lithium ion battery is exactly this characteristic utilizing elemental lithium, lithium ion battery is a kind of rechargeable battery, and main dependence lithium ion between a positive electrode and a negative electrode movement carrys out work.In charge and discharge process, Li +come and go between two electrodes and embed and deintercalation, during rechargable battery, Li +from positive pole deintercalation, embed negative pole through electrolyte, negative pole is in rich lithium state; Then contrary during electric discharge.Lithium ion battery gains great popularity because of advantages such as its voltage are high, energy density is high, have extended cycle life, environmental pollution is little, but along with the fast development of electronic information technology, it is also proposed higher requirement to the performance of lithium ion battery.
The selection of material is the first element affecting performance of lithium ion battery.From material angle, cycle performance factor the further developing restriction lithium battery of material, in the cyclic process of battery, may be on the one hand that changes in crystal structure is too fast thus cannot continue embedding lithium and take off lithium in cyclic process, may be that the SEI film that cannot generate dense uniform due to active material and corresponding electrolyte causes active material and electrolyte too early side reaction to occur and make the too fast consumption of electrolyte and then affect to circulate on the one hand.Therefore developing high performance electrode material is the key improving battery performance.
Anode material for lithium-ion batteries common at present mainly contains cobalt acid lithium, the LiMn2O4 of spinel structure and the LiFePO4 of olivine structural of layer structure.Business-like lithium ion battery mainly adopts LiCoO 2as positive electrode, LiCoO 2there is fail safe and overcharge resistance performance problem, Co belongs to scarce resource, expensive, and metallic cobalt is easily to environment, its development space is restricted, decrease the scope of application of boring series lithium ion battery to a great extent, therefore the features such as the good cycle performance of cobalt acid lithium are fully utilized, fully by the composite lithium-inserting oxide that the method synthesis multielements such as molecular level mixing, doping, coated and finishing are collaborative, the content of electrode material Co can be reduced, and adopt doped with metal elements, can to LiCoO 2lattice structure play certain support and stabilization, the phase transformation of effective suppression cell configuration in charge and discharge process and subsiding, to reach the object of the safety, cycle performance and the discharge platform that improve material, therefore the lithium ion anode material of a kind of doped F e has better development prospect.
Summary of the invention
The object of this invention is to provide a kind of anode material for lithium-ion batteries and preparation method thereof.
For realizing this purpose, the present invention is achieved through the following technical solutions:
Adopt coprecipitation legal system for the lithium ion anode material of a kind of doped F e.
Lithium ion anode material of a kind of doped F e and preparation method thereof, comprises the steps:
(1) with LiNO 3, Co (NO 3) 2and FeCl 2for raw material is by 1:(1-x): the mol ratio of x is dissolved in ethanolic solution, does not stop to shake up;
(2) getting appropriate NaOH pressed powder is dissolved in another part of ethanolic solution, does not stop to shake up;
(3) the solution of joining in is (1) added drop-wise to the speed of 1 drop/sec in the NaOH ethanolic solution (2), and constantly stirs and react fully;
(4), until (3) middle solution is not when producing precipitation, stopping instills;
(5) static a period of time, the solution in (4) by filtering to isolate precipitation;
Will (5) in isolated precipitation to spread out and at 80 DEG C of dry 10h;
(7) drier postprecipitation in is (6) placed in air 400-800 DEG C of calcining;
(8) namely gained solid abrasive after calcining is obtained final products.
The present invention has following advantages and characteristic;
(1) amount is than can accurately control, and product purity is high;
(2) gained presoma particle diameter is little, and mixes;
(3) calcining heat is lower, and synthetic product component is even;
(4) favorable reproducibility, condition easily controls, simple to operate.
Embodiment
Embodiment one:
Get a certain amount of LiNO respectively 3, Co (NO 3) 2and FeCl 2powder, is dissolved in ethanolic solution by the mol ratio of 1:0.3:0.7, is mixed with the solution that metal ion concentration is 3mol/L; Separately getting appropriate NaOH pressed powder is dissolved in another part of ethanolic solution, be made into the NaOH ethanolic solution of 3mol/L, joined solion is added drop-wise in NaOH ethanolic solution with the speed of 1 drop/sec, and constantly stirring reacts fully, mixing speed is 60r/min again; Until solution not when producing precipitation, stop instillation and static a period of time, solution is filtered to isolate precipitation, and isolated precipitation is spread out and at 80 DEG C of dry 10h, is placed in air again 400 DEG C of calcinings after drying; Namely gained solid abrasive after calcining is obtained final products.
Embodiment two:
Get a certain amount of LiNO respectively 3, Co (NO 3) 2and FeCl 2powder, is dissolved in ethanolic solution by the mol ratio of 1:0.5:0.5, is mixed with the solution that metal ion concentration is 3mol/L; Separately getting appropriate NaOH pressed powder is dissolved in another part of ethanolic solution, be made into the NaOH ethanolic solution of 3mol/L, joined solion is added drop-wise in NaOH ethanolic solution with the speed of 1 drop/sec, and constantly stirring reacts fully, mixing speed is 80r/min again; Until solution not when producing precipitation, stop instillation and static a period of time, solution is filtered to isolate precipitation, and isolated precipitation is spread out and at 80 DEG C of dry 10h, is placed in air again 600 DEG C of calcinings after drying; Namely gained solid abrasive after calcining is obtained final products.
Embodiment three:
Get a certain amount of LiNO respectively 3, Co (NO 3) 2and FeCl 2powder, is dissolved in ethanolic solution by the mol ratio of 1:0.7:0.3, is mixed with the solution that metal ion concentration is 3mol/L; Separately getting appropriate NaOH pressed powder is dissolved in another part of ethanolic solution, be made into the NaOH ethanolic solution of 3mol/L, joined solion is added drop-wise in NaOH ethanolic solution with the speed of 1 drop/sec, and constantly stirring reacts fully, mixing speed is 100r/min again; Until solution not when producing precipitation, stop instillation and static a period of time, solution is filtered to isolate precipitation, and isolated precipitation is spread out and at 80 DEG C of dry 10h, is placed in air again 800 DEG C of calcinings after drying; Namely gained solid abrasive after calcining is obtained final products.

Claims (4)

1. the lithium ion anode material and preparation method thereof of a doped F e, it is characterized in that, this preparation method carries out according to the following steps:
(1) with LiNO 3, Co (NO 3) 2and FeCl 2for raw material is by 1:(1-x): the mol ratio of x is dissolved in ethanolic solution, does not stop to shake up;
(2) getting appropriate NaOH pressed powder is dissolved in another part of ethanolic solution, does not stop to shake up;
(3) the solution of joining in is (1) added drop-wise to the speed of 1 drop/sec in the NaOH ethanolic solution (2), and constantly stirs and react fully;
(4), until (3) middle solution is not when producing precipitation, stopping instills;
(5) static a period of time, the solution in (4) by filtering to isolate precipitation;
(6) inciting somebody to action isolated precipitation (5) spreads out at 80 DEG C of dry 10h;
(7) more dried precipitation in is (6) placed in air to calcine;
(8) namely gained solid abrasive after calcining is obtained final products.
2. the lithium ion anode material and preparation method thereof of a kind of doped F e according to claim 1, is characterized in that, step (1) in X value scope be 0.3≤X≤0.7.
3. the lithium ion anode material and preparation method thereof of a kind of doped F e according to claim 1, is characterized in that, step (3) in adopt agitating mode to be mechanical agitation, mixing speed is 60-100 r/min.
4. the lithium ion anode material and preparation method thereof of a kind of doped F e according to claim 1, is characterized in that, step (7) in institute's calcining heat control within the scope of 400-800 DEG C.
CN201410474023.6A 2014-09-17 2014-09-17 Fe-doped lithium ion cathode material and preparation method thereof Pending CN104362338A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1417874A (en) * 2002-11-28 2003-05-14 清华大学 Prepn of high-rate lithium ion battery cathode material
US20050118505A1 (en) * 1998-07-13 2005-06-02 Ngk Insulators, Ltd. Lithium secondary battery
CN103570082A (en) * 2012-08-01 2014-02-12 北京当升材料科技股份有限公司 Preparation method of lithium cobaltate
CN103682326A (en) * 2013-12-13 2014-03-26 南通瑞翔新材料有限公司 High-capacity lithium cobalt oxide-base lithium ion battery anode material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050118505A1 (en) * 1998-07-13 2005-06-02 Ngk Insulators, Ltd. Lithium secondary battery
CN1417874A (en) * 2002-11-28 2003-05-14 清华大学 Prepn of high-rate lithium ion battery cathode material
CN103570082A (en) * 2012-08-01 2014-02-12 北京当升材料科技股份有限公司 Preparation method of lithium cobaltate
CN103682326A (en) * 2013-12-13 2014-03-26 南通瑞翔新材料有限公司 High-capacity lithium cobalt oxide-base lithium ion battery anode material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
N. KALAISELVI ET AL: "Iron Doped Lithium Cobalt Oxides as Lithium Intercalating Cathode Materials", 《IONICS》 *

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Application publication date: 20150218