CN103996823A - Rapid microwave reaction preparation method of ternary polyanionic phosphate/carbon cathode material for power lithium ion battery - Google Patents

Rapid microwave reaction preparation method of ternary polyanionic phosphate/carbon cathode material for power lithium ion battery Download PDF

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CN103996823A
CN103996823A CN201410192405.XA CN201410192405A CN103996823A CN 103996823 A CN103996823 A CN 103996823A CN 201410192405 A CN201410192405 A CN 201410192405A CN 103996823 A CN103996823 A CN 103996823A
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phosphate
preparation
lithium
carbon
salt
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CN103996823B (en
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栗欢欢
王亚平
陈龙
江浩斌
李云星
陈依
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Jiangsu 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
    • H01M4/36—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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
    • 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 provides a rapid microwave reaction preparation method of a ternary polyanionic phosphate/carbon cathode material for a power lithium ion battery, comprising the following steps: weighing lithium salt, ferric salt, manganese salt, cobalt salt and phosphate according to the molar ratio of 1-1.1:1/3:1/3:1/3:1 and putting them into a mill pot, adding 7-10wt% of a carbon source, carrying out ball milling for 5-10h, drying, tabletting, and decomposing in an inert atmosphere furnace at 350 DEG C for 1-5h; and grinding, tabletting, and carrying out microwave in a microwave reactor for 7-15min so as to obtain LiCo1/3Mn1/3Fe1/3PO4/C. The method provided by the invention is simple and easy to control and has advantages of short reaction time and low cost. The prepared LiCo1/3Mn1/3Fe1/3PO4/C has characteristics of small particle size, homogeneous distribution, high conductivity, high specific capacity, good cycling stability, excellent high-rate discharge performance and high energy density.

Description

The rapid microwave reaction method for preparing of ternary polyanion phosphate/carbon positive electrode for a kind of power lithium-ion battery
Technical field
The present invention relates to the preparation of power lithium-ion battery positive electrode, be specifically related to the rapid microwave reaction method for preparing of a kind of power lithium-ion battery ternary polyanion phosphate/carbon positive electrode.
Background technology
In recent years, along with the commercialized development of electric automobile, hybrid vehicle, electric bicycle of new generation etc., lithium ion battery is faced with increasing challenge.Exploitation height ratio capacity, high power, long circulation life and low cost lithium ion battery become the main direction of its development.LiFePO4 (LiFePO 4) positive electrode has that theoretical capacity is high, cost is low, fail safe is good, environmental friendliness and the feature such as multiplying power property is good, is one of main selection of lithium-ion-power cell.But it runs into some problems in actual applications, as lower plateau potential (3.4V) and little tap density (due to coated a large amount of carbon), therefore its specific energy density lower (about 580Wh/kg).Lithium manganese phosphate (LiMnPO 4) and cobalt phosphate lithium (LiCoPO 4) have and LiFePO 4similar olivine-type structure, but it has higher plateau potential (being respectively 4.1V and 4.8V), and and LiFePO 4substantially suitable theoretical specific capacity (170mAh/g), therefore they compare LiFePO 4there is very high specific energy density (being respectively about 684Wh/kg and 800Wh/kg).But, due to LiMnPO 4electronic conductivity and ionic conductivity lower, therefore its electro-chemical activity is poor.And LiCoPO 4higher plateau potential, decomposes conventional organic electrolyte, and therefore cycle performance is poor.
Three metal phosphate solid solution LiCo 1/3mn 1/3fe 1/3pO 4there are three and charge and discharge radio station platform, be respectively 3.6V, 4.1V, the corresponding Fe of 4.7V 2+/ Fe 3+, Mn 2+/ Mn 3+and Co 2+/ Co 3+electrode potential, researcher finds, risen about 0.2V of the platform of Fe, the platform of cobalt about 0.2V left and right that declined, and the platform of Mn is substantially constant.LiCo 1/3mn 1/3fe 1/3pO 4with respect to LiFePO 4improve voltage platform, increased energy density; With respect to LiMnPO 4improve the conductivity of material, strengthened electro-chemical activity phase; With respect to LiCoPO 4, improved its cycle performance.Therefore, LiCo 1/3mn 1/3fe 1/3pO 4it is a kind of phosphate cathode material with good prospect.Traditional preparation LiCo 1/3mn 1/3fe 1/3pO 4method mainly contains solid-phase synthesis, spray pyrolysis, coprecipitation, sol-gal process (Electrochem.Commun.11 (2009) 1183; Solid State Ionics178 (2008) 1676; J.Power Sources242 (2013) 627; Chem.Mater.22 (2010) 2573.) etc.But all there are some intrinsic shortcomings in these methods, as: the shortcoming such as synthesis temperature is high, synthesis cycle is long, controlled condition is harsh, cost is high and resulting materials performance is not good, these are all limiting LiCo 1/3mn 1/3fe 1/3pO 4extensive industrialization.In addition, in the research of phosphoric acid positive electrode, carbon is coated and is proved to be the electrochemistry performance that can effectively promote this class material.Therefore, a kind of LiCo with excellent electrochemical performance for preparing is proposed 1/3mn 1/3fe 1/3pO 4the fast synthesis method of positive electrode.
Summary of the invention
The object of the invention is some problems that exist for above-mentioned power lithium-ion battery polyanion phosphoric acid salt positive electrode, provide a kind of rapidly and efficiently preparation to there is the ternary polyanion phosphate solid solution LiCo of good electrical chemical property 1/3mn 1/3fe 1/3pO 4the method of/C positive electrode.The material particle size making by the method is evenly distributed, particle diameter is little, conductivity is high, and has high specific capacity, good cyclical stability, the large multiplying power discharging property of excellence and high energy density.And the method process is simple, the reaction time is short, has simplified synthesis technique, has reduced preparation cost.
The present invention realizes above-mentioned technical purpose by following technological means.
A rapid microwave reaction method for preparing for ternary polyanion phosphate/carbon positive electrode for power lithium-ion battery, is characterized in that, comprises the following steps:
(1) be that 1～1.1:1/3:1/3:1/3:1 takes lithium salts, molysite, manganese salt, cobalt salt, phosphate and puts into ball grinder in molar ratio;
(2) in ball grinder, add the carbon source of people 7～10wt%, and put into a certain amount of ethanol, raw material can be immersed and is as the criterion;
(3) ball grinder is placed on planetary ball mill, with the rotating speed ball millings of 3600 revs/min 5～10 hours, raw material after taking-up grinds, oven dry, compressing tablet, then put into the atmosphere furnace that is connected with inert gas, be warmed up to 350 DEG C with the heating rate of 5 DEG C/min, at 350 DEG C, decompose 1～5 hour;
(4) again grind, compressing tablet, in microwave reactor under the power of 700W microwave 7～15 minutes, be LiCo after cooling 1/3mn 1/3fe 1/3pO 4/ C.
Preferably, described lithium salts is the one in lithium acetate, lithium nitrate, lithium carbonate, lithium fluoride.
Preferably, described molysite is the one in ferric carbonate, ferric oxalate, ferric nitrate.
Preferably, described manganese salt is the one in manganese carbonate, manganese acetate, manganese nitrate.
Preferably, described cobalt salt is the one in cobalt carbonate, cobalt acetate, cobalt nitrate.
Preferably, described phosphate is the one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate.
Preferably, described carbon source is the one in acetylene black, conductive black super P, porous, electrically conductive carbon black Ketjenblack EC600JD, micropore superconduction carbon black BP2000, carbon nano-fiber (being called for short CNFs), ordered mesopore carbon (being called for short OMC), porous carbon CMK-3, graphene oxide (being called for short GO), Graphene.
Preferably, described inert gas is nitrogen or argon gas.
Preferably, in described step (3), the pressure of compressing tablet is 10～15 MPas.
Advantage of the present invention is:
(1) the present invention has simplified synthesis technique, and method is simple and convenient, be easy to control, the reaction time is short, homogeneous heating, and cost is low.
(2) course of reaction effectively suppresses LiCo 1/3mn 1/3fe 1/3pO 4too growing up of crystal grain, particle diameter is evenly distributed, particle diameter is little, the LiCo of gained 1/3mn 1/3fe 1/3pO 4/ C composite material has special structure, and carbon is coated on the surface of positive electrode, forms a kind of class nucleocapsid structure electrode material, also has carbon net to be connected between particle simultaneously.Conductivity is high, and has high specific capacity, good cyclical stability, the large multiplying power discharging property of excellence and high energy density.
(3) by gained LiCo 1/3mn 1/3fe 1/3pO 4/ C composite material, for lithium ion cell positive, has good charge-discharge performance, cycle performance and high rate performance etc.
Brief description of the drawings
Fig. 1 is X-ray diffraction analysis (XRD) figure of the embodiment of the present invention 1 sample.
Fig. 2 is ESEM (SEM) figure of the embodiment of the present invention 1 sample.
Fig. 3 is transmission electron microscope (TEM) figure of the embodiment of the present invention 1 sample.
Fig. 4 is high power transmission electron microscope (HRTEM) figure of the embodiment of the present invention 1 sample.
Fig. 5 is the first charge-discharge curve of the embodiment of the present invention 1 product.
Fig. 6 is the cycle performance curve of the embodiment of the present invention 1 sample.
Fig. 7 is the first charge-discharge curve under 0.1C multiplying power of the embodiment of the present invention 2 samples.
Fig. 8 is the first charge-discharge curve under 0.1C multiplying power of the embodiment of the present invention 3 samples.
Fig. 9 is the first charge-discharge curve under 0.1C multiplying power of the embodiment of the present invention 4 samples.
Figure 10 is the first charge-discharge curve under 0.1C multiplying power of the embodiment of the present invention 5 samples.
Figure 11 is the first charge-discharge curve under 0.1C multiplying power of the embodiment of the present invention 6 samples.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
Embodiment 1
In molar ratio for the ratio of 1.05:1/3:1/3:1/3:1 takes lithium acetate, ferric nitrate, cobalt acetate, manganese acetate, diammonium hydrogen phosphate, put in agate jar or zirconia ball grinding jar, then add the approximately micropore superconduction carbon black BP2000 of 7～10wt%, add 15～20mL ethanol, raw material can be immersed and is as the criterion.Then, ball grinder is placed in to ball milling on planetary ball mill, the time is 5～10 hours, and rotating speed is 3600 rpms.After ball milling, dry, 10～15 MPa lower sheetings, put in the tube furnace that is connected with argon gas, 350 DEG C of heat treatment 1～5 hour.Grind, compressing tablet, puts into microwave reactor, and 700W microwave 7～15 minutes, obtains LiFe 1/3mn 1/3co 1/3pO 4/ C composite material.
Fig. 1 is the X-ray diffraction analysis figure of the prepared product of the present embodiment, shows that product is single orderly LiMPO 4olivine structural, belongs to rhombic system, and space group is Pmnb, does not have any dephasign.According to the SEM figure shown in Fig. 2, can obtain the particle diameter of product in 250nm left and right; TEM figure shown in Fig. 3 shows between particle and is connected by carbon net; HRTEM figure carbon film shown in Fig. 4 shows the about 5nm of thickness of carbon film.
Obtained product is assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, under the multiplying power of 0.1C, discharge and recharge, obtain first charge-discharge curve as shown in Figure 5, charging and discharging curve is made up of three platforms respectively, be respectively 3.62/3.37 volt, 4.27/3.99 volt and 4.77/4.58 volt, corresponding Fe 2+/ Fe 3+, Mn 2+/ Mn 3+and Co 2+/ Co 3+electrochemical reaction current potential; First all discharge capacities are 160 MAhs/g.Cycle performance as shown in Figure 6, is circulated to 30 weeks rear capacity and still can be stabilized in 143 MAhs/g of left and right under 0.1 multiplying power current density.
Embodiment 2
Micropore superconduction carbon black BP2000 in embodiment 1 is replaced with to acetylene black, and other are identical with embodiment 1, and under 0.1 multiplying power current density, as shown in Figure 7, first all charge/discharge capacities are 211/137 MAh/g to first all charge/discharge capacity test results.
Embodiment 3
Micropore superconduction carbon black BP2000 in embodiment 1 is replaced with to conductive black super P, and other are identical with embodiment 1, and under 0.1 multiplying power current density, as shown in Figure 8, first all charge/discharge capacities are 196/145 MAh/g to first all charge/discharge capacity test results.
Embodiment 4
By in embodiment 1, micropore superconduction carbon black BP2000 replaces with porous, electrically conductive carbon black Ketjenblack EC600JD, and other are with embodiment 1, under 0.1 multiplying power current density, as shown in Figure 9, first all charge/discharge capacities are 225/147 MAh/g to first all charge/discharge capacity test results.
Embodiment 5
Lithium acetate, ferric nitrate, cobalt acetate, manganese acetate and diammonium hydrogen phosphate in embodiment 1 are replaced with respectively to lithium carbonate, ferrous oxalate, cobalt carbonate, manganese carbonate and ammonium dihydrogen phosphate, other are with embodiment 1, under 0.1 multiplying power current density, as shown in figure 10, first all charge/discharge capacities are 230/170 MAh/g to first all charge/discharge capacity test results.
Embodiment 6
Lithium acetate, ferric nitrate, cobalt acetate, manganese acetate and diammonium hydrogen phosphate in embodiment 1 are replaced with respectively to lithium carbonate, ferrous oxalate, cobalt carbonate, manganese carbonate and ammonium dihydrogen phosphate, micropore superconduction carbon black (BP2000) replaces with porous, electrically conductive carbon black Ketjenblack EC600JD, other are with embodiment 1, under 0.1 multiplying power current density, as shown in figure 11, first all charge/discharge capacities are 216/152 MAh/g to first all charge/discharge capacity test results.
Described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned execution mode; in the situation that not deviating from flesh and blood of the present invention, any apparent improvement, replacement or modification that those skilled in the art can make all belong to protection scope of the present invention.

Claims (9)

1. a rapid microwave reaction method for preparing for ternary polyanion phosphate/carbon positive electrode for power lithium-ion battery, is characterized in that, comprises the following steps:
(1) be that 1～1.1:1/3:1/3:1/3:1 takes lithium salts, molysite, manganese salt, cobalt salt, phosphate and puts into ball grinder in molar ratio;
(2) in ball grinder, add the carbon source of people 7～10wt%, and put into a certain amount of ethanol, raw material can be immersed and is as the criterion;
(3) ball grinder is placed on planetary ball mill, with the rotating speed ball millings of 3600 revs/min 5～10 hours, raw material after taking-up grinds, oven dry, compressing tablet, then put into the atmosphere furnace that is connected with inert gas, be warmed up to 350 DEG C with the heating rate of 5 DEG C/min, at 350 DEG C, decompose 1～5 hour;
(4) again grind, compressing tablet, in microwave reactor under the power of 700W microwave 7～15 minutes, be LiCo after cooling 1/3mn 1/3fe 1/3pO 4/ C.
2. preparation method according to claim 1, is characterized in that, described lithium salts is the one in lithium acetate, lithium nitrate, lithium carbonate, lithium fluoride.
3. preparation method according to claim 1, is characterized in that, described molysite is the one in ferric carbonate, ferric oxalate, ferric nitrate.
4. preparation method according to claim 1, is characterized in that, described manganese salt is the one in manganese carbonate, manganese acetate, manganese nitrate.
5. preparation method according to claim 1, is characterized in that, described cobalt salt is the one in cobalt carbonate, cobalt acetate, cobalt nitrate.
6. preparation method according to claim 1, is characterized in that, described phosphate is the one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate.
7. preparation method according to claim 1, it is characterized in that, described carbon source is the one in acetylene black, conductive black super P, porous, electrically conductive carbon black Ketjenblack EC600JD, micropore superconduction carbon black BP2000, carbon nano-fiber (being called for short CNFs), ordered mesopore carbon (being called for short OMC), porous carbon CMK-3, graphene oxide (being called for short GO), Graphene.
8. preparation method according to claim 1, is characterized in that, described inert gas is nitrogen or argon gas.
9. preparation method according to claim 1, is characterized in that, in described step (3), the pressure of compressing tablet is 10～15 MPas.
CN201410192405.XA 2014-05-08 2014-05-08 A kind of rapid microwave reaction method for preparing of power lithium-ion battery ternary polyanion phosphate/carbon positive electrode Active CN103996823B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106532007A (en) * 2016-12-19 2017-03-22 高霞 Preparation method of positive electrode of lithium-ion secondary battery for electric toothbrush or electric shaver
CN106935849A (en) * 2015-12-31 2017-07-07 比亚迪股份有限公司 A kind of anode material for lithium-ion batteries and preparation method thereof
CN107742713A (en) * 2017-10-27 2018-02-27 天津先众新能源科技股份有限公司 A kind of synthetic method of graphene/lithium ferric manganese phosphate material
CN109103444A (en) * 2018-08-30 2018-12-28 上海力信能源科技有限责任公司 A kind of LiMPO4The preparation method of In-situ reaction graphene
CN111668448A (en) * 2020-07-14 2020-09-15 贵州梅岭电源有限公司 Lithium iron phosphate modified composite material and preparation method thereof

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CN1994874A (en) * 2006-12-21 2007-07-11 四川师范大学 Polycrystalline LiFePO4 powder solid phase-microwave synthesis method
US20110300442A1 (en) * 2010-06-02 2011-12-08 Infinity Energy (Hong Kong) Co., Limited Novel nanoscale solution method for synthesizing lithium cathode active materials
KR101135700B1 (en) * 2010-01-21 2012-04-13 한국과학기술원 Method for manufacturing a metal oxalate material

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CN1911792A (en) * 2006-08-22 2007-02-14 南京大学 Microwave synthesis method for carbon coated iron phosphate of ion battery composite anode material
CN1994874A (en) * 2006-12-21 2007-07-11 四川师范大学 Polycrystalline LiFePO4 powder solid phase-microwave synthesis method
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106935849A (en) * 2015-12-31 2017-07-07 比亚迪股份有限公司 A kind of anode material for lithium-ion batteries and preparation method thereof
CN106935849B (en) * 2015-12-31 2019-12-20 比亚迪股份有限公司 Lithium ion battery anode material and preparation method thereof
CN106532007A (en) * 2016-12-19 2017-03-22 高霞 Preparation method of positive electrode of lithium-ion secondary battery for electric toothbrush or electric shaver
CN106532007B (en) * 2016-12-19 2020-10-09 高霞 Preparation method of lithium ion secondary battery anode for electric toothbrush or electric shaver
CN107742713A (en) * 2017-10-27 2018-02-27 天津先众新能源科技股份有限公司 A kind of synthetic method of graphene/lithium ferric manganese phosphate material
CN109103444A (en) * 2018-08-30 2018-12-28 上海力信能源科技有限责任公司 A kind of LiMPO4The preparation method of In-situ reaction graphene
CN111668448A (en) * 2020-07-14 2020-09-15 贵州梅岭电源有限公司 Lithium iron phosphate modified composite material and preparation method thereof
CN111668448B (en) * 2020-07-14 2023-02-24 贵州梅岭电源有限公司 Lithium iron phosphate modified composite material and preparation method thereof

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