CN1458706A - Lithium ion accumulator positive electrode material and synthetic method - Google Patents

Lithium ion accumulator positive electrode material and synthetic method Download PDF

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CN1458706A
CN1458706A CN02113739A CN02113739A CN1458706A CN 1458706 A CN1458706 A CN 1458706A CN 02113739 A CN02113739 A CN 02113739A CN 02113739 A CN02113739 A CN 02113739A CN 1458706 A CN1458706 A CN 1458706A
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electrode material
ion accumulator
lithium
compound
postive
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刘兴泉
李淑华
唐毅
何泽珍
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Chengdu Institute of Organic Chemistry of CAS
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Chengdu Institute of Organic Chemistry of CAS
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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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

This invention relates to a positive electrode material of Li-ion battery and its synthesizing method in the chemical formula of LixMn1-yMyO2, the method is to take a suitable proportion of compounds of Li, Mn and M and mix them evenly; and then the mixture is calcinated by sections for 12h-36h under 600 deg.C-1000 deg.C air atmosphere. The invented positive electrode material has good circulating stability and would not generate non-reversible phase variation from laminar structure to spinel structure.

Description

Postive electrode material of li-ion accumulator and synthetic method
Affiliated technical field
The present invention relates to a kind of positive electrode and synthetic method of lithium-ions battery, particularly a kind of novel lamellar structure consists of Li xMn 1-yM yO 2The positive electrode and the synthetic method of lithium-ions battery.
Background technology
The positive electrode of the lithium-ions battery that uses is mainly stratiform LiC at present 0O 2With spinel-type LiMn 2O 4Stratiform LiNiO 2Positive electrode is also in development and exploitation.Stratiform LiMnO 2Positive electrode because the harshness of its preparation condition and performance is undesirable, is regarded as always and can not uses.People such as Mitsuhara adopt hydrothermal synthesis method to prepare pure LiMnO 2The lamellar compound positive electrode, this positive electrode has higher first charge-discharge capacity, but its cyclical stability is relatively poor, this mainly is because there be the irreversible phase transition of layer structure to spinel structure in material in charge and discharge process, irreversible (the list of references: MitsuharaTabuchi that has caused the doff lithium of material, Kazuaki Ado, Hironori Kobayashi, et al.Synthsis ofLiMnO2With a-NaFeO 2-type Structure by a Mixed AlkalineHydrothermal Reaction J.Electrochem.Soc., 1998,145 (4) 49-55).People such as Bruce adopt ion-exchange to prepare pure LiMnO 2The lamellar compound positive electrode also exists identical deficiency (list of references: Armstrong A R, Bruce P G.Synthsis of Layered LiMnO 2As an Electrode for RechargeableLithium Batteries.Nature, 1996,381,499-500).People such as OLevi adopt high temperature (＞1000 ℃) solid reaction process to synthesize LiMnO 2Positive electrode (list of references LeviE, Zinigrad E, Teller H, et al Structure and ElectrochemicalStudies of 3V LixMnO 2Cathodes for Rechargeable Li Batteries.J.Electrochem Soc., 1997,144 (2), 4133-4141), the result is similar to the front.
The technical scheme of invention
For its cyclical stability that the positive electrode that overcomes existing lithium-ions battery exists relatively poor, there be the irreversible phase transition of layer structure to spinel structure in material in charge and discharge process, the irreversible shortcoming that has caused the doff lithium of material, the invention provides a kind of positive electrode and synthetic method of new lithium-ions battery, has good cycling stability, material structure is stable in charge and discharge process, the irreversible phase transition of layer structure to spinel structure can not take place, the manufacturing raw material is wide, price is low, characteristics such as non-environmental-pollution.
The technical solution adopted for the present invention to solve the technical problems is:
The crystal phase structure of Postive electrode material of li-ion accumulator of the present invention is shown in Figure of description 1, and the characteristic peak of X-powder diffraction phasor is 4.69,2.40 (bimodal), and 2.00.Its chemical formula is Li xMn 1-yM yO 2, wherein: 0.5≤x≤1.5,0≤y≤0.5, M is any one of Cr, Co, Ni, Al, Ga, In, Tl, Ti.
The synthetic method of Postive electrode material of li-ion accumulator of the present invention is: a kind of compound that contains lithium and a kind of compound that contains manganese and a kind of compound that contains doping metals (M) are mixed after by the proper proportion amount of getting, then in baking furnace and air atmosphere under 600 ℃ of-1000 ℃ of roasting 12h-36h, the Li that (cooling to room temperature with the furnace, through pulverizing, grind, sieving) solid phase reaction obtains consisting of xMn 1-yM yO 2The positive electrode sample.
The invention has the beneficial effects as follows: the first charge-discharge capacity of positive electrode is respectively up to 150mAh/g and 145mAh/g, good cycling stability.After the constant current charge-discharge circulation 100 times, reversible discharge capacity still remains on 135mAh/g.Material structure is stable in charge and discharge process, and the irreversible phase transition of layer structure to spinel structure can not take place.Cheap, non-environmental-pollution, electrochemistry cycle performance and stability are good.
Embodiment:
Postive electrode material of li-ion accumulator of the present invention, its crystal phase structure are shown in Figure of description 1, and the characteristic peak of X-powder diffraction phasor is 4.69,2.40 (bimodal), and 2.00.Its chemical formula is Li xMn 1-yM yO 2, wherein: 0.5≤x≤1.5,0≤y≤0.5, M is any one of Cr, Co, Ni, Al, Ga, In, Tl, Ti.This positive electrode has layer structure, and its reversible discharge capacity is greater than 140mAh/g, and cycle performance is greater than 100 times, and capability retention is not less than 90%, in charge and discharge process, the irreversible phase transition of layer structure to spinel structure can not take place.
The synthetic method of Postive electrode material of li-ion accumulator of the present invention, it is characterized in that: a kind of compound that contains lithium and a kind of compound that contains manganese and a kind of compound that contains doping metals (M) are mixed after by the proper proportion amount of getting, at air atmosphere, 600 ℃ of-1000 ℃ of roasting 12h-36h in the baking furnace, solid phase reaction synthesizing lithium ion accumulator positive electrode Li xMn 1-yM yO 2During roasting, can be earlier at 700 ℃ of-830 ℃ of following roasting 6h-18h, again at 770 ℃ of-870 ℃ of following roasting 6h-18h, the compound that wherein contains lithium is any one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate, the compound that contains manganese is chemical MnO 2, electrolysis MnO 2, manganese carbonate, manganese nitrate, manganese acetate, manganese oxalate, γ-MnOOH any one, the compound that contains doping metals (M) is its corresponding oxide, hydroxide and salt.
The present invention is described further below in conjunction with embodiment and accompanying drawing.
Fig. 1 is the X-powder diffraction phasor of Postive electrode material of li-ion accumulator crystal phase structure.
Fig. 2 is a Postive electrode material of li-ion accumulator charge/discharge capacity curve chart.
Fig. 3 is a Postive electrode material of li-ion accumulator charge-discharge performance curve chart.
Fig. 4 is a Postive electrode material of li-ion accumulator charge/discharge capacity curve chart.(embodiment 2 and 3 change raw materials, constant prescription. enforceable prescription is seen embodiment 4.)
Embodiment 1
With 29.0588g electrolytic manganese dioxide and 0.6356g four oxidations, three cobalts and 12.0631g carbon After mixing, grinds evenly the acid lithium in Muffle furnace and under the air atmosphere 600 ℃-1000 ℃ then Baking inphases 12h-36h. Cool to room temperature with the furnace, sieve through pulverizing, grind, cross 300 orders, Namely obtain the Li that consists of1.01Mn 0.975Co 0.025O 2Anodal material sample. This product is the stratiform knot Structure (seeing accompanying drawing 1). As the active material of positive pole, acetylene is black to be conductive agent, polytetrafluoro then Vac emulsion is bonding dose. Anodal material: conductive agent: bonding dose=85: 10: 5 (weight ratio). Then take aluminium foil as the collector smear, take metal lithium sheet as reference (to) electrode, with 1.0mol/L LiClO4/ EC+DEC (1: 1Vol.) be electrolyte, be full of the stainless steel gloves case of argon gas In be assembled into the simulation button cell. Then enterprising at the full-automatic battery performance test instrument of DC-5 type The row constant current charge-discharge. Voltage range 4.35V-2.70V, current density is 0.4mA/cm2, fill Discharge rate is 0.4-0.5C, charging and discharging currents 0.25mA. After tested, this material first Charging capacity is 151.30mAh/g, and discharge capacity is 147.30mAh/g first, and efficient reaches 97.3%. See accompanying drawing 4. After the constant current charge-discharge circulation 100 times, the discharge capacity of material still keeps At 135.10mAh/g, efficient is greater than 99.0%. Capability retention is 91.7%. See accompanying drawing 3. In the charge and discharge cycles process, observable phase structure does not take place anodal material changes table There are not obvious voltage jump and platform transition on the charging and discharging curve now. See accompanying drawing 2.
Embodiment 2
Present embodiment is except replacing four oxidations, three cobalts as the cobalt source take three oxidations, two cobalts, and all the other are with real Execute example 1. The first charge/discharge capacity of sample material be respectively 148.50mAh/g and 139.80mAh/g efficient is 94.1%. After the constant current charge-discharge circulation 20 times, charge/discharge capacity Be respectively 139.30mAh/g and 134.90mAh/g, efficient is 96.9%. Be equivalent to per 100 The capability retention of inferior circulation is 84.5%.
Embodiment 3
Present embodiment is the manganese source except replacing electrolytic manganese dioxide with chemical manganese bioxide, and all the other are with embodiment 1.The first charge-discharge capacity of specimen material is respectively 128.70mAh/g and 121.30mAh/g, and efficient is 94.3%.After the constant current charge-discharge circulation 20 times, charge/discharge capacity is respectively 122.70mAh/g and 117.10mAh/g, and efficient is 95.4%.The capability retention that is equivalent to per 100 circulations is 83.5%.
Embodiment 4
Present embodiment is mainly investigated the influence of Mn/Co mol ratio to material electrochemical capacity and efficient, the results are shown in Table 1.Except Mn/Co mol ratio difference, all the other are with embodiment 1.
Table 1 Mn/Co mol ratio affects first discharge capacity initial charge volumetric efficiency mol ratio of Mn/Co to the chemical property of specimen material, (mAh/g), (mAh/g), (%) 0.975: 0.025 147.30 151.30 97.30.95: 0.05 146.80 152.10 96.50.90: 0.10 143.80 151.20 95.10.80: 0.20 142.50 149.70 95.20.50: 0.50 144.40 151.10 95.60.05: 095 148.70 153.80 96.7
Embodiment 5
Present embodiment is mainly investigated sintering temperature and roasting mode to the influence of material charge/discharge capacity and efficient, the results are shown in Table 2.Except sintering temperature was different with the roasting mode, all the other were with embodiment 1.
Table 2 sintering temperature and baking modes affect first discharge capacity initial charge volumetric efficiency remarks of sintering temperature roasting to material electrochemical performance, (℃) mode, (mAh/g), (mAh/g), (%) 750 ~ 780 segmentations, 128.10 132.40 96.8780 continuous 127.30 132.60 95.9780 ~ 820 segmentations, 147.30 151.30 97.3 examples, 1820 continuous 143.20 148.30 96.6820 ~ 850 segmentations 142.30 148.10 96.1850 continuous 138.90 146.50 94.8
LiMnO 2Main X-diffraction (Miller index) characteristic peak
Compd. Value Card No.1. LiMnO 25.8 3.62 2.02 23-3612. LiMnO 25.72 3.57 2.28 9-1093. LiMnO 25.75 2.29 2.01 35-7491. Li 0.3MnO 24.37 2.65 2.44 44-1472. Li 0.9MnO 24.61 2.79 2.45 44-1443. Li 1.01Mn 0.925Co 0.025O 24.69 2.40 2.00 this patents

Claims (10)

1, a kind of Postive electrode material of li-ion accumulator, its crystal phase structure are shown in Figure of description 1, and the characteristic peak of X-powder diffraction phasor is 4.69,2.40 (bimodal), and 2.00.
2, Postive electrode material of li-ion accumulator according to claim 1 is characterized in that: its chemical formula is Li xMn 1-yM yO 2, wherein: 0.5≤x≤1.5,0≤y≤0.5, M is any one of Cr, Co, Ni, Al, Ga, In, Tl, Ti.
3, Postive electrode material of li-ion accumulator according to claim 1 and 2 is characterized in that: this positive electrode has layer structure.
4, Postive electrode material of li-ion accumulator according to claim 1 and 2 is characterized in that: the reversible discharge capacity of this positive electrode is greater than 140mAh/g, and cycle performance is greater than 100 times, and capability retention is not less than 90%.
5, according to any described Postive electrode material of li-ion accumulator of claim in front, it is characterized in that: in charge and discharge process, the irreversible phase transition of layer structure to spinel structure can not take place.
6, the synthetic method of any described Postive electrode material of li-ion accumulator of claim in front, it is characterized in that: a kind of compound that contains lithium and a kind of compound that contains manganese and a kind of compound that contains doping metals (M) are mixed after by the proper proportion amount of getting, at air atmosphere, 600 ℃ of-1000 ℃ of roasting 12h-36h in the baking furnace, solid phase reaction synthesizing lithium ion accumulator positive electrode Li xMn 1-yM yO 2
7, the synthetic method of Postive electrode material of li-ion accumulator according to claim 6 is characterized in that: at air atmosphere, and 700 ℃ of-830 ℃ of roasting 6h-18h in the baking furnace, 770 ℃ of-870 ℃ of roasting 6h-18h.
8, the synthetic method of Postive electrode material of li-ion accumulator according to claim 6 is characterized in that: the compound that contains lithium is any one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate.
9, the synthetic method of Postive electrode material of li-ion accumulator according to claim 6 is characterized in that: the compound that contains manganese is chemical MnO 2, electrolysis MnO 2, manganese carbonate, manganese nitrate, manganese acetate, manganese oxalate, γ-MnOOH any one.
10, the synthetic method of Postive electrode material of li-ion accumulator according to claim 6 is characterized in that: the compound that contains doping metals (M) is its corresponding oxide, hydroxide and salt.
CN02113739A 2002-05-15 2002-05-15 Lithium ion accumulator positive electrode material and synthetic method Pending CN1458706A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102903905A (en) * 2012-10-09 2013-01-30 江苏科捷锂电池有限公司 Preparation method of zinc-doped spinel cathode material
CN103682467A (en) * 2013-11-25 2014-03-26 武汉孚安特科技有限公司 Secondary Li-Mn soft-packed battery and preparation method thereof
CN111511688A (en) * 2017-12-18 2020-08-07 戴森技术有限公司 Compound (I)
CN115621449A (en) * 2022-11-01 2023-01-17 国联汽车动力电池研究院有限责任公司 High-capacity layered-spinel two-phase composite doped lithium manganate and preparation method thereof
US11616229B2 (en) 2017-12-18 2023-03-28 Dyson Technology Limited Lithium, nickel, manganese mixed oxide compound and electrode comprising the same
US11658296B2 (en) 2017-12-18 2023-05-23 Dyson Technology Limited Use of nickel in a lithium rich cathode material for suppressing gas evolution from the cathode material during a charge cycle and for increasing the charge capacity of the cathode material
US11769911B2 (en) 2017-09-14 2023-09-26 Dyson Technology Limited Methods for making magnesium salts
US11817558B2 (en) 2017-09-14 2023-11-14 Dyson Technology Limited Magnesium salts

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102903905A (en) * 2012-10-09 2013-01-30 江苏科捷锂电池有限公司 Preparation method of zinc-doped spinel cathode material
CN103682467A (en) * 2013-11-25 2014-03-26 武汉孚安特科技有限公司 Secondary Li-Mn soft-packed battery and preparation method thereof
CN103682467B (en) * 2013-11-25 2016-04-20 武汉孚安特科技有限公司 Secondary lithium manganese flexible-packed battery and preparation method
US11769911B2 (en) 2017-09-14 2023-09-26 Dyson Technology Limited Methods for making magnesium salts
US11817558B2 (en) 2017-09-14 2023-11-14 Dyson Technology Limited Magnesium salts
CN111511688A (en) * 2017-12-18 2020-08-07 戴森技术有限公司 Compound (I)
US11616229B2 (en) 2017-12-18 2023-03-28 Dyson Technology Limited Lithium, nickel, manganese mixed oxide compound and electrode comprising the same
CN111511688B (en) * 2017-12-18 2023-04-25 戴森技术有限公司 Compounds of formula (I)
US11658296B2 (en) 2017-12-18 2023-05-23 Dyson Technology Limited Use of nickel in a lithium rich cathode material for suppressing gas evolution from the cathode material during a charge cycle and for increasing the charge capacity of the cathode material
US11967711B2 (en) 2017-12-18 2024-04-23 Dyson Technology Limited Lithium, nickel, cobalt, manganese oxide compound and electrode comprising the same
CN115621449A (en) * 2022-11-01 2023-01-17 国联汽车动力电池研究院有限责任公司 High-capacity layered-spinel two-phase composite doped lithium manganate and preparation method thereof

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