CN104332612A - Phosphorus-modified carbon-coated lithium ion battery positive composite material, and preparation method and use thereof - Google Patents

Phosphorus-modified carbon-coated lithium ion battery positive composite material, and preparation method and use thereof Download PDF

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CN104332612A
CN104332612A CN201410448588.7A CN201410448588A CN104332612A CN 104332612 A CN104332612 A CN 104332612A CN 201410448588 A CN201410448588 A CN 201410448588A CN 104332612 A CN104332612 A CN 104332612A
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lithium ion
ion battery
composite material
coated lithium
carbon
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CN104332612B (en
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张金利
王姣
刘媛媛
李韡
谷俊杰
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Tianjin 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/5825—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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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)
  • Composite Materials (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a phosphorus-modified carbon-coated lithium ion battery positive composite material, and a preparation method and a use thereof. The preparation method comprises the following steps: 1, uniformly mixing a carbon-coated lithium ion battery positive material with a phosphorus source according to a mass ratio of 1:(0.1-1), drying the obtained mixture in a vacuum drying box at 100-200DEG C for 8-24h, and grinding to obtain powder; and 2, placing the powder obtained in step 1 in a tubular furnace, heating to 300-1000 DEG C under a heating rate of 1-10DEG C/min under the protection of nitrogen, and carrying out constant temperature calcination for 1-6h to obtain the phosphorus-modified carbon-coated lithium ion battery positive composite material. The method has the advantages of wide sources of raw materials, low price, simple synthetic process, easy control of process conditions, safety, environmental protection, and suitableness for industrialized production, and the phosphorus-modified carbon-coated lithium ion battery positive composite material prepared through the method has good cycle performance and other electrochemical performances under a high rate.

Description

P Modification carbon-coated lithium ion battery anode composite material and Preparation method and use
Technical field
The present invention relates to a kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, belong to anode material for lithium-ion batteries technical field.
Background technology
The lithium ion battery of environmental protection is the novel power supply system grown up early 1990s, because its operating voltage is high, volume is little, quality is light, memory-less effect, have extended cycle life, the feature such as pollution-free is subject to people's attention and favors, and is the green high-capacity rechargeable battery of a new generation.It replaces lithium metal to make positive pole with embedding lithium material with carbon element, overcome in the past lithium battery because of the circulating and reversible performance caused by Li dendrite and the defect in security performance, both the key properties such as lithium battery high voltage, high-energy-density had been maintained, have again serviceability temperature wide ranges (37 DEG C ~ 60 DEG C), have extended cycle life, self-discharge rate is few, advantage that memory-less effect, quickly-chargeable, non-environmental-pollution etc. are outstanding, be the storage battery of new generation after traditional lead acid accumulator, ickel-cadmium cell, Ni-H cell.But lithium ion battery comes out only more than ten years, and it has manifested obvious deficiency, as higher in cost, high rate performance is not good enough.For this reason, scientific and technological circle and the industrial quarters in the whole world are all devoted to the correlation technique improving lithium ion battery, and research and development lithium ion battery new material, improves its performance, reduce its cost.
In recent years for promoting the rate capability of anode material for lithium-ion batteries, overcome inherent defect, improve its chemical property, the main method of current employing comprises following two kinds: (1) utilizes the novel more tiny homogeneous particle of method preparation to shorten lithium ion diffusion length, and the rate capability of electrode material is got a promotion; (2) carry out sheet conductivity material on material granule surface and be coated with the electrical contact promoted in surperficial conductivity and electrode, as coated in material surface carbon etc.Scholars more both domestic and external have done further improvement research to material carbon coating layer at present, mainly carry out nitrogen modification to carbon coating layer.But not yet there is report carbon coating layer being carried out to P Modification.
Summary of the invention
The object of this invention is to provide a kind of raw material sources extensive, cheap, synthesis technique is simple, process conditions are easy to control and safety and environmental protection, be applicable to the preparation method of the P Modification carbon-coated lithium ion battery anode composite material of suitability for industrialized production.
Second object of the present invention is to provide a kind of P Modification carbon-coated lithium ion battery anode composite material with good chemical property.
3rd object of the present invention is to provide a kind of purposes of P Modification carbon-coated lithium ion battery anode composite material.
Method of the present invention is summarized as follows:
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) in mass ratio for 1:(0.1 ~ 1) ratio anode material for lithium-ion batteries coated for carbon is mixed with phosphorus source, at 100 ~ 200 DEG C of temperature in vacuum drying chamber drying 8 ~ 24h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with ramp to 300 ~ 1000 DEG C of 1 ~ 10 DEG C/min, calcining at constant temperature 1 ~ 6h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
The preferred triphenyl phosphorus in phosphorus source, phosphoric acid, phosphorous acid, pyrophosphoric acid, metaphosphoric acid, ammonium phosphate or ammonium dihydrogen phosphate.
Anode material for lithium-ion batteries is preferably LiFePO 4, LiMnPO 4, LiCoPO 4, Li 4ti 5o 12, Li 2feSiO 4, Li 3v 2(PO 4) 3or LiNi xco ymn 1-x-yo 2, wherein 0<x<0.5; 0<y<0.5.
P Modification carbon-coated lithium ion battery anode composite material prepared by said method.
Above-mentioned P Modification carbon-coated lithium ion battery anode composite material is preparing the purposes of battery.
The invention has the advantages that: method raw material sources of the present invention are extensive, cheap, synthesis technique is simple, process conditions are easy to control and safety and environmental protection, be applicable to suitability for industrialized production, the P Modification carbon-coated lithium ion battery anode composite material prepared by method of the present invention has circulation performance preferably and waits chemical property under high magnification.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of P Modification carbon-coated lithium ion battery anode composite material prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM photo of P Modification carbon-coated lithium ion battery anode composite material prepared by the embodiment of the present invention 1.
The rate charge-discharge curve chart of the anode material for lithium-ion batteries that the carbon that Fig. 3 adopts for the embodiment of the present invention 1 is coated.
Fig. 4 is the rate charge-discharge curve chart of P Modification carbon-coated lithium ion battery anode composite material as anode material for lithium-ion batteries of the embodiment of the present invention 1 preparation.
Fig. 5 is the cycle performance curve chart of P Modification carbon-coated lithium ion battery anode composite material as anode material for lithium-ion batteries of the embodiment of the present invention 1 preparation.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.The following examples understand the present invention better to enable those skilled in the art to, but do not impose any restrictions the present invention.
The coated anode material for lithium-ion batteries of the carbon that various embodiments of the present invention adopt is commercially produced product.
Embodiment 1
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.5 is by LiFePO coated for carbon in mass ratio 4mix with triphenyl phosphorus, at 100 DEG C of temperature in vacuum drying chamber dry 10h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 600 DEG C of 5 DEG C/min, calcining at constant temperature 3h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
The above-mentioned P Modification carbon-coated lithium ion battery anode composite material that obtains is made battery by the following method:
By the 80:10:10 mixing in mass ratio of P Modification carbon-coated lithium ion battery anode composite material, conductive agent (acetylene black), binding agent polyvinylidene fluoride (PVDF), add appropriate 1-METHYLPYRROLIDONE (NMP) as dispersant, magnetic agitation 10h mixes, then on clean aluminium foil, uniformly film is scraped, again film is placed in 80 DEG C of dry 12h of vacuum drying chamber, compressing tablet punching obtains pole piece, in glove box, be assembled into battery.
The XRD collection of illustrative plates of the P Modification carbon-coated lithium ion battery anode composite material that embodiment 1 is obtained as shown in Figure 1, the peak position of the peak position of this material and standard card (JCPDS#40-1499) is completely the same, provable material is LiFePO4 pure phase, and P Modification does not affect material purity.The diffraction maximum of LiFePO4 is sharply clear, and obtained LiFePO 4 material good crystallinity is described.As shown in Figure 2, material granule is club shaped structure to the SEM photo of the P Modification carbon-coated lithium ion battery anode composite material that embodiment 1 is obtained, width ~ 100nm, length ~ 200nm.
Be assembled into battery to record material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reach 165.5mAh g respectively -1, 154.1mAh g -1, 143.3mAh g -1, 134.1mAh g -1, 124.0mAh g -1, 50 capability retentions that circulate under 20C are 90%, see Fig. 4, Fig. 5.
The rate charge-discharge curve chart of the battery that the coated anode material for lithium-ion batteries of the material carbon that Fig. 3 adopts for the present embodiment is prepared by the method for the present embodiment.
Embodiment 2
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:1 is by LiMnPO coated for carbon in mass ratio 4mix with metaphosphoric acid, at 120 DEG C of temperature in vacuum drying chamber dry 8h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 700 DEG C of 7 DEG C/min, calcining at constant temperature 2h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 2.Be assembled into battery to record material specific discharge capacity under discharge current density 0.1C, 1C, 3C, 5C, 10C and reach 130.0mAh g respectively -1, 123.5mAh g -1, 116.3mAh g -1, 111.2mAh g -1, 102.0mAh g -1.50 capability retentions that circulate under 10C are 92%.
Embodiment 3
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.7 is by LiCoPO coated for carbon in mass ratio 4mix with phosphoric acid, at 200 DEG C of temperature in vacuum drying chamber dry 24h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 500 DEG C of 10 DEG C/min, calcining at constant temperature 4h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 3.Be assembled into battery to record material specific discharge capacity under discharge current density 0.05C, 0.1C, 1C, 5C, 20C and reach 145.2mAh g respectively -1, 143.5mAh g -1, 140.2mAh g -1, 131.3mAh g -1, 112.4mAh g -1.
Embodiment 4
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.1 is by LiNi coated for carbon in mass ratio 1/3co 1/3mn 1/3o 2mix with triphenyl phosphorus, at 120 DEG C of temperature in vacuum drying chamber dry 12h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 1000 DEG C of 10 DEG C/min, calcining at constant temperature 5h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 4.Be assembled into battery to record material specific discharge capacity under discharge current density 0.1C, 0.2C, 1C, 2C, 5C and reach 177.1mAh g respectively -1, 153.3mAh g -1, 144.6mAh g -1, 130.3mAh g -1, 92.4mAh g -1.
Experiment proves, adopts LiNi xco ymn 1-x-yo 2, be 0.4 when x is 0.1, y; Or x to be 0.4, y be 0.1 replaces anode material for lithium-ion batteries in the present embodiment respectively, other same the present embodiment, the character of the P Modification carbon-coated lithium ion battery anode composite material of preparation is similar to the present embodiment.
Embodiment 5
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.3 is by Li coated for carbon in mass ratio 4ti 5o 12mix with triphenyl phosphorus, at 150 DEG C of temperature in vacuum drying chamber dry 8h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 300 DEG C of 1 DEG C/min, calcining at constant temperature 6h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 5.Be assembled into battery to record material specific discharge capacity under discharge current density 0.5C, 1C, 5C, 10C, 20C and reach 161.0mAh g respectively -1, 152.5mAh g -1, 143.2mAh g -1, 112.8mAh g -1, 91.2mAh g -1.
Embodiment 6
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.1 is by Li coated for carbon in mass ratio 2feSiO 4mix with pyrophosphoric acid, at 100 DEG C of temperature in vacuum drying chamber dry 24h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 800 DEG C of 5 DEG C/min, calcining at constant temperature 2h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 6.Be assembled into battery to record material specific discharge capacity under discharge current density 0.1C, 0.2C, 0.5C, 1C, 5C and reach 164.7mAh g respectively -1, 159.2mAh g -1, 150.0mAh g -1, 140.3mAh g -1, 98.5mAh g -1.
Embodiment 7
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.2 is by Li coated for carbon in mass ratio 3v 2(PO 4) 3mix with metaphosphoric acid, at 200 DEG C of temperature in vacuum drying chamber dry 12h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 900 DEG C of 3 DEG C/min, calcining at constant temperature 1h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 7.Be assembled into battery to record material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reach 167.4mAh g respectively -1, 149.5mAh g -1, 132.5mAh g -1, 121.3mAh g -1, 102.8mAh g -1.
Embodiment 8
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.5 is by LiFePO coated for carbon in mass ratio 4mix with ammonium phosphate, at 100 DEG C of temperature in vacuum drying chamber dry 10h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 600 DEG C of 5 DEG C/min, calcining at constant temperature 4h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 8.Be assembled into battery to record material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reach 166.1mAh g respectively -1, 155.8mAh g -1, 145.0mAh g -1, 136.9mAh g -1, 125.8mAh g -1.
Embodiment 9
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.7 is by LiFePO coated for carbon in mass ratio 4mix with ammonium dihydrogen phosphate, at 120 DEG C of temperature in vacuum drying chamber dry 10h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 600 DEG C of 6 DEG C/min, calcining at constant temperature 4h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 9.Be assembled into battery to record material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reach 165.4mAh g respectively -1, 153.9mAh g -1, 142.5mAh g -1, 135.3mAh g -1, 124.8mAh g -1.
Embodiment 10
A preparation method for P Modification carbon-coated lithium ion battery anode composite material, comprises the steps:
(1) be that the ratio of 1:0.2 is by Li coated for carbon in mass ratio 4ti 5o 12mix with phosphorous acid, at 100 DEG C of temperature in vacuum drying chamber dry 8h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with the ramp to 700 DEG C of 5 DEG C/min, calcining at constant temperature 3h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made according to method described in embodiment 1 by obtaining P Modification carbon-coated lithium ion battery anode composite material in embodiment 10.Be assembled into battery to record material specific discharge capacity under discharge current density 0.5C, 1C, 5C, 10C, 20C and reach 161.4mAh g respectively -1, 151.7mAh g -1, 142.8mAh g -1, 113.3mAh g -1, 92.8mAh g -1.

Claims (5)

1. a preparation method for P Modification carbon-coated lithium ion battery anode composite material, is characterized in that comprising the steps:
(1) in mass ratio for 1:(0.1 ~ 1) ratio anode material for lithium-ion batteries coated for carbon is mixed with phosphorus source, at 100 ~ 200 DEG C of temperature in vacuum drying chamber drying 8 ~ 24h, obtain powder after grinding;
(2) powder that step (1) obtains is placed in tube furnace, under nitrogen protection, with ramp to 300 ~ 1000 DEG C of 1 ~ 10 DEG C/min, calcining at constant temperature 1 ~ 6h, obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
2. the preparation method of a kind of P Modification carbon-coated lithium ion battery anode composite material according to claim 1, is characterized in that described phosphorus source is triphenyl phosphorus, phosphoric acid, phosphorous acid, pyrophosphoric acid, metaphosphoric acid, ammonium phosphate or ammonium dihydrogen phosphate.
3. the preparation method of a kind of P Modification carbon-coated lithium ion battery anode composite material according to claim 1, is characterized in that described anode material for lithium-ion batteries is LiFePO 4, LiMnPO 4, LiCoPO 4, Li 4ti 5o 12, Li 2feSiO 4, Li 3v 2(PO 4) 3or LiNi xco ymn 1-x-yo 2, wherein 0<x<0.5; 0<y<0.5.
4. the P Modification carbon-coated lithium ion battery anode composite material prepared of the method for one of claim 1-3.
5. the purposes of the P Modification carbon-coated lithium ion battery anode composite material of claim 4.
CN201410448588.7A 2014-09-04 2014-09-04 P Modification carbon-coated lithium ion battery anode composite material and Preparation method and use Active CN104332612B (en)

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CN106876686A (en) * 2017-04-14 2017-06-20 中南大学 A kind of method for carrying out surface modification with positive electrode active materials to lithium ion battery
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