CN104332612B - P Modification carbon-coated lithium ion battery anode composite material and Preparation method and use - Google Patents
P Modification carbon-coated lithium ion battery anode composite material and Preparation method and use Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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Abstract
The invention discloses a kind of P Modification carbon-coated lithium ion battery anode composite material and Preparation method and use, preparation method is：(1) it is 1 in mass ratio：The anode material for lithium-ion batteries of carbon coating is well mixed by the ratio of (0.1~1) with phosphorus source, dries 8~24h in vacuum drying chamber at a temperature of 100~200 DEG C, powder is obtained after grinding；(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 300~1000 DEG C with 1~10 DEG C/min speed, 1~6h of calcining at constant temperature obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.The method raw material sources of the present invention are extensive, cheap, synthesis technique is simple, process conditions are easily controllable and safety and environmental protection, it is adapted to industrialized production, the P Modification carbon-coated lithium ion battery anode composite material prepared with the method for the present invention has the preferably chemical property such as circulation performance under high magnification.
Description
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 lithium ion
Cell positive material technical field.
Background technology
The lithium ion battery of environmental protection is the novel power supply system grown up early 1990s, due to its work
Voltage height, small volume, light weight, memory-less effect, have extended cycle life, it is pollution-free the features such as be valued by people and favor,
It is the green high-capacity rechargeable battery of a new generation.It makees positive pole with embedding lithium carbon material instead of lithium metal, overcome conventional lithium battery because
The defect in circulating and reversible performance and security performance caused by Li dendrite, had both maintained lithium battery high voltage, high-energy-density etc.
Key property, have again temperature in use scope wide (37 DEG C~60 DEG C), have extended cycle life, self-discharge rate is few, memory-less effect, can be fast
The prominent advantages such as fast charging, non-environmental-pollution, are new after traditional lead-acid accumulator, ickel-cadmium cell, Ni-H cell
Generation battery.But, lithium ion battery comes out only more than ten years, and it has manifested clearly disadvantageous, and such as cost is higher, multiplying power
Poor performance etc..Therefore, the scientific and technological circle and industrial quarters in the whole world are devoted to improve the correlation technique of lithium ion battery, study and open
Lithium ion battery new material is sent out, its performance is improved, reduces its cost.
It is in recent years the rate capability of lifting anode material for lithium-ion batteries, overcomes inherent defect, improve its electrochemistry
Can, the main method used at present includes following two：(1) prepare more tiny homogeneous particle to shorten using new method
Lithium ion diffusion length, makes the rate capability of electrode material get a promotion；(2) sheet conductivity material is carried out on material granule surface
Material is coated with the electrical contact in the electric conductivity on lifting surface and electrode, such as material surface carbon coating.It is more both domestic and external at present
Scholar has done further improve to material carbon coating layer and studied, and mainly carries out nitrogen modification to carbon coating layer.But not yet have pair
Carbon coating layer carries out the report of P Modification.
The content of the invention
Extensive, cheap it is an object of the invention to provide a kind of raw material sources, synthesis technique is simple, process conditions are easy to
Control and safety and environmental protection, are adapted to the preparation method of the P Modification carbon-coated lithium ion battery anode composite material of industrialized production.
Second object of the present invention is to provide a kind of P Modification carbon-coated lithium ion with good chemical property
Battery anode composite material.
Third object of the present invention is to provide a kind of purposes of P Modification carbon-coated lithium ion battery anode composite material.
The method of the present invention is summarized as follows：
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：The ratio of (0.1~1) mixes the anode material for lithium-ion batteries of carbon coating with phosphorus source
It is even, 8~24h is dried in vacuum drying chamber at a temperature of 100~200 DEG C, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, with 1~10 DEG C/min speed liter
Temperature is to 300~1000 DEG C, and 1~6h of calcining at constant temperature obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
The preferred triphenyl phosphorus of phosphorus source, phosphoric acid, phosphorous acid, pyrophosphoric acid, metaphosphoric acid, ammonium phosphate or ammonium dihydrogen phosphate.
Anode material for lithium-ion batteries is preferably LiFePO4、LiMnPO4、LiCoPO4、Li4Ti5O12、Li2FeSiO4、Li3V2
(PO4)3Or LiNixCoyMn1-x-yO2, wherein 0<x<0.5；0<y<0.5.
P Modification carbon-coated lithium ion battery anode composite material prepared by the above method.
Above-mentioned P Modification carbon-coated lithium ion battery anode composite material is preparing the purposes of battery.
The advantage of the invention is that：The method raw material sources of the present invention are extensive, cheap, and synthesis technique is simple, technique
Condition is easily controllable and safety and environmental protection, is adapted to industrialized production, the P Modification carbon-coated lithium ion prepared with the method for the present invention
Battery anode composite material has the preferably chemical property such as circulation performance under high magnification.
Brief description of the drawings
Fig. 1 is the XRD spectrum 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 photograph 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 of the anode material for lithium-ion batteries for the carbon coating that Fig. 3 is used by the embodiment of the present invention 1
Figure.
Fig. 4 is that P Modification carbon-coated lithium ion battery anode composite material prepared by the embodiment of the present invention 1 is used as lithium ion
The rate charge-discharge curve map of cell positive material.
Fig. 5 is that P Modification carbon-coated lithium ion battery anode composite material prepared by the embodiment of the present invention 1 is used as lithium ion
The cycle performance curve map of cell positive material.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.The following examples are in order that this area
Technical staff better understood when the present invention, but the present invention not imposed any restrictions.
The anode material for lithium-ion batteries for the carbon coating that various embodiments of the present invention are used is commercially produced product.
Embodiment 1
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.5 ratio is by the LiFePO of carbon coating4It is well mixed with triphenyl phosphorus, in 100 DEG C of temperature
10h is dried under degree in vacuum drying chamber, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 5 DEG C/min speed
600 DEG C, calcining at constant temperature 3h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
Battery is made in the above-mentioned P Modification carbon-coated lithium ion battery anode composite material that obtains by the following method：
P Modification carbon-coated lithium ion battery anode composite material, conductive agent (acetylene black), binding agent are gathered into inclined difluoro second
Alkene (PVDF) in mass ratio 80:10:10 mixing, add appropriate 1-METHYLPYRROLIDONE (NMP) and are used as dispersant, magnetic agitation
10h is well mixed, and uniform film is then spread on clean aluminium foil, then film is placed in into drying in 80 DEG C of vacuum drying chambers
12h, tabletting punching obtains pole piece, and battery is assembled into glove box.
The XRD spectrum of P Modification carbon-coated lithium ion battery anode composite material made from embodiment 1 is as shown in figure 1, originally
The peak position of material and the peak position of standard card (JCPDS#40-1499) are completely the same, and provable material is LiFePO4 pure phase,
P Modification does not influence on material purity.The diffraction maximum of LiFePO4 is clearly sharp, illustrates obtained LiFePO 4 material crystallization
Property is good.The SEM photograph of P Modification carbon-coated lithium ion battery anode composite material is as shown in Fig. 2 material made from embodiment 1
Grain is club shaped structure, width~100nm, length~200nm.
It is assembled into battery and measures material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reaches respectively
165.5mAh g-1、154.1mAh g-1、143.3mAh g-1、134.1mAh g-1、124.0mAh g-1, circulated 50 times under 20C
Capability retention is 90%, sees Fig. 4, Fig. 5.
The anode material for lithium-ion batteries for the raw material carbon coating that Fig. 3 is used by the present embodiment by the present embodiment method system
The rate charge-discharge curve map of standby battery.
Embodiment 2
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：1 ratio is by the LiMnPO of carbon coating4It is well mixed with metaphosphoric acid, at a temperature of 120 DEG C
8h is dried in vacuum drying chamber, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 7 DEG C/min speed
700 DEG C, calcining at constant temperature 2h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 2 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity under discharge current density 0.1C, 1C, 3C, 5C, 10C and reaches respectively
130.0mAh g-1、123.5mAh g-1、116.3mAh g-1、111.2mAh g-1、102.0mAh g-1.Circulated 50 times under 10C
Capability retention is 92%.
Embodiment 3
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.7 ratio is by the LiCoPO of carbon coating4It is well mixed with phosphoric acid, at a temperature of 200 DEG C
24h is dried in vacuum drying chamber, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is heated up with 10 DEG C/min speed
To 500 DEG C, calcining at constant temperature 4h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 3 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity difference under discharge current density 0.05C, 0.1C, 1C, 5C, 20C
Up to 145.2mAh g-1、143.5mAh g-1、140.2mAh g-1、131.3mAh g-1、112.4mAh g-1。
Embodiment 4
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.1 ratio is by the LiNi of carbon coating1/3Co1/3Mn1/3O2It is well mixed with triphenyl phosphorus,
12h is dried in vacuum drying chamber at a temperature of 120 DEG C, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is heated up with 10 DEG C/min speed
To 1000 DEG C, calcining at constant temperature 5h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 4 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity under discharge current density 0.1C, 0.2C, 1C, 2C, 5C and reaches respectively
177.1mAh g-1、153.3mAh g-1、144.6mAh g-1、130.3mAh g-1、92.4mAh g-1。
It is demonstrated experimentally that using LiNixCoyMn1-x-yO2, when x is that 0.1, y is 0.4；Or x is that 0.4, y is 0.1 replacement respectively
Anode material for lithium-ion batteries in embodiment, other same the present embodiment, the P Modification carbon-coated lithium ion battery positive pole of preparation
The property of composite is similar to the present embodiment.
Embodiment 5
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.3 ratio is by the Li of carbon coating4Ti5O12It is well mixed with triphenyl phosphorus, at 150 DEG C
At a temperature of in vacuum drying chamber dry 8h, obtain powder after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 1 DEG C/min speed
300 DEG C, calcining at constant temperature 6h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 5 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity under discharge current density 0.5C, 1C, 5C, 10C, 20C and reaches respectively
161.0mAh g-1、152.5mAh g-1、143.2mAh g-1、112.8mAh g-1、91.2mAh g-1。
Embodiment 6
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.1 ratio is by the Li of carbon coating2FeSiO4It is well mixed with pyrophosphoric acid, in 100 DEG C of temperature
24h is dried under degree in vacuum drying chamber, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 5 DEG C/min speed
800 DEG C, calcining at constant temperature 2h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 6 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity difference under discharge current density 0.1C, 0.2C, 0.5C, 1C, 5C
Up to 164.7mAh g-1、159.2mAh g-1、150.0mAh g-1、140.3mAh g-1、98.5mAh g-1。
Embodiment 7
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.2 ratio is by the Li of carbon coating3V2(PO4)3It is well mixed with metaphosphoric acid, at 200 DEG C
At a temperature of in vacuum drying chamber dry 12h, obtain powder after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 3 DEG C/min speed
900 DEG C, calcining at constant temperature 1h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 7 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reaches respectively
167.4mAh g-1、149.5mAh g-1、132.5mAh g-1、121.3mAh g-1、102.8mAh g-1。
Embodiment 8
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.5 ratio is by the LiFePO of carbon coating4It is well mixed with ammonium phosphate, in 100 DEG C of temperature
Under in vacuum drying chamber dry 10h, obtain powder after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 5 DEG C/min speed
600 DEG C, calcining at constant temperature 4h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 8 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reaches respectively
166.1mAh g-1、155.8mAh g-1、145.0mAh g-1、136.9mAh g-1、125.8mAh g-1。
Embodiment 9
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.7 ratio is by the LiFePO of carbon coating4It is well mixed with ammonium dihydrogen phosphate, at 120 DEG C
At a temperature of in vacuum drying chamber dry 10h, obtain powder after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 6 DEG C/min speed
600 DEG C, calcining at constant temperature 4h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 9 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity under discharge current density 0.1C, 1C, 5C, 10C, 20C and reaches respectively
165.4mAh g-1、153.9mAh g-1、142.5mAh g-1、135.3mAh g-1、124.8mAh g-1。
Embodiment 10
A kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, comprises the following steps：
(1) it is 1 in mass ratio：0.2 ratio is by the Li of carbon coating4Ti5O12It is well mixed with phosphorous acid, in 100 DEG C of temperature
8h is dried under degree in vacuum drying chamber, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 5 DEG C/min speed
700 DEG C, calcining at constant temperature 3h obtains a kind of P Modification carbon-coated lithium ion battery anode composite material.
P Modification carbon-coated lithium ion battery anode composite material will be obtained in embodiment 10 according to the methods described of embodiment 1
Battery is made.It is assembled into battery and measures material specific discharge capacity under discharge current density 0.5C, 1C, 5C, 10C, 20C and reaches respectively
161.4mAh g-1、151.7mAh g-1、142.8mAh g-1、113.3mAh g-1、92.8mAh g-1。
Claims (4)
1. a kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material, it is characterized in that comprising the following steps：
(1) it is 1 in mass ratio：The anode material for lithium-ion batteries of carbon coating is well mixed by the ratio of (0.1~1) with phosphorus source,
8~24h is dried in vacuum drying chamber at a temperature of 100~200 DEG C, powder is obtained after grinding；
(2) powder for obtaining step (1) is placed in tube furnace, under nitrogen protection, is warming up to 1~10 DEG C/min speed
300~1000 DEG C, 1~6h of calcining at constant temperature obtains a kind of P Modification carbon-coated lithium ion battery anode composite material；
Phosphorus source is triphenyl phosphorus, phosphoric acid, phosphorous acid, pyrophosphoric acid, metaphosphoric acid, ammonium phosphate or ammonium dihydrogen phosphate.
2. a kind of preparation method of P Modification carbon-coated lithium ion battery anode composite material according to claim 1, its
It is characterized in that the anode material for lithium-ion batteries is LiFePO4、LiMnPO4、LiCoPO4、Li4Ti5O12、Li2FeSiO4、Li3V2
(PO4)3Or LiNixCoyMn1-x-yO2, wherein 0<x<0.5；0<y<0.5.
3. P Modification carbon-coated lithium ion battery anode composite material prepared by the method for claim 1 or 2.
4. the purposes of the P Modification carbon-coated lithium ion battery anode composite material of claim 3.
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| CN103887477A (en) * | 2013-12-27 | 2014-06-25 | 杭州金马能源科技有限公司 | Preparation method of high-volume graphene-modified lithium iron phosphate positive electrode material |
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