CN102169986B - Preparation method of lithium ferric phosphate / grapheme composite positive electrode material - Google Patents
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Abstract
The invention discloses a preparation method of a lithium ferric phosphate / grapheme composite positive electrode material. The method comprises the following steps of: (1) preparing a lithium ferric phosphate precursor, namely weighing raw materials such as a catalyst, lithium salt, ferric salt and phosphate, adding the raw materials into a dispersing agent, and ball-milling to obtain the lithium ferric phosphate precursor; and (2) growing grapheme on the lithium ferric phosphate precursor first, then closing carbon source gas and ammonia gas, introducing hydrogen into a reactor, adjusting the temperature of the interior of the reactor to be 600 to 800 DEG C at a speed of 10 to 20 DEG C per minute in the process of hydrogen introduction, keeping the temperature of the interior of the reactor constant for 24 to 48 hours, and then cooling a product which is obtained in the reactor in the nitrogen atmosphere to room temperature so as to prepare the lithium ferric phosphate / grapheme composite positive electrode material. The lithium ferric phosphate / grapheme composite positive electrode material which is prepared by the method is high in conducting performance and high in power multiplying performance.
Description
Technical field
The present invention relates to the anode material for lithium-ion batteries technical field, be specifically related to a kind of preparation method of lithium ferric phosphate/grapheme composite positive electrode material.
Background technology
Ferric phosphate lithium cell is a kind of Novel power battery grown up in recent years, ferric phosphate lithium cell because of its have use safely, have extended cycle life, the advantages such as capacity is large, high temperature resistant and environmental protection become the focus of research in recent years.But the poorly conductive of LiFePO4, the lithium ion diffusion velocity is slow, and during high power charging-discharging, actual specific capacity is low, and these problems are restricting the development of LiFePO4 industrialization.For improving conductivity and the high rate performance of ferric phosphate lithium cell, in the manufacturing process of lithium ion battery electrode piece, add the chemical property that conductive agent can improve lithium ion battery in positive electrode, although the conductive additive proportion is little, its degree of crystallinity, form and addition etc. are very big to the battery charging and discharging performance impact.The conductive agent added in the LiFePO4 the inside at present mainly contains acetylene black, Supper P, carbon fiber and carbon nano-tube, as in the Chinese patent application that is 200910220007.3 at application number, disclosed in the collosol and gel presoma and added carbon nano-tube, and on the basis that provides active particle carbon to coat at sol-gal process, improve contacting between particle and particle by carbon nano-tube, strengthen the conductive network of carbon, thereby improved the chemical property of lithium ion battery.But because conductivity and the specific area of carbon nano-tube are limited, limited to the cycle life effect of the internal resistance that reduces battery, the multiplying power that improves battery and raising battery.
Graphene is a kind of new material risen rapidly in recent years, and its structure can be understood as the graphite of individual layer, therefore has extremely good conductivity, and the movement velocity of its electronics has reached 1.0 * 10
6s/m, much larger than the conductivity 1.0 * 10 of carbon nano-tube
4, also there is good conductive performance in s/m for lithium ion battery.And the two-dimensional nano layer structure of Graphene uniqueness and the huge characteristics such as specific area make Graphene have more outstanding advantage than carbon nano-particle or carbon nanocoils etc. as additive agent modified LiFePO 4 material the time
.adding grapheme material in the LiFePO4 the inside at present is mainly to pass through physical doping, directly add Graphene and prepare lithium ferric phosphate/grapheme composite positive electrode material in the LiFePO4 the inside, as disclosed a kind of composite positive pole at the LiFePO4 doped graphene in the Chinese patent application that is 201010146161.3 at application number, the conductivity of its material is improved.But very easily cause the skewness of Graphene in LiFePO4 owing to directly adding Graphene in LiFePO4, the phenomenons such as reunion occur, the lithium ferric phosphate/grapheme composite positive electrode material electric conductivity, the high rate performance that therefore adopt current preparation method to make are not very good.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of lithium ferric phosphate/grapheme composite positive electrode material, electric conductivity and the high rate performance of the lithium ferric phosphate/grapheme composite positive electrode material that adopts the method to make significantly improve.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of preparation method of lithium ferric phosphate/grapheme composite positive electrode material comprises the steps:
(1) prepare ferric lithium phosphate precursor
Press following component and mass percentage content raw materials weighing: catalyst 1%-15%, lithium salts 5%-15%, molysite 40%-60% and phosphate 25%-45%; Described catalyst is one or more in iron, cobalt, nickel; Described lithium salts is one or more in lithium carbonate, lithium hydroxide, lithium nitrate and lithium phosphate; Described molysite is one or more in ferrous oxalate, di-iron trioxide, tri-iron tetroxide and ferric phosphate; Described phosphate is one or more of ammonium dihydrogen phosphate, ammonium phosphate or diammonium hydrogen phosphate; Above-mentioned raw materials is added in dispersant, through ball milling, make ferric lithium phosphate precursor; Described dispersant is distilled water or absolute ethyl alcohol;
(2) prepare lithium ferric phosphate/grapheme composite positive electrode material
At first growing graphene on described ferric lithium phosphate precursor: the ferric lithium phosphate precursor that step (1) makes is put into reactor after drying, pass into nitrogen or hydrogen in described reactor, and heating makes the temperature in reactor reach 500-1200 ℃, stop passing into nitrogen or hydrogen, pass into carbon-source gas and ammonia afterwards in described reactor, keep 20-60 minute under 500-1200 ℃, at ferric lithium phosphate precursor superficial growth Graphene; In carbon-source gas, the purpose of doping ammonia is to change the upgrowth situation of carbon-source gas on the ferric lithium phosphate precursor surface, to guarantee to prepare the grapheme material of sheet;
Close afterwards carbon-source gas and ammonia, pass into hydrogen again in described reactor, speed with 10 ℃～20 ℃/minute in passing into the process of hydrogen is adjusted to 600 ~ 800 ℃ by the temperature in reactor, then constant temperature is 24～48 hours, in reactor, products therefrom is cooled to room temperature again under nitrogen atmosphere afterwards, makes lithium ferric phosphate/grapheme composite positive electrode material; The mist that wherein said carbon-source gas is methane gas, acetylene gas or acetylene and argon gas.
Described catalyst is superfine powder, and its particle diameter is 1 ~ 200nm.The superfine powder catalyst has the characteristics of granule and bigger serface, so the superfine powder catalyst has, and catalysis is even, catalytic capability reaches by force the advantages such as permeability is strong.
When described dispersant is distilled water, the quality of distilled water: (catalyst quality+lithium salts quality+molysite quality+phosphate quality)=5:1; When described dispersant is absolute ethyl alcohol, the quality of absolute ethyl alcohol: (catalyst quality+lithium salts quality+molysite quality+phosphate quality)=10:1.Select above-mentioned quality proportioning can guarantee that the dispersion liquid be mixed with disperses homogeneous, stable.
When mist that described carbon-source gas is acetylene and argon gas, the volume ratio of acetylene and argon gas is: acetylene: argon gas=1:9; In acetylene gas, mix a certain amount of inert gas argon gas can make the grapheme material that grows evenly, high conformity.
The preparation method of lithium ferric phosphate/grapheme composite positive electrode material provided by the invention passes through the chemical vapour deposition technique growing graphene on the ferric lithium phosphate precursor surface, and then by the standby lithium ferric phosphate/grapheme composite positive electrode material that obtains of high temperature reduction legal system.Because the present invention adopts chemical vapour deposition technique at ferric lithium phosphate precursor superficial growth Graphene, therefore can realize Graphene being uniformly distributed on the ferric lithium phosphate precursor surface, thoroughly solve the skewness of Graphene in LiFePO4, be prone to the problems such as reunion.The lithium ferric phosphate/grapheme composite positive electrode material electric conductivity, the good rate capability that adopt the inventive method to make.The battery that the lithium ferric phosphate/grapheme composite positive electrode material that adopts the inventive method to make is prepared has the advantages such as internal resistance is low, multiplying power good, have extended cycle life, the 5AH soft-package battery of preparing is that the capability retention recorded under the 4C condition significantly improves in multiplying power, reaches 92.4%.
Compared with prior art, the present invention has following advantage: (1) can realize the even growth of Graphene on the LiFePO4 surface, the adverse effects such as reunion of Graphene have been avoided, the advantage such as the battery that the composite positive pole of preparing is made as positive electrode has that resistance is little, multiplying power good, has extended cycle life, excellent radiation performance; (2) the present invention is when preparing ferric lithium phosphate precursor, metal Fe, Co, Ni catalyst have been introduced in scene, prepare lithium ferric phosphate/grapheme composite positive electrode material as cation doping in catalysis ferric lithium phosphate precursor superficial growth Graphene, this method situ growth Graphene, solved the difficult problem of dispersed graphite alkene in the slurry of high viscosity and high solids content, Graphene is as in conductive agent doping introducing LiFePO4 simultaneously, both improve the ionic conductivity of LiFePO4, improved again electronic conductivity; (3) can realize the controlled preparation to lithium ferric phosphate/grapheme composite positive electrode material, the flow of hydrogen can be prepared the different lithium ferric phosphate/grapheme composite positive electrode materials that form when adjusting catalyst, lithium salts, molysite and phosphatic proportioning and high temperature reduction, thereby accomplishes the controlled preparation to lithium ferric phosphate/grapheme composite positive electrode material.
The accompanying drawing explanation
The voltage that Fig. 1 is battery A-discharge capacity curve chart;
The voltage that Fig. 2 is battery B-discharge capacity curve chart;
The voltage that Fig. 3 is battery C-discharge capacity curve chart;
The voltage that Fig. 4 is battery D-discharge capacity curve chart.
Embodiment
The preparation method of the present embodiment lithium ferric phosphate/grapheme composite positive electrode material, concrete steps are as follows:
(1) prepare ferric lithium phosphate precursor
Iron powder, 37g lithium carbonate, 173g ferrous oxalate and 116g ammonium dihydrogen phosphate that to take the 6g particle diameter be 20nm, put into ball grinder, in ball grinder, add the 3320g absolute ethyl alcohol to make dispersant again, put into the ball mill ball milling 6 hours, make ferric lithium phosphate precursor;
(2) prepare lithium ferric phosphate/grapheme composite positive electrode material
At first growing graphene on ferric lithium phosphate precursor: the ferric lithium phosphate precursor that step (1) makes was 60 ℃ of vacuumizes 12 hours, put into afterwards tube furnace, tube furnace is vacuumized, pass into nitrogen afterwards in tube furnace, and heating makes the temperature in tube furnace reach 800 ℃, now stop passing into nitrogen, ventilating methane gas and ammonia in the changed course tube furnace, the methane gas flow is 200sccm, ammonia flow is 50sccm, at 800 ℃, keep 60 minutes, at ferric lithium phosphate precursor superficial growth Graphene;
Close afterwards methane gas and ammonia, pass into hydrogen again in tube furnace, in passing into the process of hydrogen, the temperature in tube furnace is controlled to 800 ℃, and constant temperature keeps 24 hours, in tube furnace, products therefrom is cooled to room temperature again under nitrogen atmosphere afterwards, makes lithium ferric phosphate/grapheme composite positive electrode material.
The preparation method of the present embodiment lithium ferric phosphate/grapheme composite positive electrode material, concrete steps are as follows:
(1) prepare ferric lithium phosphate precursor
Cobalt powder, 10g lithium nitrate, 45g ferric phosphate and 30g diammonium hydrogen phosphate that to take the 10g particle diameter be 1nm, put into ball grinder, then add 475g distilled water to make dispersant in ball grinder, puts into the ball mill ball milling 6 hours, makes ferric lithium phosphate precursor;
(2) prepare lithium ferric phosphate/grapheme composite positive electrode material
At first growing graphene on ferric lithium phosphate precursor: the ferric lithium phosphate precursor that step (1) makes was 60 ℃ of vacuumizes 12 hours, put into afterwards tube furnace, tube furnace is vacuumized, pass into hydrogen afterwards in tube furnace, and heating makes the temperature in tube furnace reach 500 ℃, now stop passing into hydrogen, logical acetylene gas and ammonia in the changed course tube furnace, the acetylene gas flow is 150sccm, ammonia flow is 50sccm, at 500 ℃, keep 60 minutes, at ferric lithium phosphate precursor superficial growth Graphene;
Close afterwards acetylene gas and ammonia, pass into hydrogen again in tube furnace, programming rate with 10 ℃/minute in passing into the process of hydrogen controls to 600 ℃ by the temperature in tube furnace, and constant temperature keeps 48 hours, in tube furnace, products therefrom is cooled to room temperature again under nitrogen atmosphere afterwards, makes lithium ferric phosphate/grapheme composite positive electrode material.
The preparation method of the present embodiment lithium ferric phosphate/grapheme composite positive electrode material, concrete steps are as follows:
(1) prepare ferric lithium phosphate precursor
Take the 5g particle diameter iron powder that is 200nm, nickel powder, 15g lithium hydroxide, 40g tri-iron tetroxide and the 30g ammonium phosphate that the 10g particle diameter is 100nm, put into ball grinder, in ball grinder, add 500g distilled water to make dispersant again, put into the ball mill ball milling 6 hours, make ferric lithium phosphate precursor;
(2) prepare lithium ferric phosphate/grapheme composite positive electrode material
At first growing graphene on ferric lithium phosphate precursor: the ferric lithium phosphate precursor that step (1) makes was 60 ℃ of vacuumizes 12 hours, put into afterwards tube furnace, tube furnace is vacuumized, pass into nitrogen afterwards in tube furnace, and heating makes the temperature in tube furnace reach 1200 ℃, now stop passing into nitrogen, mist and the ammonia of logical acetylene and argon gas in the changed course tube furnace, the flow of the mist of acetylene and argon gas is 220sccm, in the mist of acetylene and argon gas, the volume ratio of acetylene and argon gas is: acetylene: argon gas=1:9, ammonia flow is 50sccm, at 1200 ℃, keep 20 minutes, at ferric lithium phosphate precursor superficial growth Graphene,
Close afterwards mist and the ammonia of acetylene and argon gas, pass into hydrogen again in tube furnace, cooling rate with 20 ℃/minute in passing into the process of hydrogen controls to 600 ℃ by the temperature in tube furnace, and constant temperature keeps 24 hours, in tube furnace, products therefrom is cooled to room temperature again under nitrogen atmosphere afterwards, makes lithium ferric phosphate/grapheme composite positive electrode material.
The lithium ferric phosphate/grapheme composite positive electrode material that the embodiment 1-embodiment 3 of usining respectively makes is as positive electrode, and Delanium, as negative material, adopts LiPF
6/ EC+DEC(volume ratio 1: 1) be electrolyte, Celgard 2400 films are barrier film, preparation 5AH soft-package battery, and the code name of the battery of embodiment 1 correspondence is battery A, the code name of the battery of embodiment 2 correspondences is battery B, and the code name of the battery of embodiment 3 correspondences is battery C; The lithium ferric phosphate/grapheme composite positive electrode material that the prior art of usining makes is as positive electrode, and Delanium, as negative material, adopts LiPF
6/ EC+DEC(volume ratio 1: 1) be electrolyte, Celgard 2400 films are barrier film, also prepare the 5AH soft-package battery, battery as a comparison, and code name is battery D.The internal resistance of 4 5AH soft-package batteries that mensuration makes, the results are shown in Table shown in 1.
The internal resistance data of the 5AH soft-package battery that table 1 makes
As can be seen from Table 1, the internal resistance of cell that the lithium ferric phosphate/grapheme composite positive electrode material that the battery that the lithium ferric phosphate/grapheme composite positive electrode material that adopts the inventive method to make is prepared makes than art methods is prepared obviously reduces, and cycle life extends.
Measure battery A, B, C, the voltage of D under different multiplying and the relation of discharge capacity, draw voltage-discharge capacity curve chart, see shown in Fig. 1-Fig. 4.From Fig. 1-4, can find out, the battery that the lithium ferric phosphate/grapheme composite positive electrode material that the battery that the lithium ferric phosphate/grapheme composite positive electrode material that adopts the inventive method to make is prepared adopts art methods to make is prepared has raising preferably aspect multiplying power, under its condition that is 4C in multiplying power, battery A, B, the capability retention of C is respectively 92.4%, 86.1%, 86.3%, and the capability retention of battery D is 83.9%, can find out and adopt the battery that lithium ferric phosphate/grapheme composite positive electrode material that battery that lithium ferric phosphate/grapheme composite positive electrode material that the inventive method makes is prepared makes than art methods is prepared thering is obvious effect aspect the multiplying power that improves battery.
Claims (2)
1. the preparation method of a lithium ferric phosphate/grapheme composite positive electrode material, is characterized in that, comprises the steps:
(1) prepare ferric lithium phosphate precursor
Press following component and mass percentage content raw materials weighing: one or more 25%-45% of catalyst 1%-15%, lithium salts 5%-15%, molysite 40%-60% and ammonium dihydrogen phosphate, ammonium phosphate or diammonium hydrogen phosphate; Described catalyst is one or more in iron, cobalt, nickel; Described lithium salts is one or more in lithium carbonate, lithium nitrate and lithium phosphate; Described molysite is one or more in ferrous oxalate and ferric phosphate; Above-mentioned raw materials is added in dispersant, through ball milling, make ferric lithium phosphate precursor; Described dispersant is distilled water or absolute ethyl alcohol;
(2) prepare lithium ferric phosphate/grapheme composite positive electrode material
At first growing graphene on described ferric lithium phosphate precursor: the ferric lithium phosphate precursor that step (1) makes is put into reactor after drying, pass into nitrogen or hydrogen in described reactor, and heating makes the temperature in reactor reach 500-1200 ℃, stop passing into nitrogen or hydrogen, pass into carbon-source gas and ammonia afterwards in described reactor, keep 20-60 minute under 500-1200 ℃, at ferric lithium phosphate precursor superficial growth Graphene;
Close afterwards carbon-source gas and ammonia, pass into hydrogen again in described reactor, speed with 10 ℃～20 ℃/minute in passing into the process of hydrogen is adjusted to 600～800 ℃ by the temperature in reactor, then constant temperature is 24～48 hours, in reactor, products therefrom is cooled to room temperature again under nitrogen atmosphere afterwards, makes lithium ferric phosphate/grapheme composite positive electrode material; The mist that wherein said carbon-source gas is methane gas, acetylene gas or acetylene and argon gas;
When described dispersant is distilled water, the quality of distilled water: (catalyst quality+lithium salts quality+molysite quality+phosphate quality)=5:1; When described dispersant is absolute ethyl alcohol, the quality of absolute ethyl alcohol: (catalyst quality+lithium salts quality+molysite quality+phosphate quality)=10:1;
During mist that described carbon-source gas is acetylene and argon gas, in the mist of acetylene and argon gas, the volume ratio of acetylene and argon gas is: acetylene: argon gas=1:9.
2. the preparation method of lithium ferric phosphate/grapheme composite positive electrode material according to claim 1, is characterized in that, described catalyst is superfine powder, and its particle diameter is 1～200nm.
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| CN102553593B (en) * | 2012-01-10 | 2014-10-29 | 常州大学 | Method for preparing magnetic nanometer ferroferric oxide-graphene composite catalyst |
| CN103288105B (en) * | 2012-02-24 | 2015-07-08 | 海洋王照明科技股份有限公司 | Graphene lithium salt, preparation method thereof, positive electrode and supercapacitor |
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| CN109941990A (en) * | 2017-12-21 | 2019-06-28 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of lithium iron phosphate material surface-coated graphene |
| CN108390041A (en) * | 2018-02-28 | 2018-08-10 | 石河子大学 | Foamed nickel current collector LiFePO4/graphene composite material electrode slice and preparation method thereof |
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| CN115000347B (en) * | 2022-05-26 | 2024-06-25 | 广东奥德迈新能源有限责任公司 | Modified lithium iron oxide positive electrode plate, battery containing modified lithium iron oxide positive electrode plate and preparation method of modified lithium iron oxide positive electrode plate |
| CN119390141B (en) * | 2024-12-31 | 2025-03-25 | 帕瓦(长沙)新能源科技有限公司 | Coating material and preparation method thereof, coated modified positive electrode material and preparation method thereof, battery |
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