CN102881901A - Doped modified lithium iron phosphate and preparation method thereof - Google Patents
Doped modified lithium iron phosphate and preparation method thereof Download PDFInfo
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- CN102881901A CN102881901A CN2012103814727A CN201210381472A CN102881901A CN 102881901 A CN102881901 A CN 102881901A CN 2012103814727 A CN2012103814727 A CN 2012103814727A CN 201210381472 A CN201210381472 A CN 201210381472A CN 102881901 A CN102881901 A CN 102881901A
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Abstract
The invention discloses a raw material formula of doped modified lithium iron phosphate. Components include a ferric iron source, a phosphorus source, a lithium source, a doped element compound and excess carbon sources, wherein the mole ratio of to ferric iron source to the phosphorus source to the lithium source to the doped element compound to the carbon sources is 1:1-1.05:1-1.1:0.01-0.05:0.1-0.2. A preparation method directly adopts the ferric iron source, so that a cockamamie step of synthesizing ferrous salt by means of other synthesizing technologies is avoided, and the problem that usual products produced by means of conventional preparation methods using a ferrous salt raw material oxidizable in the air are impure is solved. A synthesized doped modified lithium iron phosphate material is small in particle diameter, narrow in distribution, high in purity, large in compaction and excellent in electrochemistry performance. A synthesized positive pole material and a carbon negative pole are assembled to form a test battery, the specific capacity is more than 130mAh/g when discharging is performed in 1C multiplying power, and excellent circulating stability performance is displayed.
Description
Technical field
The present invention relates to a kind of composition of raw materials for preparing LiFePO 4 and preparation method thereof, belong to the electrode material of lithium battery field.
Background technology
As everyone knows, LiFePO 4 is compared with other main flow positive electrodes, the shortcoming that the conductivity of itself is weak, this will directly cause this material, and to be battery take off embedding and mobile being obstructed discharging and recharging lower lithium ion in system, the utilance of active material is low, and be devoted to the LiFePO 4 research of electrokinetic cell for industry, a very important and difficult class on the improvement that affects its heavy-current discharge, therefore mainly be in the material building-up process, to add conductive agent to this improvement method in the industry, or use method that particle coats in the method for LiFePO 4 particle surface coated with conductive material in the later stage, make material have relatively preferably electric conductivity, when battery is made, also add a certain amount of conductive agent according to proportioning.Present technology has following shortcoming, has hindered its practical application:
(1) Fe in synthetic
2+Easily be oxidized to Fe
3+, be difficult to obtain single-phase LiFePO
4
(2) lithium ion is at LiFePO
4Middle diffusion difficulty causes the utilance of active material low;
(3) LiFePO
4The conductivity of itself is also very low, causes its heavy-current discharge performance poor;
(4) in the application process of material because repeatedly conductive agent adds the error that produces final battery performance mix poor unevenly, reduce the consistency of product.
Summary of the invention
The technical problem to be solved in the present invention is to overcome existing defective, and a kind of composition of raw materials that can improve product purity, the better doping vario-property LiFePO 4 of electrical property is provided;
Another object of the present invention provides the preparation method of a kind of technique doping vario-property LiFePO 4 simple, that control and production cost are low easily.
Purpose of the present invention is come specific implementation by the following technical programs:
A kind of doping vario-property LiFePO 4 (LiFePO
4/ X/C), each component of its composition of raw materials comprises ferric iron source, phosphorus source, lithium source, doping element compound and excessive carbon source, wherein, ferric iron source: phosphorus source: lithium source: the mol ratio of doping element compound is 1:1 ~ 1.05:1 ~ 1.1:0.01 ~ 0.05:0.1 ~ 0.2.
It is two hydration ferric orthophosphates of 1:1 ~ 1.05 that iron phosphorus mol ratio is adopted in described ferric iron source, phosphorus source;
Described lithium source is selected from one or more the mixture in a hydronium(ion) oxidation lithium, lithium acetate, lithium chloride, lithium nitrate, the lithium carbonate, preferred lithium hydroxide or lithium acetate or lithium carbonate;
Described doping element compound is selected from AgNO
3, MnCO
3, Mn (NO
3)
2, MoO
3, Mg (OH)
2, Mg (NO
3)
2, NiPO
4In a kind of, preferred AgNO
3Or MnCO
3Or Mg (OH)
2
Described carbon source is selected from one or more the mixture in sucrose, glucose, dextrin, polypropylene, polyacrylamide, citric acid, the starch, preferably sucrose or glucose or citric acid.
The preparation method of above-mentioned doping vario-property LiFePO 4 comprises the steps:
The preparation of step 1, presoma:
A. raw material weighing: ferric iron source, phosphorus source, lithium source, doping element compound, carbon source are pressed the formula ratio weighing;
B. ball milling mixes: load weighted ferric iron source, phosphorus source, lithium source, doping element compound, carbon source are placed dispersant, again with said mixture ball milling 24-36h;
C. dry: place air atmosphere to dry the ball milling product, bake out temperature is 90-110 ℃, and drying time is 10-20h;
D. grind: grind after dried product is cooled off naturally, get the high density precursor of LiFePO 4;
Step 2, roasting:
The precursor of the LiFePO 4 for preparing is placed high temperature furnace, in non-oxidizing atmosphere, be warming up to 700-1000 ℃ with the rate of heat addition of 50 ~ 60 ℃/h, keep temperature, behind the roasting 15-20h, naturally cool to below 80 ℃, get doping vario-property ferrous phosphate lithium powder.
Among the step b of above-mentioned steps one, described dispersant is selected from one or more the mixture in water, ethanol, the ether.
Nonoxidizing atmosphere in the above-mentioned steps two adopts nitrogen atmosphere.
In the above-mentioned steps two, described sintering temperature is 700-800 ℃.
Beneficial effect of the present invention:
1, the LiFePO 4 of preparation doping vario-property provided by the invention, need not to prepare in advance or use the ferrous salt of easy oxidation in air, and directly adopt the source of iron of trivalent, avoid ferrous salt synthesis step loaded down with trivial details in other synthetic technologys, solved the impure problem of product that often has among the conventional preparation method of the ferrous salt raw material of easy oxidation in air of using.
2, the LiFePO 4 (LiFePO of preparation doping vario-property provided by the invention
4/ X/C) method adopts mechanical process for solid phase synthesis, and synthetic doping vario-property ferrousphosphate lithium material particle diameter is little, and narrowly distributing, purity are high, and jolt ramming is large, and chemical property is good.The positive electrode that the present invention synthesizes and carbon negative pole are assembled into test battery, and specific capacity and shows outstanding stable circulation performance greater than 130mAh/g when the 1C multiplying power discharging.
3, the LiFePO 4 (LiFePO of preparation doping vario-property provided by the invention
4/ X/C) method, by the control synthesis technique, at first synthetic a kind of high density precursor that mixes be used to making LiFePO 4, this precursor being calcined under given conditions is gained again, this method technique is simple, easily control, and production cost is low, can realize the industrialized production cleaned, three-waste free discharge.
Description of drawings
Accompanying drawing is used to provide a further understanding of the present invention, and consists of the part of specification, is used for together with embodiments of the present invention explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is preparation method's process chart of the LiFePO 4 (LiFePO4/X/C) of doping vario-property of the present invention.
Embodiment
Below in conjunction with accompanying drawing the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for description and interpretation the present invention, is not intended to limit the present invention.
Embodiment 1:
A kind of preparation method of doping vario-property LiFePO 4, such as Fig. 1 flow process, as follows:
1, presses the weighing of table 1 indication composition of raw materials;
2, place 300ml ethanol to mix load weighted raw material, again the material that mixes is placed ball mill container, ball milling 36 hours;
3, the ball milling product is placed air atmosphere in 110 ℃ of oven dry 10 hours, naturally being ground to particle size after the cooling is more than 80 orders, the high density precursor of the LiFePO 4 that must mix;
4, the precursor with above-mentioned gained LiFePO 4 places high temperature furnace, in the atmosphere of nitrogen, is warmed up to 800 ℃ with the rate of heat addition of 60 ℃/h, behind 800 ℃ of lower constant temperature calcining 20h, naturally cools to below 80 ℃, makes silver-colored ferrous phosphate doping lithium powder.
The products obtained therefrom performances and parameters is referring to table 1.
Embodiment 2:
A kind of preparation method of doping vario-property LiFePO 4, such as Fig. 1 flow process, as follows:
1, presses the weighing of table 1 indication composition of raw materials;
2, place 300ml water to mix load weighted raw material, again the material that mixes is placed ball mill container, ball milling 24 hours;
3, the ball milling product is placed air atmosphere in 90 ℃ of oven dry 20 hours, naturally being ground to particle size after the cooling is more than 80 orders, the high density precursor of the LiFePO 4 that must mix;
4, the precursor with above-mentioned gained LiFePO 4 places high temperature furnace, in the atmosphere of nitrogen, is warmed up to 700 ℃ with the rate of heat addition of 50 ℃/h, behind 700 ℃ of lower constant temperature calcining 20h, naturally cools to below 80 ℃, makes manganese ferrous phosphate doping lithium powder.
The products obtained therefrom performances and parameters is referring to table 1.
Embodiment 3:
A kind of preparation method of doping vario-property LiFePO 4, such as Fig. 1 flow process, as follows:
1, presses the weighing of table 1 indication composition of raw materials;
2, load weighted raw material is placed the mixed liquor of 300ml ether and water (mol ratio of ether and water is 1:1) mix, again the material that mixes is placed ball mill container, ball milling 30 hours;
3, the ball milling product is placed air atmosphere in 100 ℃ of oven dry 15 hours, naturally being ground to particle size after the cooling is more than 80 orders, the high density precursor of the LiFePO 4 that must mix;
4, the precursor with above-mentioned gained LiFePO 4 places high temperature furnace, in the atmosphere of nitrogen, is warmed up to 750 ℃ with the rate of heat addition of 55 ℃/h, behind 750 ℃ of lower constant temperature calcining 18h, naturally cools to below 80 ℃, makes magnesium ferrous phosphate doping lithium powder.
The products obtained therefrom performances and parameters is referring to table 1.
Embodiment 4:
A kind of preparation method of doping vario-property LiFePO 4, such as Fig. 1 flow process, as follows:
1, presses the weighing of table 1 indication composition of raw materials;
2, place 300ml water to mix load weighted raw material, again the material that mixes is placed ball mill container, ball milling 36 hours;
3, the ball milling product is placed air atmosphere in 110 ℃ of oven dry 10 hours, naturally being ground to particle size after the cooling is more than 80 orders, the high density precursor of the LiFePO 4 that must mix;
4, the precursor with above-mentioned gained LiFePO 4 places high temperature furnace, in the atmosphere of nitrogen, is warmed up to 800 ℃ with the rate of heat addition of 60 ℃/h, behind 800 ℃ of lower constant temperature calcining 20h, naturally cools to below 80 ℃, makes magnesium ferrous phosphate doping lithium powder.
The products obtained therefrom performances and parameters is referring to table 1.
Embodiment 5:
A kind of preparation method of doping vario-property LiFePO 4, such as Fig. 1 flow process, as follows:
1, presses the weighing of table 1 indication composition of raw materials;
2, place 300ml ethanol to mix load weighted raw material, again the material that mixes is placed ball mill container, ball milling 24 hours;
3, the ball milling product is placed air atmosphere in 100 ℃ of oven dry 10 hours, naturally being ground to particle size after the cooling is more than 80 orders, the high density precursor of the LiFePO 4 that must mix;
4, the precursor with above-mentioned gained LiFePO 4 places high temperature furnace, in the atmosphere of nitrogen, is warmed up to 750 ℃ with the rate of heat addition of 55 ℃/h, behind 750 ℃ of lower constant temperature calcining 18h, naturally cools to below 80 ℃, makes magnesium ferrous phosphate doping lithium powder.
The products obtained therefrom performances and parameters is referring to table 1.
Table 1:
The above only is the preferred embodiments of the present invention, be not limited to the present invention, although mix according to previous embodiment the present invention is had been described in detail, for a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment puts down in writing, and perhaps part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. doping vario-property LiFePO 4, it is characterized in that: its composition of raw materials comprises ferric iron source, phosphorus source, lithium source, doping element compound and excessive carbon source, wherein, ferric iron source: phosphorus source: lithium source: doping element compound: the mol ratio of reproducibility carbon is 1:1 ~ 1.05:1 ~ 1.1:0.01 ~ 0.05:0.1 ~ 0.2.
2. doping vario-property LiFePO 4 according to claim 1 is characterized in that: it is two hydration ferric orthophosphates of 1:1 ~ 1.05 that iron phosphorus mol ratio is adopted in described ferric iron source, phosphorus source.
3. doping vario-property LiFePO 4 according to claim 1 is characterized in that: described lithium source is selected from one or more the mixture in a hydronium(ion) oxidation lithium, lithium acetate, lithium chloride, lithium nitrate, the lithium carbonate.
4. doping vario-property LiFePO 4 according to claim 1, it is characterized in that: described doping element compound is selected from AgNO
3, MnCO
3, Mn (NO
3)
2, MoO
3, Mg (OH)
2, Mg (NO
3)
2, NiPO
4In a kind of.
5. doping vario-property LiFePO 4 according to claim 1 is characterized in that: described carbon source is selected from one or more the mixture in sucrose, glucose, dextrin, polypropylene, polyacrylamide, citric acid, the starch.
6. the preparation method of each described doping vario-property LiFePO 4 is characterized in that: comprise the steps: according to claim 1-5
The preparation of step 1, presoma:
A. raw material weighing: ferric iron source, phosphorus source, lithium source, doping element compound, carbon source are pressed the formula ratio weighing;
B. ball milling mixes: load weighted ferric iron source, phosphorus source, lithium source, doping element compound, carbon source are placed dispersant, again with said mixture ball milling 24-36h;
C. dry: place air atmosphere to dry the ball milling product, bake out temperature is 90-110 ℃, and drying time is 10-20h;
D. grind: grind after dried product is cooled off naturally, get the high density precursor of LiFePO 4;
Step 2, roasting:
The precursor of the LiFePO 4 for preparing is placed high temperature furnace, in non-oxidizing atmosphere, be warming up to 700-1000 ℃ with the rate of heat addition of 50 ~ 60 ℃/h, keep temperature, behind the roasting 15-20h, naturally cool to below 80 ℃, get doping vario-property ferrous phosphate lithium powder.
7. the preparation method of doping vario-property LiFePO 4 according to claim 6 is characterized in that: the dispersant among the step b of described step 1 is selected from one or more the mixture in water, ethanol, the ether.
8. the preparation method of doping vario-property LiFePO 4 according to claim 6 is characterized in that: the nonoxidizing atmosphere employing nitrogen atmosphere in the described step 2.
9. the preparation method of doping vario-property LiFePO 4 according to claim 6, it is characterized in that: the sintering temperature in the described step 2 is 700-800 ℃.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103107332A (en) * | 2013-01-24 | 2013-05-15 | 北大先行科技产业有限公司 | LFP (lithium iron phosphate) positive electrode material with excellent low-temperature property and preparation method thereof |
| CN103441269A (en) * | 2013-08-05 | 2013-12-11 | 北大先行科技产业有限公司 | Lithium/carbon pyrophosphate coated lithium iron phosphate composite and preparation method thereof |
| CN105449206A (en) * | 2015-12-23 | 2016-03-30 | 邬石根 | LiFe1-xZrxPO4 electrode material and preparation method thereof |
| CN106602060A (en) * | 2016-12-26 | 2017-04-26 | 贝特瑞（天津）纳米材料制造有限公司 | Low-cost lithium iron phosphate material, and preparation method and application thereof |
| CN108155361A (en) * | 2017-12-24 | 2018-06-12 | 扬州工业职业技术学院 | A kind of iron lithium phosphate battery |
| CN108172788A (en) * | 2017-12-24 | 2018-06-15 | 扬州工业职业技术学院 | The LiFePO of nickel doping vario-property4/ C composite and its application as anode material of lithium battery |
| CN108448113A (en) * | 2018-03-29 | 2018-08-24 | 中国地质科学院矿产综合利用研究所 | Preparation method of doped modified lithium iron phosphate positive-grade material |
| CN109244424A (en) * | 2018-10-24 | 2019-01-18 | 东莞理工学院 | A kind of preparation method of alumina-coated additive Mn lithium iron phosphate positive material |
| CN111276693A (en) * | 2020-01-22 | 2020-06-12 | 上海华谊（集团）公司 | Modification method of lithium manganese iron phosphate, modified lithium manganese iron phosphate and application thereof |
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| CN101976734A (en) * | 2010-11-03 | 2011-02-16 | 江苏方舟新能源股份有限公司 | Preparation method of high-density lithium iron phosphate as lithium battery anode material |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103107332A (en) * | 2013-01-24 | 2013-05-15 | 北大先行科技产业有限公司 | LFP (lithium iron phosphate) positive electrode material with excellent low-temperature property and preparation method thereof |
| CN103107332B (en) * | 2013-01-24 | 2015-10-14 | 北大先行科技产业有限公司 | A kind of lithium iron phosphate positive material and preparation method thereof |
| CN103441269A (en) * | 2013-08-05 | 2013-12-11 | 北大先行科技产业有限公司 | Lithium/carbon pyrophosphate coated lithium iron phosphate composite and preparation method thereof |
| CN103441269B (en) * | 2013-08-05 | 2016-08-17 | 北大先行科技产业有限公司 | A kind of pyrophosphoric acid lithium/carbon-coated lithium iron phosphate composite and preparation method thereof |
| CN105449206A (en) * | 2015-12-23 | 2016-03-30 | 邬石根 | LiFe1-xZrxPO4 electrode material and preparation method thereof |
| CN106602060A (en) * | 2016-12-26 | 2017-04-26 | 贝特瑞（天津）纳米材料制造有限公司 | Low-cost lithium iron phosphate material, and preparation method and application thereof |
| CN108155361A (en) * | 2017-12-24 | 2018-06-12 | 扬州工业职业技术学院 | A kind of iron lithium phosphate battery |
| CN108172788A (en) * | 2017-12-24 | 2018-06-15 | 扬州工业职业技术学院 | The LiFePO of nickel doping vario-property4/ C composite and its application as anode material of lithium battery |
| CN108155361B (en) * | 2017-12-24 | 2020-06-26 | 扬州工业职业技术学院 | Lithium iron phosphate battery |
| CN108172788B (en) * | 2017-12-24 | 2020-06-30 | 扬州工业职业技术学院 | Nickel-doped modified LiFePO4/C composite material and application thereof as lithium battery anode material |
| CN108448113A (en) * | 2018-03-29 | 2018-08-24 | 中国地质科学院矿产综合利用研究所 | Preparation method of doped modified lithium iron phosphate positive-grade material |
| CN108448113B (en) * | 2018-03-29 | 2021-06-04 | 中国地质科学院矿产综合利用研究所 | Preparation method of doped modified lithium iron phosphate positive-grade material |
| CN109244424A (en) * | 2018-10-24 | 2019-01-18 | 东莞理工学院 | A kind of preparation method of alumina-coated additive Mn lithium iron phosphate positive material |
| CN111276693A (en) * | 2020-01-22 | 2020-06-12 | 上海华谊（集团）公司 | Modification method of lithium manganese iron phosphate, modified lithium manganese iron phosphate and application thereof |
| CN111276693B (en) * | 2020-01-22 | 2022-09-20 | 上海华谊（集团）公司 | Modification method of lithium manganese iron phosphate, modified lithium manganese iron phosphate and application thereof |
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Application publication date: 20130116 |