CN101901903A - Preparation method of high activity lithium ion battery anode material lithium iron phosphate - Google Patents
Preparation method of high activity lithium ion battery anode material lithium iron phosphate Download PDFInfo
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Abstract
The invention discloses a preparation method of high activity lithium ion battery anode material lithium iron phosphate, comprising the following steps: adding ferrous source solution of 0.05-3mol/L and phosphorus source solution in the ratio of 1:1 into a stirring reaction kettle and reacting for 0.5-8h; introducing ozone into the solution and reacting for 2-12h; aging for 2-4h, then filtering; washing and driving so as to obtain the high activity FePO4.2H2O powder; then with the FePO4.2H2O, using lithium source compound and composite carbon source as raw materials according to the mol ratio of iron, phosphorus, lithium and carbon elements of 1:1:(1-1.1):(1-10); with the absolute ethyl alcohol as the medium, mechanically activating for 0.5-10h so as to obtain the LiFePO4 precursor of the composite carbon source; then roasting at low temperature in the protective atmosphere for 4-16h so as to obtain the lithium ion battery anode material LiFePO4 of two particle sizes being 0.5-1 micron and 1-2 microns. The product produced by the invention has high reaction activity, excellent electrochemical performance, high tap density, good processing performance and simple operation process without producing pollution, waste water nor waste gas in preparation process.
Description
Technical field
The present invention relates to a kind of preparation method of high activity lithium ion battery anode material lithium iron phosphate.
Background technology
LiFePO with olivine structural
4Present actual discharge capacity has reached about 95 % of theoretical capacity, and has advantages such as low price, safe, Stability Analysis of Structures, non-environmental-pollution, is considered to that the utmost point has desirable positive electrode in the large-scale lithium ion battery.The preparation of lithium iron phosphate cathode material can be divided into solid phase method and liquid phase method simply.Solid phase method is divided into direct solid phase method and carbothermic method again.The former generally is to be raw material with ferrous iron, makes finished product through oversintering.The latter generally adopts ferric iron as raw material, by the reduction of the material in the course of reaction, ferric iron is reduced to ferrous iron, makes the LiFePO 4 finished product.Liquid phase method is meant the reaction by ion between solution, generates LiFePO 4 or presoma, makes finished product by heat treatment then.Liquid phase method is specially adapted to the preparation of ion doping type ferrousphosphate lithium material.CN101209820。Patents such as CN101209819, CN101106189, CN101117216, CN101121509 have proposed to make the process of presoma and LiFePO 4 finished product respectively.Above method all is to utilize reactor, by certain atmosphere, temperature or pressure condition realization response.But when being used for actual production, exist long, stirring heating time and reaction condition be difficult to control, can not the continous way discharging, problem such as slow, the energy consumption height of conducting heat.Above problem is the key that liquid phase synthesizing method can not be realized industrialized mass production rapidly.CN200880001173.8 discloses a kind of preparation method of active material for anode of Li-ion secondary battery LiFePO 4, this method comprises and will contain mixture drying, the sintering of lithium source, source of iron, phosphorus source, carbon source and solvent, wherein, described solvent is water and/or water-miscible organic solvent, described source of iron is a di-iron trioxide, and described phosphorus source is a phosphoric acid; The mol ratio of its lithium source, di-iron trioxide and phosphoric acid is Li:Fe:P=0.95-1.1: 1: 0.95-1.1; With respect to the ferric oxide of 100 weight portions, the consumption of its carbon source is the 30-110 weight portion, and the consumption of its solvent is the 125-500 weight portion.
Summary of the invention
The objective of the invention is to utilize the different carbonization mechanism of carbon source that the preparation method of another kind of high activity lithium ion battery anode material lithium iron phosphate is provided, to realize improving effectively cycle performance and the high rate performance and the tap density of battery, processing characteristics is obviously improved, preparation process is pollution-free, the generation of no waste water and waste gas, operating process is simple.
Technical scheme of the present invention may further comprise the steps:
(1) the source of iron solution of 1: 1 0.05 ~ 3 mol/L and the phosphorus source solution speed with 200 ~ 1200 mL/h being added in the stirred autoclave simultaneously, is that 50 ~ 90 ℃, mixing speed are under 200 ~ 1200 rpm conditions in reaction temperature, reaction 0.5 ~ 8 h;
(2) be that the ozone of 5 ~ 30 kg/h feeds in the solution and reacts 2 ~ 12 h with flow, ageing 2 ~ 4 h obtain highly active FePO42H at blast drier in 120 ℃ of drying 0.5 h after fully filtering, wash, separating
2The O powder;
(3) with FePO42H
2O, Li source compound and compounded carbons are raw material, by iron, phosphorus, lithium and carbon mol ratio is 1: 1: (1 ~ 1.1): (1 ~ 10), be that medium mixes to be placed on and carries out mechanical activation in the milling apparatus with the absolute ethyl alcohol, soak time is 0.5h ~ 10h, obtain containing the ferric lithium phosphate precursor of compounded carbons
(4) low-temperature bake 4 ~ 16h in protective atmosphere, water is chilled to room temperature, and obtaining primary particle is the lithium ion battery anode material lithium iron phosphate of the compounded carbons doping of 0.5 μ m ~ 1 μ m and 1 μ m ~ two kinds of particle diameters of 2 μ m.
Described source of iron solution is a kind of in cysteine ferrous iron solution, ferrous gluconate solution, iron iodide solution, ferrous oxalate solution, copperas solution, solution of ferrous chloride or the ferrous nitrate solution.
Described phosphorus source solution is ammonium hydrogen phosphate solution, ammonium dihydrogen phosphate, ammonium phosphate solution, ammonium dibasic phosphate solution, lithium phosphate solution, trisodium phosphate solution, triethyl phosphate, tributyl phosphate or phosphate a kind of.
Described Li source compound is a kind of in lithium hydroxide, lithium acetate, lithium carbonate, lithium phosphate, lithium chloride or the lithium nitrate.
Described compounded carbons is two or three in acetylene black, graphite, coke, sucrose, shitosan, lactic acid, glucose, acetate, phenolic resins, acrylic resin, epoxy resin, oxalic acid or the citric acid.
Described protective gas is a kind of of argon gas, nitrogen, hydrogen, carbon dioxide or carbon monoxide.
Described milling apparatus is a kind of of horizontal ball mill, planetary ball mill, stirring mill or grinder.
Operating process of the present invention is easy, equipment simple, be easy to control; Resulting LiFePO4 grain diameter difference, obtaining primary particle is the lithium ion battery anode material lithium iron phosphate of the compounded carbons doping of 0.5 μ m ~ 1 μ m and 1 μ m ~ two kinds of particle diameters of 2 μ m, the reactivity height, improve the cycle performance and the high rate performance of material effectively, improved the processing characteristics of material greatly.
Description of drawings
Fig. 1 is the SEM collection of illustrative plates of embodiment 1 prepared LiFePO4;
Fig. 2 is the XRD figure spectrum of embodiment 1 prepared LiFePO4;
Fig. 3 is charging and discharging capacity figure under the 0.1C of embodiment 1 prepared LiFePO4 and the 1C condition;
Fig. 4 is the cyclic curve figure under the 0.1C condition of embodiment 1 prepared LiFePO4.
Embodiment
Embodiment 1:
(1) take by weighing ferrous sulfate heptahydrate 55.604 kg, ammonium dihydrogen phosphate 23.004 kg are dissolved in it respectively in the deionized water of 200 L, stir to make it dissolving; Copperas solution and ammonium dihydrogen phosphate are joined in the stirred autoclave with the speed of 800 L/h simultaneously, and carry out strong stirring, and control reaction temperature is 80 ℃, low whipping speed is under the 800 r/min conditions, react 1 h, obtain the suspension-turbid liquid of grey ferrous phosphate; The flow that ozone generator is produced is that the ozone of 20 kg/h feeds reaction 3 h in the solution, behind ageing 3 h, filters repeatedly and washs again, obtains the sediment ferric phosphate; The separation back in 120 ℃ of drying 0.5 h, obtains 35.8 kg FePO at blast drier
42H
2The O powder;
Take by weighing FePO
42H
2O 28.8 kg, lithium carbonate 6.0 kg, glucose 4.0 kg and oxalic acid 11.2 kg, be that medium mixes to be placed on to stir in the mill and carries out mechanical activation with the absolute ethyl alcohol, soak time is 1 h, obtain containing the ferric lithium phosphate precursor slurry of compounded carbons, 120 ℃ of dry 12h obtain the ferric lithium phosphate precursor powder in air dry oven, in high pure nitrogen atmosphere, be heated to 400 ℃ again, and constant temperature calcining 12 h, subsequently by water-cooled to room temperature, obtain primary particle and be the lithium ion battery anode material lithium iron phosphate that the compounded carbons of 0.6 μ m and two kinds of particle diameters of 1.0 μ m mixes.
The assembling of battery: the LiFePO4 that takes by weighing the 0.4g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing and make positive plate on the aluminium foil, in vacuum glove box, be negative pole with the metal lithium sheet, with Celgard 2300 is barrier film, 1mol/L LiPF
6/ EC: be electrolyte DMC(volume ratio 1: 1), can be assembled into the button cell of CR2025, the 0.1C first discharge specific capacity is 160.9 mAh/g, and the 1C first discharge specific capacity is 139.6 mAh/g.
Embodiment 2:
(2) take by weighing four water frerrous chlorides, 39.8 kg, ammonium hydrogen phosphate 26.4 kg are dissolved in it respectively in the deionized water of 100 L, stir to make it dissolving; Copperas solution and ammonium dihydrogen phosphate are joined in the stirred autoclave with the speed of 1200 L/h simultaneously, and control reaction temperature is 90 ℃, and low whipping speed is under the 200 r/min conditions, reacts 0.5 h, obtains the suspension-turbid liquid of grey ferrous phosphate; The flow that ozone generator is produced is that the ozone of 30 kg/h feeds reaction 2 h in the solution, behind ageing 2h, filters repeatedly and washs again, obtains the sediment ferric phosphate; The separation back in 120 ℃ of drying 0.5 h, obtains the dried FePO of 29.4 kg at blast drier
42H
2The O powder;
Take by weighing FePO
42H
2O 28.8 kg, lithium nitrate 11.2 kg, sucrose 10kg, graphite 5kg and shitosan 10.0 kg, be that medium mixes to be placed on and carries out mechanical activation in the planetary ball mill with the absolute ethyl alcohol, soak time is 0.5 h, obtain containing the ferric lithium phosphate precursor slurry of compounded carbons, 120 ℃ of dry 12h obtain the ferric lithium phosphate precursor powder in air dry oven, in high-purity argon gas atmosphere, be heated to 400 ℃ again, and constant temperature calcining 4 h, subsequently by water-cooled to room temperature, obtain the lithium ion battery anode material lithium iron phosphate that the uniform compounded carbons of particle size distribution mixes, the primary particle particle diameter is 1.2 μ m.
The assembling of battery: the LiFePO4 that takes by weighing the 0.4g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing and make positive plate on the aluminium foil, in vacuum glove box, be negative pole with the metal lithium sheet, with Celgard 2300 is barrier film, 1mol/L LiPF
6/ EC: be electrolyte DMC(volume ratio 1: 1), can be assembled into the button cell of CR2025, the 0.1C first discharge specific capacity is 142.4 mAh/g, and the 1C first discharge specific capacity is 116.8 mAh/g.
Embodiment 3:
(3) take by weighing six water ferrous nitrates, 36.0 kg, ammonium dihydrogen phosphate 23.004 kg are dissolved in it respectively in the deionized water of 2000 L, stir to make it dissolving; Copperas solution and ammonium dihydrogen phosphate are joined in the stirred autoclave with the speed of 200 L/h simultaneously, and carry out strong stirring, and control reaction temperature is 70 ℃, low whipping speed is under the 1200 r/min conditions, react 8 h, obtain the suspension-turbid liquid of grey ferrous phosphate; The flow that ozone generator is produced is that the ozone of 5 kg/h feeds reaction 12 h in the solution, behind ageing 4 h, filters repeatedly and washs again, obtains the sediment ferric phosphate; The separation back in 120 ℃ of drying 0.5 h, obtains the dried FePO of 36.8 kg at blast drier
42H
2The O powder;
Take by weighing FePO
42H
2O 28.8 kg, lithium acetate 5.9 kg, acetylene black 2 kg, citric acid 10 kg and phenolic resins 10 kg, be that medium mixes to be placed on and carries out mechanical activation in the grinder with the absolute ethyl alcohol, soak time is 10 h, obtain containing the ferric lithium phosphate precursor slurry of compounded carbons, 120 ℃ of dry 12h obtain the ferric lithium phosphate precursor powder in air dry oven, in high-purity hydrogen atmosphere, be heated to 400 ℃ again, and constant temperature calcining 20 h, subsequently by water-cooled to room temperature, obtain primary particle and be the lithium ion battery anode material lithium iron phosphate that the compounded carbons of 0.8 μ m and two kinds of particle diameters of 1.2 μ m mixes.
The assembling of battery: the LiFePO4 that takes by weighing the 0.4g gained, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) make binding agent, be coated in after mixing and make positive plate on the aluminium foil, in vacuum glove box, be negative pole with the metal lithium sheet, with Celgard 2300 is barrier film, 1mol/L LiPF
6/ EC: be electrolyte DMC(volume ratio 1: 1), can be assembled into the button cell of CR2025, the 0.1C first discharge specific capacity is 152.2 mAh/g, and the 1C first discharge specific capacity is 131.5 mAh/g.
Claims (7)
1. the preparation method of a high activity lithium ion battery anode material lithium iron phosphate is characterized in that, may further comprise the steps:
(1) the source of iron solution of 1: 1 0.05 ~ 3 mol/L and the phosphorus source solution speed with 200 ~ 1200 mL/h being added in the stirred autoclave simultaneously, is that 50 ~ 90 ℃, mixing speed are under 200 ~ 1200 rpm conditions in reaction temperature, reaction 0.5 ~ 8 h;
(2) be that the ozone of 5 ~ 30 kg/h feeds in the solution and reacts 2 ~ 12 h with flow, ageing 2 ~ 4 h obtain highly active FePO at blast drier in 120 ℃ of drying 0.5 h after fully filtering, wash, separating
42H
2The O powder;
(3) with FePO
42H
2O, Li source compound and compounded carbons are raw material, by iron, phosphorus, lithium and carbon mol ratio is 1: 1: (1 ~ 1.1): (1 ~ 10), be that medium mixes to be placed on and carries out mechanical activation in the milling apparatus with the absolute ethyl alcohol, soak time is 0.5h ~ 10h, obtains containing the ferric lithium phosphate precursor of compounded carbons;
(4) low-temperature bake 4 ~ 16h in protective atmosphere, water is chilled to room temperature, and obtaining particle is the lithium ion battery anode material lithium iron phosphate of the compounded carbons doping of 0.5 μ m ~ 1 μ m and 1 μ m ~ two kinds of particle diameters of 2 μ m.
2. preparation method according to claim 1, it is characterized in that described source of iron solution is a kind of in cysteine ferrous iron solution, ferrous gluconate solution, iron iodide solution, ferrous oxalate solution, copperas solution, solution of ferrous chloride or the ferrous nitrate solution.
3. preparation method according to claim 1, it is characterized in that, described phosphorus source solution is ammonium hydrogen phosphate solution, ammonium dihydrogen phosphate, ammonium phosphate solution, ammonium dibasic phosphate solution, a kind of in lithium phosphate solution, trisodium phosphate solution, triethyl phosphate, tributyl phosphate or the phosphate.
4. preparation method according to claim 1 is characterized in that, described Li source compound is a kind of in lithium hydroxide, lithium acetate, lithium carbonate, lithium phosphate, lithium chloride or the lithium nitrate.
5. preparation method according to claim 1, it is characterized in that described compounded carbons is two or three in acetylene black, graphite, coke, sucrose, shitosan, lactic acid, glucose, acetate, phenolic resins, acrylic resin, epoxy resin, oxalic acid or the citric acid.
6. preparation method according to claim 1 is characterized in that, described protective gas is a kind of in argon gas, nitrogen, hydrogen, carbon dioxide or the carbon monoxide.
7. preparation method according to claim 1 is characterized in that, described milling apparatus is a kind of of horizontal ball mill, planetary ball mill, stirring mill or grinder.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102097619A (en) * | 2011-01-12 | 2011-06-15 | 合肥国轩高科动力能源有限公司 | Method for preparing high-performance lithium iron phosphate cathode material by using composite reducing agent |
| CN102244246A (en) * | 2011-06-09 | 2011-11-16 | 大连交通大学 | Preparation method of lithium iron phosphate/carbon composite material |
| CN102386407A (en) * | 2011-11-02 | 2012-03-21 | 中南大学 | Method for preparing anode material lithium vanadium phosphate by adopting quenching |
| CN102569738A (en) * | 2010-12-30 | 2012-07-11 | 北京当升材料科技股份有限公司 | Preparation method of lithium iron phosphate material |
| TWI480227B (en) * | 2011-09-13 | 2015-04-11 | Showa Denko Kk | Method of manufacturing a cathode active material for lithium secondary batteries |
| CN105789573A (en) * | 2016-03-04 | 2016-07-20 | 贵州安达科技能源股份有限公司 | Positive electrode active material of lithium ion battery, preparation method for positive electrode active material, lithium ion battery positive electrode, and lithium ion battery |
| CN106410134A (en) * | 2016-09-13 | 2017-02-15 | 青海泰丰先行锂能科技有限公司 | Method for preparing polyanionic compound cathode material of lithium secondary battery |
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| CN106898734A (en) * | 2015-12-17 | 2017-06-27 | 江苏华东锂电技术研究院有限公司 | The method for coating of positive electrode active materials covering liquid and preparation method thereof and positive electrode active materials |
| CN110380020A (en) * | 2019-06-18 | 2019-10-25 | 清华大学深圳研究生院 | Carbon-coated composite ferric lithium phosphate material, preparation method and application |
| CN110620214A (en) * | 2018-06-20 | 2019-12-27 | 深圳市贝特瑞纳米科技有限公司 | Lithium hexafluorozirconate and carbon co-coated lithium iron phosphate composite material, and preparation method and application thereof |
| CN110970608A (en) * | 2019-12-19 | 2020-04-07 | 湖南裕能新能源电池材料有限公司 | Lithium iron battery material and preparation method thereof |
| CN113871596A (en) * | 2021-09-27 | 2021-12-31 | 湖南亿普腾科技有限公司 | Lithium composite material, preparation method of lithium ion battery cathode material and lithium ion battery |
| CN114068919A (en) * | 2020-08-06 | 2022-02-18 | 比亚迪股份有限公司 | Lithium iron phosphate positive electrode active material, preparation method thereof, positive plate and battery |
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2010
- 2010-08-13 CN CN2010102529223A patent/CN101901903A/en active Pending
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| CN102569738A (en) * | 2010-12-30 | 2012-07-11 | 北京当升材料科技股份有限公司 | Preparation method of lithium iron phosphate material |
| CN102097619A (en) * | 2011-01-12 | 2011-06-15 | 合肥国轩高科动力能源有限公司 | Method for preparing high-performance lithium iron phosphate cathode material by using composite reducing agent |
| CN102244246A (en) * | 2011-06-09 | 2011-11-16 | 大连交通大学 | Preparation method of lithium iron phosphate/carbon composite material |
| CN102244246B (en) * | 2011-06-09 | 2013-07-31 | 大连交通大学 | Preparation method of lithium iron phosphate/carbon composite material |
| TWI480227B (en) * | 2011-09-13 | 2015-04-11 | Showa Denko Kk | Method of manufacturing a cathode active material for lithium secondary batteries |
| CN102386407A (en) * | 2011-11-02 | 2012-03-21 | 中南大学 | Method for preparing anode material lithium vanadium phosphate by adopting quenching |
| CN106898734B (en) * | 2015-12-17 | 2019-06-14 | 江苏华东锂电技术研究院有限公司 | The method for coating of positive electrode active materials covering liquid and preparation method thereof and positive electrode active materials |
| CN106898735A (en) * | 2015-12-17 | 2017-06-27 | 江苏华东锂电技术研究院有限公司 | The method for coating of positive electrode active materials covering liquid and preparation method thereof and positive electrode active materials |
| CN106898734A (en) * | 2015-12-17 | 2017-06-27 | 江苏华东锂电技术研究院有限公司 | The method for coating of positive electrode active materials covering liquid and preparation method thereof and positive electrode active materials |
| CN106898735B (en) * | 2015-12-17 | 2019-06-14 | 江苏华东锂电技术研究院有限公司 | The method for coating of positive electrode active materials covering liquid and preparation method thereof and positive electrode active materials |
| CN105789573A (en) * | 2016-03-04 | 2016-07-20 | 贵州安达科技能源股份有限公司 | Positive electrode active material of lithium ion battery, preparation method for positive electrode active material, lithium ion battery positive electrode, and lithium ion battery |
| CN106410134B (en) * | 2016-09-13 | 2019-09-06 | 青海泰丰先行锂能科技有限公司 | A method of preparing lithium secondary battery polyanionic compound cathode material |
| CN106410134A (en) * | 2016-09-13 | 2017-02-15 | 青海泰丰先行锂能科技有限公司 | Method for preparing polyanionic compound cathode material of lithium secondary battery |
| CN110620214B (en) * | 2018-06-20 | 2022-05-03 | 贝特瑞（天津）纳米材料制造有限公司 | Lithium hexafluorozirconate and carbon co-coated lithium iron phosphate composite material, and preparation method and application thereof |
| CN110620214A (en) * | 2018-06-20 | 2019-12-27 | 深圳市贝特瑞纳米科技有限公司 | Lithium hexafluorozirconate and carbon co-coated lithium iron phosphate composite material, and preparation method and application thereof |
| CN110380020A (en) * | 2019-06-18 | 2019-10-25 | 清华大学深圳研究生院 | Carbon-coated composite ferric lithium phosphate material, preparation method and application |
| CN110970608A (en) * | 2019-12-19 | 2020-04-07 | 湖南裕能新能源电池材料有限公司 | Lithium iron battery material and preparation method thereof |
| CN114068919A (en) * | 2020-08-06 | 2022-02-18 | 比亚迪股份有限公司 | Lithium iron phosphate positive electrode active material, preparation method thereof, positive plate and battery |
| CN113871596A (en) * | 2021-09-27 | 2021-12-31 | 湖南亿普腾科技有限公司 | Lithium composite material, preparation method of lithium ion battery cathode material and lithium ion battery |
| CN113871596B (en) * | 2021-09-27 | 2024-01-02 | 湖南亿普腾科技有限公司 | Lithium composite material, preparation method of lithium ion battery positive electrode material and lithium ion battery |
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Assignee: Shandong Jiuli Electronic Technology Co., Ltd. Assignor: Zhang Bao Contract record no.: 2012370000032 Denomination of invention: Preparation method of high activity lithium ion battery anode material lithium iron phosphate License type: Exclusive License Open date: 20101201 Record date: 20120327 |
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