CN102013468A - Method for preparing high-conductivity lithium iron phosphate anode material - Google Patents
Method for preparing high-conductivity lithium iron phosphate anode material Download PDFInfo
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- CN102013468A CN102013468A CN2009101901061A CN200910190106A CN102013468A CN 102013468 A CN102013468 A CN 102013468A CN 2009101901061 A CN2009101901061 A CN 2009101901061A CN 200910190106 A CN200910190106 A CN 200910190106A CN 102013468 A CN102013468 A CN 102013468A
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Abstract
The invention relates to a method for preparing a high-conductivity lithium iron phosphate anode material, which comprises the following steps of: firstly, mixing a lithium source compound, an iron source compound and a phosphorus source compound in deionized water; adding an organic carbon source and a dopant and uniformly mixing; then placing a uniformly mixed mixture into a closed reactor with the temperature of 80-350 DEG C, the pressure of 1-16.5MPa and the stirring speed of 50-500r/min for reacting and drying a reacted substance; finally, sintering reacted substance at a protective atmosphere, heating at the rate of 1-20 DEG C/min and sintering at the constant temperature of 560-740 DEG C for 1.1-9 hours; and cooling at the rate of 2-9 DEG C/min to obtain the lithium iron phosphate material. By utilizing the method of the invention, the lithium iron phosphate anode material with even and fine granularity, coating of even film carbon on the surface, high conductive performance and high electrochemical performance can be obtained.
Description
Technical field
The present invention relates to a kind of preparation method of high conductivity lithium iron phosphate positive material, particularly be used in the preparation method of the olivine-type lithium iron phosphate positive material in the secondary lithium battery.
Background technology
Along with developing rapidly of battery industry, various types of batteries have appearred in the problems such as useful life, energy density, self discharge or quality in order to solve battery.At present, because lithium battery has advantages such as energy density height, long service life, light weight, self discharge are little, now become the first-selected power supply of portable sets such as communication apparatus, notebook computer, and also begun to be applied in the medium-and-large-sized equipment such as electric motor car, national defence.
At present, because abundant raw material, the cost of LiFePO4 are low, safety and cycle performance are good, use positive electrode major part to be LiFePO 4 material at lithium ion battery, in order to realize the practicability of LiFePO4 as soon as possible, the potential performance of performance LiFePO4, the preparation method to lithium iron phosphate positive material has carried out a large amount of experiments and research.At present, the preparation method of lithium iron phosphate positive material mainly contains high temperature solid-state method, liquid phase reactor method, sol-gal process and mechanical ball milling method etc.
High temperature solid-state method is with Li source compound, Fe source compound and P source compound roasting synthesizing iron lithium phosphate under inert atmosphere protection; The advantage of high temperature solid-state method is that technology simply, easily realizes industrialization, but the common mixing of reactant is inhomogeneous, and product particle, crystal grain are easily grown up; purity is not high, and the excessive lithium ion migration path that causes of primary particle is long, and the lithium ion conducting performance is poor; therefore, chemical property is bad.Adopt sol-gal process can make evengranular lithium iron phosphate nano material, but for obtaining the purity of nano material and assurance material, need template or inert environments, the technical process control ratio is strict, and complex process is difficult for realizing suitability for industrialized production.
Summary of the invention
The objective of the invention is for a kind of method that adopts hydrothermal synthesis method to prepare the high conductivity lithium iron phosphate positive material is provided, utilize method of the present invention, the lithium iron phosphate positive material that can obtain epigranular, tiny, carbon that the surface coats even thin layer, conduct electricity very well, chemical property is good.
For achieving the above object, a kind of preparation method of high conductivity lithium iron phosphate positive material the steps include:
1) with Li source compound, Fe source compound and P source compound in molar ratio the ratio of 1.5-4: 1.1-1.5: 1.1-1.5 in deionized water, mix;
2) add organic carbon source and alloy and mix, the content of alloy is 0.01-10%;
3) mixture that mixes being placed temperature is that 80-350 ℃, pressure are that 1-16.5MPa, mixing speed are that the closed reactor of 50-500r/min reacts 0.1-9h;
4) with reacted material drying;
5) sintering under restitutive protection's atmosphere heats up with 1-20 ℃/min speed, at temperature 560-740 ℃ of constant temperature sintering 1.1-9h;
6) with 2-9 ℃/min cooling, prepare LiFePO 4 material.
As specializing, described Li source compound is one or more mixtures of lithia, lithium hydroxide, lithium phosphate, lithium carbonate, lithium nitrate, lithium dihydrogen phosphate, lithium formate, lithium acetate.
As specializing, described Fe source compound is one or more mixtures in iron, ferric phosphate, ferrous sulfate, di-iron trioxide, ferrous oxide, tri-iron tetroxide, iron ammonium sulfate, ferrous sulfate, ferrous phosphate, ferrous ammonium phosphate, ferrous citrate, the frerrous chloride.
As specializing, described P source compound is one or more mixtures in phosphorus pentoxide, phosphoric acid, ammonium dihydrogen phosphate, lithium dihydrogen phosphate, diammonium hydrogen phosphate, ferrous ammonium phosphate, the ammonium hydrogen phosphate salt.
As specializing, described organic carbon source is one or more mixtures in sucrose, glucose, polyethylene glycol, polyvinyl alcohol or the starch.
As specializing, described alloy is one or more mixtures in manganese, cobalt, vanadium, nickel, aluminium, magnesium, calcium, zinc simple substance or the compound.
As specializing, described restitutive protection's atmosphere is nitrogen, argon gas, hydrogen, carbon monoxide or their blended gaseous mixture.
Technique scheme owing to adopt hydrothermal synthesis method to prepare lithium iron phosphate positive material, therefore, can be formed and epigranular degree implementation better controlled element, guarantees final lithium iron phosphate positive material epigranular, tiny; Because Li source compound, Li source compound, P source compound and doped chemical or compound are that dissolving mixes in deionized water, therefore, the lithium iron phosphate positive material for preparing can be realized the doping of molecular level; Owing to added the organic carbon source of dissolved state, therefore, can obtain the carbon that material surface coats even thin layer, improved the performance of conduction, stable electrochemical property.
Description of drawings
Fig. 1 is the XRD spectra of LiFePO4 product;
Fig. 2 a, b, c are the SEM figure of LiFePO 4 material;
Fig. 3 is the charging and discharging curve of LiFePO4 product;
Fig. 4 is the cycle performance of LiFePO4.
Specific embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in more detail.
First embodiment
With LiOH, FeSO
47H
2O, H
3PO
4Join in the deionized water at 3: 1.1: 1.1 according to mol ratio, and the organic carbon source and the alloy of one or more composition mixtures in interpolation sucrose, glucose, polyethylene glycol, polyvinyl alcohol or the starch, described alloy is one or more in the compound of manganese, cobalt, vanadium, nickel, aluminium, magnesium, calcium, zinc etc., the content of alloy is 0.01%, mixes.In 80 ℃, the closed reactor of 1MPa; mixing speed is 50r/min; reacted centrifuge dewatering, vacuum drying 9 hours; under nitrogen protection, carry out sintering; be warmed up to 560 degree with 5 ℃/min, constant temperature sintering 9 hours cools to room temperature with 2 ℃/min again; see Fig. 1, obtain the iron phosphate powder of carbon coated.
Above-mentioned preparation method, owing to adopt hydrothermal synthesis method to prepare lithium iron phosphate positive material, therefore, can form and epigranular degree implementation better controlled element, shown in Fig. 2 a, guaranteed final lithium iron phosphate positive material epigranular, tiny, particle diameter is a nanoscale; Because Li source compound, Fe source compound and P source compound are to mix in deionized water, therefore, the lithium iron phosphate positive material purity height for preparing; Owing to added the organic carbon source of dissolved state, therefore, can obtain the carbon that material surface coats even thin layer; Adopt above-mentioned preparation method and parameter, the electronic conductivity of material is 3.28 * 10
-4S/cm, specific discharge capacity is 137mAh/g, as Fig. 3.
Second embodiment
With Li (HCOO) H
2O, FeCl
24H
2O, NH
4H
2PO
4Join in the deionized water at 1.5: 1.5: 1.5 according to mol ratio, and the organic carbon source and the alloy of one or more composition mixtures in interpolation sucrose, glucose, polyethylene glycol, polyvinyl alcohol or the starch, described alloy is one or more in the compound of manganese, cobalt, vanadium, nickel, aluminium, magnesium, calcium, zinc etc., the content of alloy is 5%, mixes.In 350 ℃, the closed reactor of 16.5MPa, mixing speed is 500r/min, reacts centrifuge dewatering 0.1 hour; vacuum drying carries out sintering under the protection of argon gas, 5 ℃/min is warmed up to 740 degree; constant temperature 1.1 hours cools to room temperature naturally, obtains the iron phosphate powder of carbon coated.The electronic conductivity of material is 8.51 * 10
-5S/cm.
Above-mentioned preparation method, owing to adopt hydrothermal synthesis method to prepare lithium iron phosphate positive material, therefore, can form and epigranular degree implementation better controlled element, shown in Fig. 2 b, guaranteed final lithium iron phosphate positive material epigranular, tiny, particle diameter is a nanoscale; Because Li source compound, Fe source compound and P source compound are to mix in deionized water, therefore, the lithium iron phosphate positive material purity height for preparing; Owing to added the organic carbon source of dissolved state, therefore, can obtain the carbon that material surface coats even thin layer; Adopt above-mentioned preparation method and parameter, the electronic conductivity of material is 8.51 * 10
-5S/cm as shown in Figure 4, with the simulated battery cycle performance excellence of this material, therefore, has improved the performance of conduction, stable electrochemical property.
The 3rd embodiment
With LiOH, FeSO
4H
2O, NH
4H
2PO
4Join in the deionized water at 1.5: 1.2: 1.2 according to mol ratio, and the organic carbon source and the alloy of one or more composition mixtures in interpolation sucrose, glucose, polyethylene glycol, polyvinyl alcohol or the starch, described alloy is one or more in the compound of manganese, cobalt, vanadium, nickel, aluminium, magnesium, calcium, zinc etc., the content of alloy is 10%, mixes.In 200 ℃, the closed reactor of 1.6MPa, mixing speed is 300r/min, reacts centrifuge dewatering 5 hours; vacuum drying carries out sintering under argon shield, be warmed up to 650 degree with 5 ℃/min; constant temperature 6 hours with 5 ℃/min cooling, obtains the iron phosphate powder of carbon coated.
Above-mentioned preparation method, owing to adopt hydrothermal synthesis method to prepare lithium iron phosphate positive material, therefore, can form and epigranular degree implementation better controlled element, shown in Fig. 2 c, guaranteed final lithium iron phosphate positive material epigranular, tiny, particle diameter is a nanoscale; Because Li source compound, Fe source compound and P source compound are to mix in deionized water, therefore, the lithium iron phosphate positive material purity height for preparing; Owing to added the organic carbon source of dissolved state, therefore, can obtain the carbon that material surface coats even thin layer; Adopt above-mentioned preparation method and parameter, the electronic conductivity of material is 6.62 * 10
-4S/cm.
Claims (7)
1. the preparation method of a high conductivity lithium iron phosphate positive material the steps include:
1) with Li source compound, Fe source compound and P source compound in molar ratio the ratio of 1.5-4: 1.1-1.5: 1.1-1.5 in deionized water, mix;
2) add organic carbon source and alloy and mix, the content of alloy is 0.01-10%;
3) mixture that mixes being placed temperature is that 80-350 ℃, pressure are that 1-16.5MPa, mixing speed are that the closed reactor of 50-500r/min reacts 0.1-9h;
4) with reacted material drying;
5) sintering under restitutive protection's atmosphere heats up with 1-20 ℃/min speed, at temperature 560-740 ℃ of constant temperature sintering 1.1-9h;
6) with 2-9 ℃/min cooling, prepare LiFePO 4 material.
2. the preparation method of high conductivity lithium iron phosphate positive material according to claim 1 is characterized in that: described Li source compound is one or more mixtures of lithia, lithium hydroxide, lithium phosphate, lithium carbonate, lithium nitrate, lithium dihydrogen phosphate, lithium formate, lithium acetate.
3. the preparation method of high conductivity lithium iron phosphate positive material according to claim 1 is characterized in that: described Fe source compound is one or more mixtures in iron, ferric phosphate, ferrous sulfate, di-iron trioxide, ferrous oxide, tri-iron tetroxide, iron ammonium sulfate, ferrous sulfate, ferrous phosphate, ferrous ammonium phosphate, ferrous citrate, the frerrous chloride.
4. the preparation method of high conductivity lithium iron phosphate positive material according to claim 1 is characterized in that: described P source compound is one or more mixtures in phosphorus pentoxide, phosphoric acid, ammonium dihydrogen phosphate, lithium dihydrogen phosphate, diammonium hydrogen phosphate, ferrous ammonium phosphate, the ammonium hydrogen phosphate salt.
5. the preparation method of high conductivity lithium iron phosphate positive material according to claim 1 is characterized in that: described organic carbon source is one or more mixtures in sucrose, glucose, polyethylene glycol, polyvinyl alcohol or the starch.
6. the preparation method of high conductivity lithium iron phosphate positive material according to claim 1 is characterized in that: described alloy is one or more mixtures in manganese, cobalt, vanadium, nickel, aluminium, magnesium, calcium, zinc simple substance or the compound.
7. the preparation method of high conductivity lithium iron phosphate positive material according to claim 1 is characterized in that: described restitutive protection's atmosphere is nitrogen, argon gas, hydrogen, carbon monoxide or their blended gaseous mixture.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694169A (en) * | 2012-03-07 | 2012-09-26 | 湖北万润新能源科技发展有限公司 | FePO4/high polymer cracked carbon composite material and preparation method thereof, and NH4Fe2(OH)(PO4)2.2H2O/high polymer composite material and preparation method thereof |
| CN103682338A (en) * | 2013-12-23 | 2014-03-26 | 向勇 | Preparation method for high-conductivity LiFePO4 cathode material |
| CN104091946A (en) * | 2014-07-14 | 2014-10-08 | 中国科学技术大学苏州研究院 | Method for integrally synthesizing LiMnPO4/C by solvent and carbon source |
| CN105514430A (en) * | 2015-12-30 | 2016-04-20 | 山东精工电子科技有限公司 | Spherical LiFexMnyPO4 anode material and preparation method thereof |
| CN106207178A (en) * | 2015-04-30 | 2016-12-07 | 苏州艾美得新能源材料有限公司 | The preparation method of positive electrode, positive electrode and battery |
| CN107452949A (en) * | 2017-08-06 | 2017-12-08 | 长沙小新新能源科技有限公司 | A kind of LiFe1‑XNiXPO4The preparation method of/C Anode of lithium cell materials |
| CN109346698A (en) * | 2018-10-15 | 2019-02-15 | 西北有色金属研究院 | A kind of in-situ preparation method of the lithium-rich manganese-based two-phase electrode material of LiFePO4- |
| CN110323434A (en) * | 2019-07-11 | 2019-10-11 | 江苏力泰锂能科技有限公司 | Prepare iron manganese phosphate for lithium-carbon composite method and iron manganese phosphate for lithium-carbon composite |
| CN112390241A (en) * | 2020-11-17 | 2021-02-23 | 湖北融通高科先进材料有限公司 | Lithium iron phosphate material and method for preparing lithium iron phosphate material by taking mixed iron source and mixed lithium source as raw materials |
| CN112490439A (en) * | 2020-12-03 | 2021-03-12 | 湖北融通高科先进材料有限公司 | Method for preparing lithium iron phosphate material by taking mixed iron source and mixed phosphorus source as raw materials and lithium iron phosphate material prepared by method |
| CN113745503A (en) * | 2021-08-04 | 2021-12-03 | 北京泰丰先行新能源科技有限公司 | Preparation method of high-compaction lithium iron phosphate cathode material |
| CN115259128A (en) * | 2022-08-05 | 2022-11-01 | 湖北融通高科先进材料有限公司 | Preparation method of high-compaction high-capacity low-cost lithium iron phosphate |
-
2009
- 2009-09-07 CN CN2009101901061A patent/CN102013468A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694169A (en) * | 2012-03-07 | 2012-09-26 | 湖北万润新能源科技发展有限公司 | FePO4/high polymer cracked carbon composite material and preparation method thereof, and NH4Fe2(OH)(PO4)2.2H2O/high polymer composite material and preparation method thereof |
| CN102694169B (en) * | 2012-03-07 | 2014-11-12 | 湖北万润新能源科技发展有限公司 | FePO4/high polymer cracked carbon composite material and preparation method thereof, and NH4Fe2(OH)(PO4)2.2H2O/high polymer composite material and preparation method thereof |
| CN103682338A (en) * | 2013-12-23 | 2014-03-26 | 向勇 | Preparation method for high-conductivity LiFePO4 cathode material |
| CN103682338B (en) * | 2013-12-23 | 2017-02-15 | 向勇 | Preparation method for high-conductivity LiFePO4 cathode material |
| CN104091946A (en) * | 2014-07-14 | 2014-10-08 | 中国科学技术大学苏州研究院 | Method for integrally synthesizing LiMnPO4/C by solvent and carbon source |
| CN106207178A (en) * | 2015-04-30 | 2016-12-07 | 苏州艾美得新能源材料有限公司 | The preparation method of positive electrode, positive electrode and battery |
| CN105514430A (en) * | 2015-12-30 | 2016-04-20 | 山东精工电子科技有限公司 | Spherical LiFexMnyPO4 anode material and preparation method thereof |
| CN107452949A (en) * | 2017-08-06 | 2017-12-08 | 长沙小新新能源科技有限公司 | A kind of LiFe1‑XNiXPO4The preparation method of/C Anode of lithium cell materials |
| CN109346698A (en) * | 2018-10-15 | 2019-02-15 | 西北有色金属研究院 | A kind of in-situ preparation method of the lithium-rich manganese-based two-phase electrode material of LiFePO4- |
| CN109346698B (en) * | 2018-10-15 | 2020-06-26 | 西北有色金属研究院 | In-situ preparation method of lithium iron phosphate-lithium-rich manganese-based dual-phase electrode material |
| CN110323434A (en) * | 2019-07-11 | 2019-10-11 | 江苏力泰锂能科技有限公司 | Prepare iron manganese phosphate for lithium-carbon composite method and iron manganese phosphate for lithium-carbon composite |
| CN110323434B (en) * | 2019-07-11 | 2022-07-22 | 江苏力泰锂能科技有限公司 | Method for preparing lithium iron manganese phosphate-carbon composite material and lithium iron manganese phosphate-carbon composite material |
| CN112390241A (en) * | 2020-11-17 | 2021-02-23 | 湖北融通高科先进材料有限公司 | Lithium iron phosphate material and method for preparing lithium iron phosphate material by taking mixed iron source and mixed lithium source as raw materials |
| CN112490439A (en) * | 2020-12-03 | 2021-03-12 | 湖北融通高科先进材料有限公司 | Method for preparing lithium iron phosphate material by taking mixed iron source and mixed phosphorus source as raw materials and lithium iron phosphate material prepared by method |
| CN113745503A (en) * | 2021-08-04 | 2021-12-03 | 北京泰丰先行新能源科技有限公司 | Preparation method of high-compaction lithium iron phosphate cathode material |
| CN115259128A (en) * | 2022-08-05 | 2022-11-01 | 湖北融通高科先进材料有限公司 | Preparation method of high-compaction high-capacity low-cost lithium iron phosphate |
| CN115259128B (en) * | 2022-08-05 | 2023-10-13 | 湖北融通高科先进材料集团股份有限公司 | Preparation method of high-compaction high-capacity low-cost lithium iron phosphate |
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Application publication date: 20110413 |