CN102074687A - Hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate - Google Patents
Hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate Download PDFInfo
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Abstract
The invention discloses a hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate, which belongs to the field of lithium-ion battery anode materials and comprises the following steps of: sequentially adding a phosphorus-source solution, an iron-source solution, a carbon source, a lithium-source solution and a boiling-point elevator into a reaction device in sequence, mixing, then heating to the temperature of 60-180 DEG C for reaction under inert gas, cooling after the reaction, filtering precipitates to obtain a nano-scale lithium iron phosphate precursor, and then sintering the nano-scale lithium iron phosphate precursor at the temperature of 400-600 DEG C under the protection of the mixed gas of the inert gas and hydrogen gas. The combination of lithium, iron, phosphorus and the like on a molecular level is realized by the method, and the grains of a product are quite fine and are uniformly distributed; because the boiling-point elevator is adopted, the reaction temperature and pressure of the reaction kettle are decreased; and the hydrothermal synthesis method has the advantages of simple preparation process, short flow, easiness in operational control, low reaction temperature, short time, low energy consumption and easiness in realizing large-scale industrialized production.
Description
Technical field
The invention belongs to the anode material for lithium-ion batteries field, be specifically related to a kind of preparation method of anode material for lithium-ion batteries nano-scale carbon-covered iron lithium phosphate.
Background technology
Along with the fast development of new energy automobile, lithium ion battery particularly is that anodal lithium ion battery will be widely used in hybrid vehicle (HEV), pure electric automobile (EV) with the LiFePO 4 material.Compare with the lithium ion battery of other positive electrodes, ferric phosphate lithium cell has and has extended cycle life, and fail safe is good, can fast charging and discharging, and advantage such as cost is low, and is pollution-free.There is following shortcoming in the synthetic LiFePO4 of known method at present: ferrous iron Fe in (1) building-up process
2+Be oxidized to ferric iron Fe easily
3+, be difficult to obtain the LiFePO4 of pure phase, promptly impurity is more, influences capacity; (2) particulate is thicker, and inhomogeneous, and lithium ion is at LiFePO
4The speed of middle diffusion mobility is slower, has caused the active material ionic conducting property bad, and influence discharges and recharges speed; (3) LiFePO
4The electric conductor of itself is lower, influences its high-rate discharge ability.
Summary of the invention
The objective of the invention is to improve, a kind of method of new synthesis nano carbon-coated LiFePO 4 for lithium ion batteries is provided at the problems referred to above.
Purpose of the present invention can reach by following measure:
A kind of hydrothermal synthesis method for preparing nano-scale carbon-covered iron lithium phosphate; the steps include: to add in the reaction unit successively phosphorus source solution, source of iron solution, carbon source, lithium source solution and boiling point elevator in order; fully mix; be full of under the condition of inert gas; being heated to 60 ℃～180 ℃ reacts; reaction back cooling (as natural cooling); filter out sediment; obtain the nano-scale lithium iron phosphate presoma; then with this nano-scale lithium iron phosphate presoma inert gas and hydrogen mixed gas protected down, in 400 ℃～600 ℃ following sintering.Be cooled to room temperature behind the sintering, promptly make nanoscale, carbon-coated LiFePO 4 for lithium ion batteries powder (LiFePO
4/ C).
This method is mixed with the aqueous solution or water slurry with deionized water or pure water with lithium compound, iron compound, phosphorus compound respectively earlier in proportion.Wherein the phosphorus source is selected from one or more in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, lithium phosphate, the ferric phosphate; Described phosphorus source solution is the aqueous solution in phosphorus source, and its concentration is 0.2～3.5mol/L.
Source of iron is selected from one or more in frerrous chloride, ferrous sulfate, ferrous acetate, the ferrous oxalate; The aqueous solution or water slurry that described source of iron solution is source of iron, its concentration are 0.2～3.5mol/L.
The lithium source is selected from one or more in lithium hydroxide, lithium chloride, lithium nitrate, lithium carbonate, lithium sulfate, the lithium phosphate; Described lithium source solution is the aqueous solution or the water slurry in lithium source, and its concentration is 0.2～3.5mol/L.
The consumption of lithium source, source of iron and P source compound is preferably 1～3 in lithium, iron, its mol ratio of P elements respectively in this method: 1: 1.
Carbon source comprises reducing agent and/or dispersant, described carbon source is selected from one or more in sucrose, carbon black, graphite, multiple-wall carbon nanotube, ascorbic acid, citric acid, glycine, glycerine, polyethylene glycol, the softex kw, and the consumption of carbon source is 0.1～25% of nanoscale, a carbon-coated LiFePO 4 for lithium ion batteries target product weight.Reducing agent adds reaction system prior to dispersant in the carbon source.
The boiling point elevator is selected from one or more in glycerine, polyethylene glycol, dimethyl sulfoxide (DMSO), the sulfolane; Described boiling point elevator consumption is for adding 30%～50% of the preceding reaction solution volume of boiling point elevator.
Inert gas of the present invention is preferably nitrogen or argon gas, and in the mist of described inert gas and hydrogen, the volume content of nitrogen or argon gas is 95～98%, and the volume content of hydrogen is 2～5%.Inert gas can inject from the reaction unit bottom.
In the said method, filter out sediment after, washing earlier, vacuumize oven dry again can obtain nanoscale, carbon-coated LiFePO 4 for lithium ion batteries presoma.The reaction time for preparing described nano-scale lithium iron phosphate presoma is 2～8 hours, and reaction temperature is preferably 120 ℃～150 ℃, and the preceding elder generation of reaction for preparing described nano-scale lithium iron phosphate presoma injects and the expulsion air from the reaction unit bottom with inert gas; The time of described sintering is 2～8 hours.Method of the present invention can obtain the carbon-coated LiFePO 4 for lithium ion batteries that average grain diameter D50 is 200～300nm, and particle diameter evenly distributes.
The present invention is directed to the problems of the prior art, adopted new synthesis technique to solve:
(1) before adding thermal response, mixed liquor nitrogen injection or argon gas are added reducing agent simultaneously to suppress Fe
2+Oxidation; (2) by adding the former and dispersant of carbon with the restriction crystal growth, thus the nanometer particle of synthetic uniformity, and the stroke when taking off embedding to reduce lithium ion is accelerated the diffusion velocity of lithium ion in positive electrode, has just improved ionic conductivity; (3), product is just realized that carbon coats when the crystallization, thereby improve conductivity of electrolyte materials by adding carbon, particularly organic carbon source.(4) the present invention has adopted the technology that boiling point promotes, making hydro-thermal reaction to carry out under lower temperature under the cooperatively interacting of each material, than being easier to realize suitability for industrialized production.
Characteristics of the present invention are: the gram volume of (1) product can pass through to change technological parameter, as different lithium sources, and different sources of iron, or different carbon sources, different reaction temperatures, control flexibly.(2) the present invention is chemical synthesis, has realized the combination on lithium, iron and the phosphorus equimolecular level, the even particle distribution of product, and D50 is between 200～300nm.(3) the carbon coating is even realization of method by chemistry; (4) application of boiling point elevator, it can improve the boiling point of overall reaction liquid under the cooperation of each component, and with the reaction temperature and the pressure of reduction reactor, and the organic carbon that decomposites at last is again good carbon source.The use of (5) dispersant, particularly softex kw has stoped the reunion of nanometer powder in the preparation process effectively and has grown up, and also is simultaneously the carbon source of high-quality very.(6) Zhi Bei technology is simple, and flow process is short, operation control easily, and reaction temperature is low, and the time is short, and energy consumption is low, easily realizes large-scale industrial production.
Description of drawings
Fig. 1 is the XRD diffraction pattern of embodiment 1 product;
Fig. 2 embodiment 1 product S EM electron-microscope scanning;
Fig. 3 embodiment 2 product X RD diffraction patterns;
Fig. 4 embodiment 2 product S EM electron-microscope scannings.
Embodiment
Synthesis technique of the present invention mainly divides two stages:
1, heating reaction precipitation nanoscale presoma
With deionized water or pure water preparation Li source compound solution or suspension, the lithium source is selected from a kind of in lithium hydroxide, lithium chloride, lithium nitrate, lithium carbonate, lithium sulfate, the lithium phosphate; With deionized water or pure water preparation Fe source compound solution, Fe source compound is selected from a kind of in frerrous chloride, ferrous sulfate, ferrous oxalate, the ferrous acetate.With deionized water or pure water preparation P source compound solution, P source compound is selected from phosphoric acid, ammonium dihydrogen phosphate, a kind of in the diammonium hydrogen phosphate.Consumption in molar ratio, lithium: iron: phosphorus=1～3: determine that solution concentration is 0.2～3.5mol/L at 1: 1.Carbon source comprises that reducing agent, dispersant are selected from sucrose, carbon black, graphite, Duo Bina; In rice carbon pipe, ascorbic acid, citric acid, glycine, glycerine, polyethylene glycol, the softex kw one or more, consumption is the 0.1-25% of target product weight.The boiling point elevator is selected from a kind of in glycerine, polyethylene glycol, dimethyl sulfoxide (DMSO), the sulfolane.Consumption is 30%～50% of a reactant liquor volume, pressing order adds in the reactor successively: phosphorus source-source of iron-carbon source (comprising reducing agent and dispersant)-lithium source-boiling point elevator capping still, from reactor bottom nitrogen injection or argon gas expulsion oxygen, begin to be heated to 60 ℃～180 ℃ then, and constant temperature stirred 2～8 hours.Mother liquor is taken out in cooling back, to sediment filter, washing, vacuumize oven dry.
2, high temperature sintering nanoscale presoma
With the nanometer presoma of the step 1 preparation saggar of packing into, and saggar placed meshbeltfurnace or pusher furnace or the nanometer presoma is placed directly in rotary furnace, heat-treat.Be full of the mist of the hydrogen of 95～98% inert gas (nitrogen or argon gas) and 2～5% in the whole burner hearth; make sintering under the protection of mist; stop new ferrous iron to be oxidized to ferric iron, simultaneously oxidized ferric iron is reduced into ferrous iron.The temperature of sintering is 400 ℃～600 ℃, and constant temperature time is 2～8 hours.
Embodiment 1.
Press Li: Fe: P=3: 1: 1 molar ratio, get 12.6 kilograms of monohydrate lithium hydroxide (LiOHH
2O) add 100 liters of deionized waters, get 27.8 kilograms of ferrous sulfate heptahydrate (FeSO
47H
2O) add 200 liters of deionized waters, get 11.5 kilograms of phosphoric acid (85%H
3PO
4) add 30 liters of deionized waters, be mixed with the aqueous solution respectively.15 kilograms of scheduled target products.At first add phosphoric acid solution in reactor, next adds copperas solution, then adds 1.5 kilograms carbon black, after fully mixing, adds lithium hydroxide solution, adds 350 liters of glycerine at last.Be blown into nitrogen one hour from the reactor bottom, discharge all air in the reactor, sealed reactor begins heating then, is heated to 120 ℃, and keeps 3 hours, cooled and filtered, washing, vacuumize oven dry products therefrom.The saggar of at last it being packed into, through the meshbeltfurnace sintering, sintering condition: nitrogen with 95% and 5% hydrogen mixed gas protected, 550 ℃ of sintering temperatures, sintering time 3 hours obtains 13.8 kilograms of finished product LiFePO
4/ C powder.
Through X-ray diffraction analysis, show that product is olivine-type LiFePO
4, crystalline structure is complete, does not have the dephasign (see figure 1).The particle diameter of product is seen SEM electron-microscope scanning (Fig. 2) about 200nm.The nanoscale LiFePO4/C of preparation is carried out the charge-discharge performance test, positive pole is made by weight 7.5: 1.5: 1 with prepared material, acetylene black and Kynoar (PVDF), negative pole adopts metal lithium sheet, and barrier film adopts Celgard 2400, and electrolyte is 1mol/L lithium hexafluoro phosphate (LiPF
6) being dissolved in ethylene carbonate, the mixed liquor of dimethyl carbonate and diethyl carbonate (volume ratio EC: DMC: DEC=1: 1: 1) is made the CR2032 button cell.Through the test of BTS high accuracy battery detection system, the voltage range that discharges and recharges is 2.5V～4.2V, and sample 0.1C multiplying power discharging capacity is 146mAh/g, and 1C multiplying power discharging capacity is 131mAh/g.
Embodiment 2.
Press Li: Fe: P=1: 1: 1 molar ratio, get 6.9 kilograms of lithium nitrate (LiNO
3) add 100 liters of deionized waters, get 12.7 kilograms of frerrous chloride (FeCl
2) add 200 liters of deionized waters and 11.5 kilograms of phosphoric acid (85%H
3PO
4) add 30 liters of deionized waters, be mixed with the aqueous solution respectively.10 kilograms of scheduled target products.Get 0.5 kilogram of softex kw, add 35 ℃ of left and right sides deionized waters and fully be mixed with dispersant solution after the stirring for 2 liters.At first add phosphoric acid solution in reactor, next adds solution of ferrous chloride, then adds 0.5 kilogram of sucrose and 0.5 kilogram of carbon black, after fully mixing, adds lithium nitrate solution, along with adding dispersant solution, adds 350 liters of polyethylene glycol at last.Be blown into nitrogen one hour from the reactor bottom, discharge all air in the reactor, sealed reactor begins heating then, is heated to 150 ℃, and keeps 3 hours, cooled and filtered, washing, vacuumize oven dry products therefrom.The saggar of at last it being packed into, through the meshbeltfurnace sintering, sintering condition: nitrogen with 98% and 2% hydrogen mixed gas protected, 600 ℃ of sintering temperatures, sintering time 3 hours obtains 8.9 kilograms of finished product LiFePO
4/ C powder.
Through X-ray diffraction analysis, show that product is olivine-type LiFePo
4, crystalline structure is complete, does not have the dephasign (see figure 3).The particle diameter of product is seen SEM electron-microscope scanning (Fig. 4) about 200nm.The nanoscale LiFePO4/C of preparation is carried out the charge-discharge performance test, positive pole is made by weight 8: 1: 1 with prepared material, acetylene black and Kynoar (PVDF), negative pole adopts metal lithium sheet, and barrier film adopts Celgard 2400, and electrolyte is 1mol/L lithium hexafluoro phosphate (LiPF
6) being dissolved in ethylene carbonate, the mixed liquor of dimethyl carbonate and diethyl carbonate (volume ratio EC: DMC: DEC=1: 1: 1) is made the CR2032 button cell.Through the test of BTS high accuracy battery detection system, the voltage range that discharges and recharges is 2.5V～4.2V, and sample 0.1C multiplying power discharging capacity is 152mAh/g, and 1C multiplying power discharging capacity is 138mAh/g.
Claims (9)
1. hydrothermal synthesis method for preparing nano-scale carbon-covered iron lithium phosphate; it is characterized in that: add in the reaction unit successively phosphorus source solution, source of iron solution, carbon source, lithium source solution and boiling point elevator in order; fully mix; be full of under the condition of inert gas; being heated to 60 ℃～180 ℃ reacts; the cooling of reaction back; filter out sediment; obtain the nano-scale lithium iron phosphate presoma; then with this nano-scale lithium iron phosphate presoma inert gas and hydrogen mixed gas protected down, in 400 ℃～600 ℃ following sintering.
2. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1 is characterized in that: described phosphorus source is selected from one or more in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, lithium phosphate, the ferric phosphate; Described phosphorus source solution is the aqueous solution in phosphorus source, and its concentration is 0.2～3.5mol/L.
3. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1 is characterized in that: described source of iron is selected from one or more in frerrous chloride, ferrous sulfate, ferrous acetate, the ferrous oxalate; The aqueous solution or water slurry that described source of iron solution is source of iron, its concentration are 0.2～3.5mol/L.
4. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1, it is characterized in that: described carbon source comprises reducing agent and/or dispersant, described carbon source is selected from one or more in sucrose, carbon black, graphite, multiple-wall carbon nanotube, ascorbic acid, citric acid, glycine, glycerine, polyethylene glycol, the softex kw, and the consumption of carbon source is 0.1～25% of a nano-scale carbon-covered iron lithium phosphate product weight.
5. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1 is characterized in that: described lithium source is selected from one or more in lithium hydroxide, lithium chloride, lithium nitrate, lithium carbonate, lithium sulfate, the lithium phosphate; Described lithium source solution is the aqueous solution or the water slurry in lithium source, and its concentration is 0.2～3.5mol/L.
6. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1 is characterized in that: described boiling point elevator is selected from one or more in glycerine, polyethylene glycol, dimethyl sulfoxide (DMSO), the sulfolane; Described boiling point elevator consumption is for adding 30%～50% of the preceding reaction solution volume of boiling point elevator.
7. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1 is characterized in that: the consumption of described lithium source, source of iron and P source compound is 1～3 in lithium, iron, its mol ratio of P elements respectively: 1: 1.
8. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1, it is characterized in that: described inert gas is nitrogen or argon gas, in the mist of described inert gas and hydrogen, the volume content of inert gas is 95～98%, and the volume content of hydrogen is 2～5%.
9. the hydrothermal synthesis method of preparation nano-scale carbon-covered iron lithium phosphate according to claim 1, it is characterized in that: the reaction time for preparing described nano-scale lithium iron phosphate presoma is 2～8 hours, and the preceding elder generation of reaction for preparing described nano-scale lithium iron phosphate presoma injects and the expulsion air from the reaction unit bottom with inert gas; The time of described sintering is 2～8 hours.
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| CN102522551A (en) * | 2011-12-26 | 2012-06-27 | 彩虹集团公司 | Preparation method for LiFePO4 (lithium iron phosphate) superfine powder serving as power battery anode materials |
| CN102593457A (en) * | 2012-02-22 | 2012-07-18 | 中国石油大学(北京) | Preparation method of lithium iron phosphate-carbon material composite |
| CN103030128A (en) * | 2011-09-29 | 2013-04-10 | 北京当升材料科技股份有限公司 | Industrial production method for preparing nanometer lithium iron phosphate by adopting solvent thermal method |
| CN103904325A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | High-multiplying-power type lithium iron phosphate/carbon composite material and preparation method thereof |
| CN104051732A (en) * | 2014-04-10 | 2014-09-17 | 魏宏政 | Method for preparing lithium iron phosphate by clathration technology |
| US8962186B2 (en) | 2011-11-24 | 2015-02-24 | Tsinghua University | Lithium ion phosphate hierarchical structure, method for making the same, and lithium ion battery using the same |
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| US8962186B2 (en) | 2011-11-24 | 2015-02-24 | Tsinghua University | Lithium ion phosphate hierarchical structure, method for making the same, and lithium ion battery using the same |
| CN102522551A (en) * | 2011-12-26 | 2012-06-27 | 彩虹集团公司 | Preparation method for LiFePO4 (lithium iron phosphate) superfine powder serving as power battery anode materials |
| CN102593457A (en) * | 2012-02-22 | 2012-07-18 | 中国石油大学(北京) | Preparation method of lithium iron phosphate-carbon material composite |
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| CN103904325A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | High-multiplying-power type lithium iron phosphate/carbon composite material and preparation method thereof |
| CN104051732A (en) * | 2014-04-10 | 2014-09-17 | 魏宏政 | Method for preparing lithium iron phosphate by clathration technology |
| 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 |
| CN105576199A (en) * | 2015-12-09 | 2016-05-11 | 山东精工电子科技有限公司 | Preparation method of novel nano manganese lithium titanate LiMnxTiO4 cathode material |
| CN107069005A (en) * | 2017-04-19 | 2017-08-18 | 龙能科技如皋市有限公司 | A kind of preparation method of double-carbon-source coated LiFePO 4 material |
| CN108390057A (en) * | 2018-03-07 | 2018-08-10 | 南京理工大学 | The preparation method of additive Mn lithium iron phosphate electrode material |
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| CN114361448B (en) * | 2021-12-31 | 2023-07-14 | 欣旺达电动汽车电池有限公司 | Lithium iron phosphate, preparation method thereof and lithium ion battery |
| CN116216686A (en) * | 2023-03-28 | 2023-06-06 | 陕西创普斯新能源科技有限公司 | Preparation method of lithium iron phosphate anode material |
| CN116216686B (en) * | 2023-03-28 | 2024-04-19 | 陕西创普斯新能源科技有限公司 | Preparation method of lithium iron phosphate anode material |
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