CN107265429B - Method for producing lithium iron phosphate R by water phase method - Google Patents
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- CN107265429B CN107265429B CN201710332655.2A CN201710332655A CN107265429B CN 107265429 B CN107265429 B CN 107265429B CN 201710332655 A CN201710332655 A CN 201710332655A CN 107265429 B CN107265429 B CN 107265429B
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
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Abstract
The invention relates to a method for producing iron phosphate R lithium by a water phase method (R is manganese, vanadium and cobalt). Its purpose is to provide a low-cost, working voltageA production method of lithium iron phosphate R lithium (R is manganese, vanadium and cobalt) which is a high and sufficient specific energy lithium ion battery anode material. The method for producing the lithium iron phosphate R by the aqueous phase method comprises the following steps: firstly, excessive phosphoric acid and dissolved LiNixCoyMnzO2Reacting to generate nickel phosphate precipitate, filtering and washing to obtain LiCoyMnzPO4(ii) a Adding iron powder and hydrogen peroxide into the mixture in sequence to react to obtain LiR' FePO4(R' is Co and Mn), and then centrifuging, washing and drying; then vanadium source and LiR' FePO are added4(R' is Co and Mn) and roasting at a certain temperature to obtain a product LiRFePO4(R is Co, Mn, V). The iron phosphate R lithium (R is manganese, vanadium and cobalt) produced by the method has the advantages of low cost, high working voltage, high specific energy, strong rate capability, safety, good cycle performance and the like. The invention is used in the technical field of lithium ion batteries.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for producing lithium iron phosphate R (R is manganese, vanadium and cobalt) by a water phase method.
Background
The positive electrode material of the lithium ion battery is an important component of a lithium ion battery system, and factors such as the performance and price of the positive electrode material are bottlenecks which restrict the further development of the lithium ion battery to high energy, long service life and low cost, and are one of important factors which determine the performance of the lithium ion battery.
LiFePO having an olivine structure has been reported by Goodenough et al 19974The lithium ion battery anode material can be used as a lithium ion battery, is low in price, good in cycling stability and the like, and is considered to be one of lithium ion battery anode materials with development prospects. But the use voltage is only 3.2V, the rate capability is insufficient, and the requirement of a high-energy power battery cannot be met. And LiMnPO4The cycling stability is weaker, and the lithium ion battery has the characteristics of higher use voltage (3.8V), low self-discharge rate and low cost. LiFePO doped with Mn4As the lithium ion anode material-lithium manganese iron phosphate (LiMn)xFe1－xPO4)，Mn3+/Mn2+The potential for lithium is about 4.1V, and the operating voltage is between the two, and Li insertion and extraction can be achieved, but there are problems of poor storage performance, insufficient cycle stability, and the like.
Then, Ohzuku et al and Dahn project group prepare ternary material LiNixCoyMnzO2. The ternary material used as the anode material of the lithium ion battery has the characteristics of (1) stable structure in the charge and discharge process, and Mn4+Do not take part in the contraryShould thus have no Jahn-Teller effect; (2) the safety performance is high, and the working temperature range is wide; (3) the specific capacity is high; (4) the cost is higher than that of LiCoO2Low. However, the ternary material has the problems of low tap density, cation mixed arrangement caused by the existence of nickel and the like.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for producing the lithium iron phosphate R (R is manganese, vanadium and cobalt) by a water phase method, which has the advantages of low cost, high working voltage, sufficient specific energy, strong rate capability, safety and good cycle performance.
On the basis of a ternary positive electrode material of a lithium ion battery, the ternary positive electrode material is doped and modified, nickel in the ternary positive electrode material is removed, vanadium is doped, and iron phosphate R lithium (R is manganese, vanadium and cobalt) is obtained.
In order to achieve the purpose, the invention provides a method for preparing lithium iron phosphate R (R is manganese, vanadium and cobalt) by an aqueous phase method, which comprises the following steps:
(1) the ternary positive electrode material LiNi of the lithium ion batteryxCoyMnzO2After dissolution, adding excessive phosphoric acid solution, reacting phosphoric acid with doping material-nickel to generate nickel phosphate precipitate, filtering, and washing to obtain LiCoyMnzPO4Said LiNixCoyMnzO2Wherein x + y + z is 1, and x, y and z are the mole numbers thereof;
(2) sequentially adding iron powder and hydrogen peroxide into the LiCo obtained in the step (1)yMnzPO4In the middle, the reaction is complete, LiR' FePO is generated4Wherein R' is Co or Mn;
(3) the obtained LiR' FePO4Wherein R' is Co and Mn, centrifuging, washing with water, and drying;
(4) mixing a vanadium source with LiR' FePO4Wherein R' is Co and Mn, mixing, grinding and roasting to obtain a product LiRFePO4Wherein R is Co, Mn, V.
Firstly, adding excessive phosphoric acid into a ternary cathode material LiNi of the lithium ion batteryxCoyMnzO2In the reaction, nickel phosphate precipitate is generated, and the obtained precipitate is filtered and washed to obtain LiCoyMnzPO4(ii) a Sequentially adding a certain amount of iron powder and hydrogen peroxide (adding hydrogen peroxide to oxidize ferrous ions into trivalent iron ions and ensure that the ferric ions in a system are trivalent) into LiCo according to a certain proportionyMnzPO4In the reaction, the LiR' FePO is obtained through hydrothermal reaction4(R' is Co or Mn); the obtained LiR' FePO4(R' is Co and Mn) and centrifuging, washing and drying; then a certain amount of vanadium source and LiR' FePO are added4(R' is Co and Mn) and roasting at a certain temperature to obtain a product LiRFePO4(R is Co, Mn, V).
H2O2+2Fe2++2H+＝2Fe3++2H2O
The cobalt-doped material not only can stabilize the layered structure of the material, but also can improve the cycle and rate performance of the material; the manganese doping is characterized by reducing material cost, high working voltage and improving material safety and structural stability. The doping of V can simultaneously improve the electron multiplying power performance and Li of the material+The rate of diffusion.
Preferably, LiNi in the step (1)xCoyMnzO2Is a solution.
Preferably, the lithium ion ternary material LiNi in the step (1)xCoyMnzO2Wherein y: z ═ 1 to 2: 1.
preferably, the molar ratio of the iron powder to the hydrogen peroxide in the step (2) is 2: 1.
Preferably, the reaction temperature in the step (2) is 80-120 ℃, and the reaction time is 1-3 h.
Preferably, the vanadium source in the step (4) is one or more of vanadium pentoxide, vanadium trioxide and vanadium dioxide.
Preferably, the vanadium source added in the step (4) is LiR' FePO40.01-0.05% of the mass.
Preferably, the roasting temperature in the step (4) is 600-900 ℃.
The method for producing the lithium iron phosphate R by the aqueous phase method is different from the prior art in that:
by adopting the technical scheme of the invention, the obtained lithium iron phosphate R has the advantages of low cost, high working voltage, high specific energy, strong rate capability, safety, good cycle performance and the like.
Detailed Description
The method for producing lithium iron phosphate R according to the invention by the aqueous phase process is further illustrated by the following examples and validation tests.
Example 1
The method for producing lithium iron phosphate R (R is manganese, vanadium and cobalt) by the aqueous phase method in the embodiment comprises the following steps:
a. the lithium ion battery ternary material LiNixCoyMnzO2After dissolution (LiNi)xCoyMnzO2Wherein x + y + z is 1, and x, y and z are the mole numbers), adding excessive phosphoric acid solution, reacting phosphoric acid with doping material nickel in the ternary material to generate nickel phosphate precipitate, filtering the precipitate, and washing to obtain LiCoyMnzPO4The molar ratio y: z is 1;
b. adding iron powder and hydrogen peroxide in a molar ratio of 2:1 into the obtained LiCo in sequenceyMnzPO4In the solution, the hydrothermal reaction is carried out to generate LiR' FePO4(R' is Co and Mn), the reaction temperature is 80 ℃, and the reaction is carried out for 1 h;
c. the obtained LiR' FePO4(R' is Co and Mn), centrifuging, washing with water, and drying;
d. 0.01 percent of vanadium source and LiR' FePO4(R' is Co and Mn) and roasting at a certain temperature to obtain a product LiRFePO4(R is Co, Mn and V), and the roasting temperature is 600 ℃.
After the treatment, the product is measured, the discharge voltage of the anode material is 3.6V, the first discharge specific capacity is 157.8mAh/g under 0.1C multiplying power, and the discharge capacity is attenuated by 2.8% after 30 times of circulation.
Example 2
The method for producing lithium iron phosphate R (R is manganese, vanadium and cobalt) by the aqueous phase method in the embodiment comprises the following steps:
a. the lithium ion battery ternary material LiNixCoyMnzO2After dissolution, adding excessive phosphoric acid solution, reacting phosphoric acid with doping material nickel in the ternary material to generate nickel phosphate precipitate, filtering the precipitate, and washing to obtain LiCoyMnzPO4，y：z＝1；
b. Adding iron powder and hydrogen peroxide into the obtained LiCo in sequence according to the molar ratio of 2:1yMnzPO4In the solution, the hydrothermal reaction is carried out to generate LiR' FePO4(R' is Co and Mn), the reaction temperature is 90 ℃, and the reaction time is 1.5 h;
c. the obtained LiR' FePO4(R' is Co and Mn), centrifuging, washing with water, and drying;
d. 0.02% of vanadium source and LiR' FePO4(R' is Co and Mn) and roasting at a certain temperature to obtain a product LiRFePO4(R is Co, Mn and V), and the roasting temperature is 650 ℃.
After the treatment, the product is measured, the discharge voltage of the anode material is 3.8V, the first discharge specific capacity is 164.8mAh/g under 0.1C multiplying power, and the discharge capacity is attenuated by 2.5 percent after 30 times of circulation.
Example 3
The method for producing lithium iron phosphate R (R is manganese, vanadium and cobalt) by the aqueous phase method in the embodiment comprises the following steps:
a. the lithium ion battery ternary material LiNixCoyMnzO2After dissolution, adding excessive phosphoric acid solution, reacting phosphoric acid with doping material nickel in the ternary material to generate nickel phosphate precipitate, filtering the precipitate, and washing to obtain LiCoyMnzPO4，y：z＝1.5；
b. Adding iron powder and hydrogen peroxide into the obtained LiCo in sequence according to the molar ratio of 2:1yMnzPO4In the solution, the hydrothermal reaction is carried out to generate LiR' FePO4(R' is Co and Mn), the reaction temperature is 100 ℃, and the reaction is carried out for 2 hours;
c. the obtained LiR' FePO4(R' is Co and Mn), centrifuging, washing with water, and drying;
d. 0.03 percent of vanadium source and LiR' FePO4(R' is Co and Mn) and roasting at a certain temperature to obtain a product LiRFePO4(R is Co, Mn and V), and the roasting temperature is 700 ℃.
After the treatment, the product is measured, the discharge voltage of the anode material is 4.5V, the first discharge specific capacity is 175.2mAh/g under 0.1C multiplying power, and the discharge capacity is attenuated by 2.3% after 30 times of circulation.
Example 4
The method for producing lithium iron phosphate R (R is manganese, vanadium and cobalt) by the aqueous phase method in the embodiment comprises the following steps:
a. the lithium ion battery ternary material LiNixCoyMnzO2After dissolution, adding excessive phosphoric acid solution, reacting phosphoric acid with doping material nickel in the ternary material to generate nickel phosphate precipitate, filtering the precipitate, and washing to obtain LiCoyMnzPO4，y：z＝1.5；
b. Adding iron powder and hydrogen peroxide into the obtained LiCo in sequence according to the molar ratio of 2:1yMnzPO4In the solution, the hydrothermal reaction is carried out to generate LiR' FePO4(R' is Co and Mn), the reaction temperature is 110 ℃, and the reaction lasts for 2.5 h;
c. the obtained LiR' FePO4(R' is Co and Mn), centrifuging, washing with water, and drying;
d. 0.04% vanadium source was mixed with LiR' FePO4(R' is Co and Mn) and roasting at a certain temperature to obtain a product LiRFePO4(R is Co, Mn and V) and the roasting temperature is 800 ℃.
After the treatment, the product is measured, the discharge voltage of the anode material is 4.2V, the first discharge specific capacity is 173.2mAh/g under 0.1C multiplying power, and the discharge capacity is attenuated by 2.1% after 30 times of circulation.
Example 5
The method for producing lithium iron phosphate R (R is manganese, vanadium and cobalt) by the aqueous phase method in the embodiment comprises the following steps:
a. ternary lithium ion batteryLiNi materialxCoyMnzO2After dissolution, adding excessive phosphoric acid solution, reacting phosphoric acid with doping material nickel in the ternary material to generate nickel phosphate precipitate, filtering the precipitate, and washing to obtain LiCoyMnzPO4，y：z＝2；
b. Adding iron powder and hydrogen peroxide into the obtained LiCo in sequence according to the molar ratio of 2:1yMnzPO4In the solution, the hydrothermal reaction is carried out to generate LiR' FePO4(R' is Co and Mn), the reaction temperature is 120 ℃, and the reaction is carried out for 3 hours;
c. the obtained LiR' FePO4(R' is Co and Mn), centrifuging, washing with water, and drying;
d. 0.05% vanadium source was mixed with LiR' FePO4(R' is Co and Mn) and roasting at a certain temperature to obtain a product LiRFePO4(R is Co, Mn and V), and the roasting temperature is 900 ℃.
After the treatment, the product is measured, the discharge voltage of the anode material is 4.5V, the first discharge specific capacity is 168.7mAh/g under 0.1C multiplying power, and the discharge capacity is attenuated by 1.8% after 30 times of circulation.
According to the embodiment, the iron phosphate R lithium prepared by the method has the advantages of low cost, high working voltage, high specific energy, strong rate capability, good safety cycle performance and the like, and can meet the use requirement of the lithium ion battery cathode material.
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and that the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the spirit and scope of the invention, and these changes and modifications are within the scope of the invention.
Claims (8)
1. A method for producing lithium iron phosphate R by a water phase method is characterized by comprising the following steps: the method comprises the following steps:
(1) LiNixCoyMnzO2After dissolution, add an excessPhosphoric acid solution, phosphoric acid and nickel react to generate nickel phosphate precipitate, and LiCoyMnzPO is obtained after filtering and washing4Said LiNixCoyMnzO2Wherein x + y + z is 1, and x, y and z are the mole numbers thereof;
(2) sequentially adding iron powder and hydrogen peroxide into the LiCoyMnzPO obtained in the step (1)4In the middle, the reaction is complete, LiR' FePO is generated4Wherein R' is Co and Mn;
(3) the obtained LiR' FePO4Wherein R' is Co and Mn, centrifuging, washing with water, and drying;
(4) mixing a vanadium source with LiR' FePO4Wherein R' is Co and Mn, mixing, grinding and roasting to obtain a product LiRFePO4Wherein R is Co, Mn and V.
2. The aqueous phase method for producing lithium iron phosphate R according to claim 1, characterized in that: LiNixCoyMnzO in the step (1)2Is a solution.
3. The aqueous phase method for producing lithium iron phosphate R according to claim 1, characterized in that: the lithium ion ternary material LiNixCoyMnzO in the step (1)2Wherein y: and z is (1-2) and 1.
4. The aqueous phase method for producing lithium iron phosphate R according to claim 1, characterized in that: the molar ratio of the iron powder to the hydrogen peroxide in the step (2) is 2: 1.
5. The aqueous phase method for producing lithium iron phosphate R according to claim 1, characterized in that: the reaction temperature in the step (2) is 80-120 ℃, and the reaction time is 1-3 h.
6. The aqueous phase method for producing lithium iron phosphate R according to claim 1, characterized in that: and (3) the vanadium source in the step (4) is one or more of vanadium pentoxide, vanadium trioxide and vanadium dioxide.
7. According to the claimsThe method for producing the lithium iron phosphate R by the aqueous phase method according to the formula 1 is characterized by comprising the following steps: the addition amount of the vanadium source in the step (4) is LiR' FePO40.01-0.05% of the mass.
8. The aqueous phase method for producing lithium iron phosphate R according to claim 1, characterized in that: the roasting temperature in the step (4) is 600-900 ℃.
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