CN114291852B - Preparation method of nickel-aluminum-coated nickel-iron-manganese-sodium ion precursor material - Google Patents
Preparation method of nickel-aluminum-coated nickel-iron-manganese-sodium ion precursor material Download PDFInfo
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Abstract
The invention discloses a preparation method of a nickel-aluminum coated nickel-iron-manganese sodium ion precursor material, which comprises the following steps: preparation of Ni x1 Fe y1 Mn 1‑x1‑y1 (OH) 2 A precursor; preparation of Ni with outer layer coated with Ni-Al hydroxide x2 Fe y2 Mn z2 Al 1‑x2‑y2‑z2 (OH) 2 An iron-based precursor; and uniformly mixing the nickel-iron-manganese-aluminum precursor coated with nickel-aluminum on the outer layer and sodium carbonate in a mortar and calcining. According to the invention, a layer of nickel-aluminum hydroxide is coated on the surface of the nickel-iron-manganese hydroxide at the precursor end, so that the distribution of aluminum elements on the surface of the finally formed sodium ion precursor material is uniform, and the reaction of the anode material and the electrolyte in the charge and discharge process is reduced; meanwhile, the nickel on the surface can also improve the energy of the sodium ion battery, and the nickel compound can also improve the ionic conductivity of the material and increase the rate capability. The sodium electrode material prepared by the method disclosed by the invention is of a sphere-like structure and has higher stability and safety.
Description
Technical Field
The invention relates to the field of sodium ion batteries, in particular to a preparation method of a nickel-aluminum coated nickel-iron-manganese sodium ion precursor material.
Background
In recent years, the new energy automobile industry is developed rapidly, the power battery material is mainly a lithium battery and comprises two technical routes of lithium iron phosphate and a ternary power battery, the lithium battery has excellent safety performance and low cost, and the ternary power battery has high energy density and strong cruising ability and is suitable for high-end automobile types. However, the cost of the power battery is gradually increasing due to the limited reserve of lithium resources and the high price cost. Compared with a lithium ion battery, the sodium ion battery has low cost and rich and easily-obtained Na resources, so that the sodium ion battery plays a role as a substitute in the new energy industry. The lithium ion battery is expected to be used for replacing and applying lithium ion batteries in the fields of energy storage and low-speed vehicles with low requirements on energy density and high cost sensitivity and partial low-endurance passenger vehicles. Meanwhile, the electrochemical performance of the sodium ion battery is relatively stable, passivation and inactivation are easy to occur in the thermal runaway process, and the safety test performance is better than that of a lithium battery. However, the radius of sodium ions is larger than that of lithium ions, so that multiple complex phase changes exist in the charging and discharging processes of the material, the structure is unstable, the material is sensitive to water and is easy to react with electrolyte, and the sodium ion battery material is limited due to the factors.
In the prior art, the performance of a sodium ion battery is improved by adopting a structural modification mode, for example, patent CN 109817970a provides an electrode material of a single crystal sodium ion battery, which can reduce the side reaction of the sodium ion electrode and improve the material from the structural aspect. However, the method for modifying the internal structure can only solve the problem that the internal structure of the sodium ion battery material is unstable, but cannot solve the problem that sodium ions are sensitive to water and easily react with electrolyte.
Disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a preparation method of a nickel-aluminum coated nickel-iron-manganese sodium ion precursor material, which specifically comprises the following steps:
a preparation method of a nickel-aluminum coated nickel-iron-manganese-sodium ion precursor material comprises the following steps:
(1) Soluble nickel salt, soluble iron salt and soluble manganese salt are mixed according to the molar ratio of x 1 :y 1 :1-x 1 -y 1 Preparing a nickel-iron-manganese metal salt solution A with the total metal ion concentration of 2-5mol/L according to the proportion, wherein x1 is more than or equal to 0.2 and less than or equal to 0.6,0.1 and less than or equal to y1 and less than or equal to 0.5; preparing ammonia water complexing agent solution with the concentration of 1-3 mol/L; preparation of OH - 1-3mol/L aqueous alkali;
(2) Adding the solution A prepared in the step (1), an ammonia water complexing agent solution and an alkali solution into a reaction kettle at a certain feeding speed, reacting for 50-80h at 40-70 ℃, controlling the reaction pH of the system to be 8.5-11 and the ammonia concentration to be 3.0-8.0g/L, and obtaining Ni x1 Fe y1 Mn 1-x1-y1 (OH) 2 A precursor;
(3) Preparing a soluble nickel salt solution with the nickel ion concentration of 0.5-1.5 mol/L; preparing a sodium metaaluminate solution with the aluminum ion concentration of 0.3-0.6 mol/L; preparing ammonia water solution with the concentration of 1-3 mol/L; preparing an alkali solution with the OH < - > concentration of 1-3 mol/L; adding the solution into the reaction kettle in the step (2) at a certain feeding speed, maintaining the pH of the reaction to be 10-12 and the ammonia concentration to be 5.0-10.0g/L, and stopping the reaction for 2-8h to obtain Ni with the outer layer coated with the nickel-aluminum hydroxide x2 Fe y2 Mn z2 Al 1-x2-y2-z2 (OH) 2 Iron-based precursor (x is more than or equal to 0.3) 2 ≤0.7,0.1≤y 2 ≤0.5,0.05≤z 2 ≤0.5);
(4) And uniformly mixing the nickel-iron-manganese-aluminum precursor coated with nickel and aluminum on the outer layer with sodium carbonate in a mortar, and calcining at 800-950 ℃ for 10-20h to obtain the nickel-iron-manganese-sodium ion precursor material coated with nickel and aluminum on the outer layer.
Specifically, the soluble nickel salt in the steps (1) and (3) is nickel sulfate, nickel chloride or nickel nitrate.
Specifically, the soluble iron salt in the step (1) is ferrous sulfate or ferrous chloride.
Specifically, the soluble manganese salt in the step (1) is manganese sulfate, manganese chloride or manganese nitrate.
Specifically, the step alkali solution is a sodium hydroxide, sodium carbonate or potassium hydroxide solution.
Specifically, the flow rate of the solution A in the step (2) is 30-50L/h, the flow rate of the ammonia water solution is 3-6L/h, the flow rate of the liquid caustic soda is 8-15L/h, and the stirring speed is 250-500r/min.
Specifically, in the step (3), the flow rate of the nickel sulfate solution is 10L/h, the flow rate of the ammonia water solution is 4-10L/h, the flow rate of the alkali solution is 2-6L/h, the flow rate of the sodium metaaluminate solution is 5-10L/h, and the stirring speed is 150-280r/min.
The invention has the beneficial effects that: according to the invention, a layer of nickel-aluminum hydroxide is coated on the surface of the nickel-iron-manganese hydroxide at the precursor end, so that the distribution of aluminum elements on the surface of the finally formed sodium ion precursor material is uniform, and the reaction of the anode material and the electrolyte in the charge and discharge process is reduced; meanwhile, the nickel on the surface can also improve the energy of the sodium ion battery, and the nickel compound can also improve the ionic conductivity of the material and increase the rate capability. The sodium electrode material prepared by the method disclosed by the invention is of a sphere-like structure and has higher stability and safety.
Drawings
FIG. 1 is Ni 0.65 Fe 0.16 Mn 0.16 Al 0.03 (OH) 2 SEM picture of the precursor;
FIG. 2 is Ni 0.65 Fe 0.16 Mn 0.16 Al 0.03 (OH) 2 SEM image of the cross-section of the precursor.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments. The embodiments shown below do not limit the inventive content described in the claims. The entire contents of the configurations shown in the following embodiments are not limited to those required as solutions of the inventions described in the claims.
Example 1
Step 1, preparing a nickel-iron-manganese metal salt A solution with the concentration of 2mol/L, and preparing an ammonia water complexing agent solution with the concentration of 1mol/L and a sodium hydroxide solution with the concentration of 1mol/L according to the molar ratio of 0.25.
Step 2, adding the solution A, the ammonia water complexing agent and the sodium hydroxide solution into a 1000L reaction kettle at a certain feeding speed, reacting for 50h at 40 ℃, and controlling the reaction pH of the system9.5-10, and the ammonia concentration is 3-5g/L. The precursor which has better sphericity, uniform primary particles and dense stacking is obtained: ni 0.25 Fe 0.5 Mn 0.25 (OH) 2 The average particle diameter of the precursor was 3 μm. The flow rate of the solution A is 30L/h, the flow rate of ammonia water is 3L/h, the flow rate of a sodium hydroxide solution is 8L/h, and the stirring speed is 280-350r/min.
And 3, preparing a nickel sulfate solution with the concentration of 1mol/L, a sodium metaaluminate solution with the concentration of 0.3mol/L, an ammonia water solution with the concentration of 2mol/L and a sodium hydroxide solution with the concentration of 2mol/L, continuously adding the above solutions into a reaction kettle at a certain feeding speed to continue the reaction, maintaining the pH of the reaction to be 10.5-11.0, the ammonia concentration to be 5.0-6.0g/L, the stirring speed to be 180-230r/min, the flow of the nickel sulfate to be 10L/h, the flow of the ammonia water to be 4L/h, the flow of the liquid alkali to be 2L/h, the flow of the sodium metaaluminate solution to be 5L/h, and stopping the reaction after 5h of reaction. To obtain a Ni 0.3 Fe 0.46 Mn 0.23 Al 0.01 (OH) 2 The sodium ion layered precursor comprises a precursor body, wherein a shell of the sodium ion layered precursor body is coated with a layer of nickel aluminum hydroxide.
Step 4, uniformly mixing the sodium ion layered precursor with the shell coated with the nickel-aluminum hydroxide layer and sodium carbonate in a mortar, and calcining at 800 ℃ for 20 hours to obtain the sodium ion battery anode material Na (Ni) coated with nickel-aluminum 0.3 Fe 0.46 Mn 0.23 Al 0.01 )O 2 。
SEM observation of the external and internal appearances of the obtained precursors was carried out, and the results are shown in FIGS. 1 and 2.
The prepared sodium ion battery cathode material is assembled into a button battery, and the capacity retention rate after 100 cycles under the current density of 120mA/g is 93%. Compared with the capacity retention rate of 85% of the conventional sodium ion precursor material, the battery prepared by the scheme has obvious advantages in the aspect of capacity retention rate.
Example 2
Step 1, preparing a nickel iron manganese metal salt A solution with the concentration of 2mol/L, and preparing an ammonia water complexing agent solution with the concentration of 2mol/L and a sodium carbonate solution with the concentration of 2mol/L according to the molar ratio of 0.34.
And 2, adding the solution A, an ammonia water complexing agent and a sodium carbonate solution into a 1000L reaction kettle at a certain feeding speed, reacting for 60 hours at 50 ℃, and controlling the reaction pH of the system to be 9-9.5 and the ammonia concentration to be 4-6g/L. Obtaining a precursor with good sphericity, coarse primary particles and dense stacking: ni 0.34 Fe 0.33 Mn 0.33 (OH) 2 The average particle diameter of the precursor was 5 μm. The flow rate of the solution A is 40L/h, the flow rate of ammonia water is 4L/h, the flow rate of liquid caustic soda is 10L/h, and the stirring speed is 260-320r/min.
And 3, continuously adding a nickel sulfate solution with the concentration of 0.5mol/L, a sodium metaaluminate solution with the concentration of 0.4mol/L, an ammonia water solution with the concentration of 1mol/L and a sodium carbonate solution with the concentration of 1mol/L into the reaction kettle at a certain feeding speed to continue the reaction, maintaining the pH value of the reaction to be 10.5-10.8, the ammonia concentration to be 5.5-6.5g/L, the stirring rotation speed to be 180-210r/min, the flow rate of the nickel sulfate to be 10L/h, the flow rate of the ammonia water to be 5L/h, the flow rate of the sodium carbonate solution to be 4L/h, the flow rate of the sodium metaaluminate solution to be 6L/h, and stopping the reaction for 3 h. To obtain a Ni 0.35 Fe 0.32 Mn 0.32 Al 0.01 (OH) 2 The shell of the sodium ion layered precursor is coated with a layer of nickel aluminum hydroxide.
Step 4, uniformly mixing the precursor of the nickel-aluminum hydroxide coated with the shell and sodium carbonate in a mortar, and calcining at 850 ℃ for 20 hours to obtain the nickel-aluminum-coated iron-based sodium-ion battery positive electrode material Na (Ni) 0.35 Fe 0.32 Mn 0.32 Al 0.01 )O 2 . The prepared sodium ion battery cathode material is assembled into a button battery, and the capacity retention rate of the button battery after 100 cycles under the current density of 120mA/g is 95%.
Example 3
Step 1, preparing a nickel-iron-manganese metal salt A solution with the concentration of 3mol/L, and preparing an ammonia water complexing agent solution with the concentration of 3mol/L and a potassium hydroxide solution with the concentration of 3mol/L according to the molar ratio of 0.6.
Step 2,Adding the solution A, an ammonia water complexing agent and a potassium hydroxide solution into a 1000L reaction kettle at a certain feeding speed, reacting for 80h at 70 ℃, and controlling the reaction pH of the system to be 9.8-10 and the ammonia concentration to be 6-8g/L. The precursor with better sphericity, more uniform primary particles and dense accumulation is obtained: ni 0.6 Fe 0.2 Mn 0.2 (OH) 2 The average particle size of the precursor was 10 μm. The flow rate of the solution A is 50L/h, the flow rate of ammonia water is 6L/h, the flow rate of a potassium hydroxide solution is 15L/h, and the stirring speed is 230-250r/min.
And 3, continuously adding a nickel sulfate solution with the concentration of 1.5mol/L, a sodium metaaluminate solution with the concentration of 0.6mol/L, an ammonia water solution with the concentration of 3mol/L and a potassium hydroxide solution with the concentration of 3mol/L into the reaction kettle at a certain feeding speed for continuous reaction, maintaining the pH value of the reaction to be 10.6-11.0, the ammonia concentration to be 8-10g/L, the stirring speed to be 150-180r/min, the flow rate of the nickel sulfate to be 10L/h, the flow rate of the ammonia water to be 10L/h, the flow rate of the liquid alkali to be 6L/h, the flow rate of the sodium metaaluminate solution to be 10L/h, and stopping the reaction when the reaction kettle is 6 h. To obtain a Ni 0.65 Fe 0.16 Mn 0.16 Al 0.03 (OH) 2 The nickel-aluminum oxide composite material comprises an iron-based precursor, wherein a layer of nickel-aluminum hydroxide is coated on an iron-based precursor shell.
Step 4, uniformly mixing the iron-based precursor with the shell coated with a layer of nickel-aluminum hydroxide and sodium carbonate in a mortar, and calcining at 950 ℃ for 20 hours to obtain the nickel-aluminum-coated iron-based sodium-ion battery anode material Na (Ni) 0.65 Fe 0.16 Mn 0.16 Al 0.03 )O 2 . Obtaining the positive electrode material Na (Ni) of the iron-based sodium-ion battery coated with nickel aluminum outside 0.65 Fe 0.16 Mn 0.16 Al 0.03 )O 2 . The prepared sodium ion battery cathode material is assembled into a button battery, and the capacity retention rate of the button battery after 100 cycles under the current density of 120mA/g is 94%.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A preparation method of a nickel-aluminum coated nickel-iron-manganese-sodium ion precursor material is characterized by comprising the following steps:
(1) Soluble nickel salt, soluble iron salt and soluble manganese salt are mixed according to the molar ratio of x 1 :y 1 :1-x 1 -y 1 Preparing a nickel-iron-manganese metal salt solution A with the total metal ion concentration of 2-5mol/L according to the proportion that x is more than or equal to 0.2 1 ≤0.6,0.1≤y 1 Less than or equal to 0.5; preparing ammonia water complexing agent solution with the concentration of 1-3 mol/L; preparation of OH - 1-3mol/L aqueous alkali; the soluble ferric salt is ferrous sulfate or ferrous chloride;
(2) Adding the solution A prepared in the step (1), an ammonia water complexing agent solution and an alkali solution into a reaction kettle at a certain feeding speed, reacting for 50-80h at 40-70 ℃, controlling the pH of the reaction system to be 8.5-11 and the ammonia concentration to be 3.0-8.0g/L, and obtaining Ni x1 Fe y1 Mn 1-x1-y1 (OH) 2 A precursor;
(3) Preparing a soluble nickel salt solution with the nickel ion concentration of 0.5-1.5 mol/L; preparing a sodium metaaluminate solution with the aluminum ion concentration of 0.3-0.6 mol/L; preparing ammonia water solution with the concentration of 1-3 mol/L; preparing an alkali solution with the OH < - > concentration of 1-3 mol/L; adding the solution into the reaction kettle in the step (2) at a certain feeding speed, maintaining the pH of the reaction to be 10-12 and the ammonia concentration to be 5.0-10.0g/L, and stopping the reaction for 2-8h to obtain Ni with the outer layer coated with the nickel-aluminum hydroxide x2 Fe y2 Mn z2 Al 1-x2-y2-z2 (OH) 2 X is more than or equal to 0.3 of iron-based precursor 2 ≤0.7,0.1≤y 2 ≤0.5,0.05≤z 2 ≤0.5;
(4) And uniformly mixing the nickel-iron-manganese precursor coated with nickel-aluminum on the outer layer with sodium carbonate in a mortar, and calcining at 800-950 ℃ for 10-20h to obtain the nickel-iron-manganese sodium ion precursor material coated with nickel-aluminum on the outer layer.
2. The method for preparing the nickel-aluminum coated nickel-iron-manganese-sodium ion precursor material according to claim 1, wherein the soluble nickel salt in the steps (1) and (3) is nickel sulfate, nickel chloride or nickel nitrate.
3. The method for preparing the nickel-aluminum coated nickel-iron-manganese-sodium ion precursor material according to claim 1, wherein the soluble manganese salt in the step (1) is manganese sulfate, manganese chloride or manganese nitrate.
4. The method for preparing the nickel-aluminum coated nickel-iron-manganese-sodium ion precursor material according to claim 1, wherein the alkali solution is a sodium hydroxide solution, a sodium carbonate solution or a potassium hydroxide solution.
5. The method for preparing the nickel-aluminum coated nickel-iron-manganese-sodium ion precursor material according to claim 1, wherein the flow rate of the solution A in the step (2) is 30-50L/h, the flow rate of the ammonia water solution is 3-6L/h, the flow rate of the liquid alkali is 8-15L/h, and the stirring speed is 250-500r/min.
6. The method for preparing the nickel-aluminum coated nickel-iron-manganese-sodium ion precursor material according to claim 1, wherein the flow rate of the soluble nickel salt solution in the step (3) is 10L/h, the flow rate of the ammonia water solution is 4-10L/h, the flow rate of the alkali solution is 2-6L/h, the flow rate of the sodium metaaluminate solution is 5-10L/h, and the stirring speed is 150-280r/min.
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