CN115043442B - Aluminum-doped lanthanum nickel lithium oxide-coated positive electrode material, precursor and preparation method thereof - Google Patents

Aluminum-doped lanthanum nickel lithium oxide-coated positive electrode material, precursor and preparation method thereof Download PDF

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CN115043442B
CN115043442B CN202210900439.4A CN202210900439A CN115043442B CN 115043442 B CN115043442 B CN 115043442B CN 202210900439 A CN202210900439 A CN 202210900439A CN 115043442 B CN115043442 B CN 115043442B
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precursor
positive electrode
matrix
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lanthanum
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CN115043442A (en
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吴飞翔
周金伟
褚宇航
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Central South University
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    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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    • H01M4/00—Electrodes
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    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
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    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention belongs to the technical field of lithium ion battery materials, and discloses Al doping and La doping 4 NiLiO 8 Coated positive electrode material, precursor and preparation method thereof. The invention regulates and controls the surface state of the precursor of the positive electrode material through the surfactantMaking La 3+ And AlO 2 ‑ In situ reaction occurs on the surface to produce La (OH) 3 And Al (OH) 3 Precipitation to obtain a uniform coating of La (OH) 3 And Al (OH) 3 Is a positive electrode material precursor. Then matching with a lithium source for sintering to obtain Al doped and La 4 NiLiO 8 Coated nickel-based multi-component positive electrode material. The invention has simple process flow and low cost, and is suitable for large-scale industrial production.

Description

Aluminum-doped lanthanum nickel lithium oxide-coated positive electrode material, precursor and preparation method thereof
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a lithium ion battery anode material and a preparation method thereof.
Background
The excessive use of non-renewable fossil fuels and the environmental problems that they present have led to the recognition of the importance of renewable clean energy sources. Lithium ion batteries are a clean energy storage system, and are particularly important in the current age of popular clean energy sources. The positive electrode material occupies a half-wall mountain in the whole lithium ion battery element. It can be said that the performance of the cathode material directly determines the performance of the entire battery system. Among them, nickel-based positive electrode materials having high specific capacity and low cost are used as the most explosive materials, but they also face a number of problems. Such as cation mixing, interfacial side reaction, structural collapse, crack generation, etc. Doping and cladding are the two most commonly used means for solving a series of problems faced by nickel-based cathode materials, but the existing doping and cladding are all performed in a single step, and the process is long and complex. Therefore, it is important to dope and coat the nickel-based multi-element positive electrode material in a short process by a simple method.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide an Al doping and La 4 NiLiO 8 The coated positive electrode material, the precursor and the preparation method thereof improve the interface stability of the positive electrode material, reduce the occurrence of side reaction, stabilize the material structure, finally improve the electrochemical performance of the battery and prolong the service life of the battery by simultaneously realizing the doping and coating of the nickel-based multi-element positive electrode material.
In order to achieve the above object, the present invention provides the following specific technical solutions.
First, the present invention provides a precursor of a positive electrode materialA body comprising Ni x M 1-x (OH) 2 A matrix, and lanthanum and aluminum hydroxides uniformly coated on the surface of the matrix; wherein x is more than or equal to 0.30 and less than or equal to 1, and M is one or more than two of Co, mn, al, mg, ti, fe, V, B, W.
Secondly, the invention provides a preparation method of the precursor of the positive electrode material, which comprises the following steps:
step S1, ni is added x M 1-x (OH) 2 Adding the matrix and the anionic surfactant into water to form a suspension;
step S2, adding lanthanum salt into the suspension in the step S1, stirring for a period of time, adding aluminate solution, and aging to obtain slurry;
and S3, carrying out solid-liquid separation, washing and drying on the solid phase of the slurry obtained in the step S2 to obtain a precursor.
Based on the same inventive concept, the present invention provides another preparation method of the precursor material of the positive electrode material, including the following steps:
step S1, ni is added x M 1-x (OH) 2 Adding the matrix and the cationic surfactant into water to form a suspension;
step S2, aluminate is added into the suspension in the step S1, after stirring for a period of time, lanthanum salt solution is added, and after the reaction is finished, the slurry is obtained after aging for a period of time;
and S3, carrying out solid-liquid separation, washing and drying on the solid phase of the slurry obtained in the step S2 to obtain a precursor.
Further, in a part of the preferred embodiments of the above preparation method, the anionic surfactant is selected from one or more of PVP, polyacrylamide, fatty acid salt and sulfonate.
Preferably, the anionic surfactant is added in an amount of Ni x M 1-x (OH) 2 1% -5% of the mass of the matrix.
Further, in some preferred embodiments of the above preparation method, the cationic surfactant is one or more selected from amine salt type, quaternary ammonium salt type, heterocyclic type, and salt type cationic surfactants.
Preferably, the cationic surfactant is added in an amount of Ni x M 1-x (OH) 2 1% -5% of the mass of the matrix.
Further, in some preferred embodiments of the above preparation method, the lanthanum salt is one or more of lanthanum nitrate, lanthanum chloride and lanthanum acetate.
Preferably, the lanthanum salt is added in an amount of Ni x M 1-x (OH) 2 The molar amount of the matrix is 0.5% -5%.
Further, in a part of the preferred embodiments of the above preparation method, the aluminate is one or both of potassium aluminate and sodium aluminate.
Preferably, the concentration of the aluminate solution is 0.5-2 mol/L.
Preferably, the aluminate is used in an amount following AlO 2 - And La (La) 3+ The molar ratio of (3) to (5): 1.
preferably, the adding speed of the aluminate solution is 0.03-6 ml/min.
Further, in some preferred embodiments of the above preparation method, the aging time is 1 to 12 hours.
In addition, the invention provides a positive electrode material, which is obtained by mixing and sintering the precursor prepared by the precursor or the preparation method and a lithium source.
Preferably, the oxygen concentration of the sintering atmosphere is 21 to 100%.
Preferably, the sintering process is as follows: presintering for 1-5 hours at 450-500 ℃, and then sintering for 10-20 hours at 650-900 ℃; or sintering at 700-1000 ℃ for 12-25 hours.
The invention regulates and controls the surface state of the precursor of the positive electrode material through the surfactant to lead La to 3+ And AlO 2 - In situ reaction occurs on the surface to produce La (OH) 3 And Al (OH) 3 Precipitation to obtain a uniform coating of La (OH) 3 And Al (OH) 3 Is a positive electrode material precursor. Then matching with a lithium source for sintering to obtain Al doped and La 4 NiLiO 8 Coated nickel-based multi-component positive electrode material. Al is doped at the Ni site, so that cation mixing can be inhibited, and the structural stability of the material is improved. La, la obtained by epitaxial growth of La, li and Ni 4 NiLiO 8 The coating layer can greatly reduce the side reaction of the interface, reduce the dissolution of transition metal and finally improve the electrochemical performance of the anode material. This simultaneous realization of Al doping and La 4 NiLiO 8 The coating method has extremely short flow, is extremely simple and convenient to operate, and can greatly reduce the preparation cost of the anode material. In addition, the doping and coating internal and external modification strategy ensures that the nickel-based multi-element positive electrode material shows excellent electrochemical performance and longer battery life.
Compared with the prior art, the invention has the following obvious beneficial technical effects:
(1) Simple process flow and low cost, and is suitable for large-scale industrial production.
(2) The existing production line of the factory can be used for producing the precursor and the positive electrode material, and no extra equipment is needed, and excessive changes are not needed to be made to the production line.
(3) The prepared positive electrode material can further improve the energy density of the battery and reduce the cost of the battery.
Drawings
Fig. 1 is a schematic diagram of a process for preparing a precursor and a positive electrode material according to the present invention.
FIG. 2 is an SEM image of a precursor obtained in example 1 of the present invention
Fig. 3 is an SEM image of the positive electrode material prepared in example 1 of the present invention.
Fig. 4 is an XRD pattern of the positive electrode material prepared in example 1 of the present invention.
Fig. 5 is an electrochemical performance chart of a battery including the positive electrode material prepared in example 1 of the present invention.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
As shown in FIG. 1, in the process of preparing the precursor, a surfactant is used to regulate the surface state of the precursor of the positive electrode material, so that La 3+ And AlO 2 - In situ reaction occurs on the surface to produce La (OH) 3 And Al (OH) 3 Precipitation to obtain a uniform coating of La (OH) 3 And Al (OH) 3 Is a positive electrode material precursor. Then matching with a lithium source for sintering to obtain Al doped and La 4 NiLiO 8 Coated nickel-based multi-component positive electrode material.
Example 1
The embodiment comprises the following steps:
s1: 10g of spherical Ni (OH) 2 Adding the precursor and 0.3g of PVP anionic surfactant into 50ml of deionized water, and stirring for 1h to form a suspension;
s2: adding 0.3871g of lanthanum nitrate hydrate into the suspension of the step S1, and continuously stirring for 1h to obtain a feed liquid;
s3: adding 20ml of sodium aluminate solution (with the concentration of 1 mol/L) into the feed liquid in the step S2 at the flow rate of 0.5ml/min, and continuing to age for 4 hours after the addition is finished to obtain a composite precursor;
s4: washing the composite precursor for many times by deionized water, and after suction filtration, placing the composite precursor into a vacuum oven for drying at 150 ℃ for 10 hours;
s5: mixing the dried composite precursor with lithium source LiOH.H according to the ratio of the sum of Ni and Al element substances to Li element substance being 1:1.03 2 O is uniformly mixed, and is presintered for 4 hours at 500 ℃ under the environment of high-purity oxygen, and then 7Sintering at 00 ℃ for 15 hours to obtain the Al doping and La 4 NiLiO 8 Coated nickel-based multi-component positive electrode material.
FIG. 2 is an SEM image of the precursor obtained in step S4, from which it can be seen that Ni (OH) is spherical 2 The surface contains Al (OH) with uniform coating 3 And La (OH) 3 。
Fig. 3 is an SEM image of the positive electrode material obtained in step S5, and it can be seen from the image that the positive electrode material is composed of secondary spheres of 2 to 20 micrometers, and the surface of the spheres is composed of primary spheres of approximately 300 nanometers.
Fig. 4 is an XRD pattern of the cathode material synthesized in example 1. It can be seen that the peak of the cathode material is opposite to that of standard LiNiO due to the doping of Al 2 The peaks of (a) are shifted to a small angle as a whole. Furthermore, between 20-35 degrees, la was observed 4 NiLiO 8 Is shown to successfully coat a layer of La on the surface of the material 4 NiLiO 8 . It can also be confirmed that the method provided by the invention can realize Al doping and La simultaneously 4 NiLiO 8 Is coated with a coating of (a).
Al doping and La synthesized in example 1 4 NiLiO 8 The coated positive electrode material is matched with conductive agent acetylene black and binder polyvinylidene fluoride (PVDF) to prepare a positive electrode plate, and then matched with a lithium metal negative electrode to carry out half-cell assembly, and the electrochemical performance of the battery is tested.
At the same time, commercially available LiNiO 2 And preparing a positive pole piece by matching conductive agent acetylene black and binder polyvinylidene fluoride (PVDF), and then performing half-cell assembly by matching a lithium metal negative pole, and testing the electrochemical performance of the positive pole piece.
Fig. 5 is a charge-discharge cycle chart of the above two types of half batteries. As can be seen from FIG. 5, the mixture is circulated for 100 circles under the condition that the cut-off voltage is 2.8-4.3V under the charge and discharge of 1C multiplying power, and comprises the Al doping and La synthesized in the embodiment 1 4 NiLiO 8 The half-cell discharge specific capacity of the coated positive electrode material is maintained above 146.3 mAh/g, and the half-cell discharge specific capacity comprises commercially available LiNiO 2 The capacity after 30 cycles of half cell cycle was only 94.5 mAh/g, indicating the Al doping and La in example 1 4 NiLiO 8 The coated nickel-based multi-component positive electrode material exhibits excellent propertiesElectrochemical performance and potential as a next-generation lithium battery anode material.
Example 2
The embodiment comprises the following steps:
s1: taking 5g of spherical Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Adding the ternary precursor and 0.3g of polyacrylamide anionic surfactant into 30ml of deionized water, and stirring for 1h to form a suspension;
s2: adding 0.2513g of lanthanum chloride hydrate into the suspension in the step S1, and continuously stirring for 1h to obtain a feed liquid;
s3: adding 15ml of potassium aluminate solution (with the concentration of 0.8 mol/L) into the feed liquid in the step S2 at the flow rate of 0.1ml/min, and continuing to age for 3 hours after the addition is finished to obtain a composite precursor;
s4: washing the composite precursor for multiple times by deionized water, and drying the composite precursor in a vacuum oven at 80 ℃ for 15 hours after suction filtration;
s5: mixing the dried composite precursor with lithium source LiOH H according to the ratio of the sum of Ni, co, mn, al element substances to Li element substances of 1:1.03 2 O is uniformly mixed, and is presintered for 5 hours at 480 ℃ and then sintered for 12 hours at 720 ℃ in the environment of high-purity oxygen to obtain the Al doping and La 4 NiLiO 8 Coated nickel-based multi-component positive electrode material.
Example 3
The embodiment comprises the following steps:
s1: taking 25g of spherical Ni 0.9 Co 0.1 (OH) 2 Adding the precursor and 1g of octadecyl dimethyl benzyl ammonium chloride cationic surfactant into 100ml of deionized water, and stirring for 1h to form a suspension;
s2: 0.5142g of sodium aluminate hydrate is added into the suspension in the step S1, and stirring is continued for 1h;
s3: adding 50ml of lanthanum nitrate solution (with the concentration of 1.5 mol/L) into the feed liquid in the step S2 at the flow rate of 0.3ml/min, and continuing to age for 5 hours after the addition is finished to obtain a composite precursor;
s4: washing the composite precursor for many times by deionized water, and after suction filtration, placing the composite precursor into a vacuum oven for drying at the drying temperature of 100 ℃ for 10 hours;
s5: mixing the dried composite precursor with lithium source LiOH.H according to the ratio of the sum of Ni, co and Al element substances to Li element substance being 1:1.05 2 O is uniformly mixed, and is presintered for 6 hours at 480 ℃ and then sintered for 15 hours at 700 ℃ in the environment of high-purity oxygen to obtain the Al doping and La 4 NiLiO 8 Coated nickel-based multi-component positive electrode material.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (6)

1. A method for preparing a precursor of a positive electrode material, wherein the precursor comprises Ni x M 1-x (OH) 2 A matrix, and lanthanum and aluminum hydroxides uniformly coated on the surface of the matrix; wherein x is more than or equal to 0.30 and less than or equal to 1, and M is one or more than two of Co, mn, al, mg, ti, fe, V, B, W;
the preparation method is characterized by comprising the following steps of:
step S1, ni is added x M 1-x (OH) 2 Adding the matrix and the anionic surfactant into water to form a suspension;
step S2, adding lanthanum salt into the suspension in the step S1, stirring for a period of time, adding aluminate solution, and aging for a period of time after the reaction is finished to obtain slurry;
and S3, carrying out solid-liquid separation, washing and drying on the solid phase of the slurry obtained in the step S2 to obtain a precursor.
2. A method for preparing a precursor material of a positive electrode material, wherein the precursor comprises Ni x M 1-x (OH) 2 A matrix, and lanthanum and aluminum hydroxides uniformly coated on the surface of the matrix; wherein, the content of the active ingredients is less than or equal to 0.30 percentx is less than or equal to 1, and M is one or more than two of Co, mn, al, mg, ti, fe, V, B, W;
the preparation method is characterized by comprising the following steps of:
step S1, ni is added x M 1-x (OH) 2 Adding the matrix and the cationic surfactant into water to form a suspension;
step S2, aluminate is added into the suspension in the step S1, after stirring for a period of time, lanthanum salt solution is added, and after the reaction is finished, the slurry is obtained after aging for a period of time;
and S3, carrying out solid-liquid separation, washing and drying on the solid phase of the slurry obtained in the step S2 to obtain a precursor.
3. The method according to claim 1, wherein the anionic surfactant is one or more selected from PVP, polyacrylamide, fatty acid salt and sulfonate; the addition amount of the anionic surfactant is Ni x M 1-x (OH) 2 1% -5% of the mass of the matrix.
4. The preparation method of claim 2, wherein the cationic surfactant is one or more than two selected from amine salt type, quaternary ammonium salt type, heterocyclic type and salt type cationic surfactants; the addition amount of the cationic surfactant is Ni x M 1-x (OH) 2 1% -5% of the mass of the matrix.
5. The preparation method according to claim 1 or 2, wherein the lanthanum salt is one or more of lanthanum nitrate, lanthanum chloride and lanthanum acetate; the addition amount of the lanthanum salt is Ni x M 1-x (OH) 2 The molar amount of the matrix is 0.5% -5%.
6. The preparation method according to claim 1 or 2, wherein the aluminate is one or both of potassium aluminate and sodium aluminate; the concentration of the aluminate solution is 0.5-2 mol/L; the aluminate is used in an amount following AlO 2 - And La (La) 3+ The molar ratio of (3) to (5): 1, a step of; the adding speed of the aluminate solution is 0.03-6 ml/min.
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