CN114940518B - Surface layer and bulk phase silicon doping-based ternary cathode material and preparation method thereof - Google Patents

Surface layer and bulk phase silicon doping-based ternary cathode material and preparation method thereof Download PDF

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CN114940518B
CN114940518B CN202210668896.5A CN202210668896A CN114940518B CN 114940518 B CN114940518 B CN 114940518B CN 202210668896 A CN202210668896 A CN 202210668896A CN 114940518 B CN114940518 B CN 114940518B
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cathode material
mixing
ternary cathode
nickel
silicon
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CN114940518A (en
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周成冈
孙睿敏
饶文锦
韩波
夏开胜
高强
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China University of Geosciences
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    • C01G53/00—Compounds of nickel
    • C01G53/40—Nickelates
    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
    • C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
    • H—ELECTRICITY
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    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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
    • H01M4/50—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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • 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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    • 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 discloses a preparation method of a ternary cathode material based on surface layer and bulk silicon doping, which comprises the following steps: dissolving a silicon source in a solvent, dissolving nickel-cobalt-manganese hydroxide powder in the solvent, uniformly stirring, evaporating the solvent to dryness, and drying in vacuum to obtain a precursor; pouring the precursor and lithium hydroxide into a high-speed mixer for mixing, and calcining after mixing to obtain a silicon-doped ternary cathode material; the invention also discloses a ternary cathode material based on surface layer and bulk silicon doping. In the invention, nickel-cobalt-manganese hydroxide powder and a silicon source are subjected to liquid phase mixing, and silicon is doped into a bulk phase lattice by high-temperature calcination to form SiO 4 4– The form of the structure occupies tetrahedral sites, and the stronger Si-O bond can stabilize lattice oxygen in a bulk phase, maintain the layered structure of the material and improve the cycle stability; at the same time, siO 4 4– The lithium ion battery has larger thermochemical radius, can widen a lithium ion transmission channel, improves the multiplying power performance of a material, and reduces the cost.

Description

Surface layer and bulk phase silicon doping-based ternary cathode material and preparation method thereof
Technical Field
The invention relates to the technical field of lithium ion battery materials. More specifically, the invention relates to a ternary cathode material based on surface layer and bulk silicon doping and a preparation method thereof.
Background
The layered nickel-cobalt-manganese (NCM) ternary cathode material has a stable structure, excellent cycle performance and high capacity, is an excellent lithium ion battery cathode material, and is widely applied to the fields of electric automobiles and the like. In recent years, with the increasing demand of lithium ion batteries, the price of cobalt rises dramatically, resulting in the increasing cost of lithium ion batteries. Therefore, it is imperative to develop high nickel, low cobalt, cobalt-free materials.
In the high-nickel low-cobalt ternary cathode material, the cycle performance and the rate capability of the material are reduced and the thermal stability is reduced due to the reduction of the cobalt content and the increase of the nickel content. The common modification method of the ternary cathode material comprises doping and coating, and can effectively reduce the mixed discharge of lithium and nickel by doping, maintain the layered structure of the material in the charging and discharging process and widen a lithium ion transmission channel; meanwhile, the formation of microcracks of the material can be effectively improved, and the decomposition of the electrolyte is reduced. By coating the excellent ionic and electronic conductor material, the structural stability of the ternary cathode material can be effectively improved, the ionic and electronic conductivity of the material can be improved, and the cycle performance and the rate capability of the material can be further improved. In addition, the cladding can prevent the side reaction of the bulk phase material and the electrolyte, and further improve the cycle performance and the rate capability of the material.
Most of the existing doping methods are to mix a precursor and a nano-scale metal oxide in a solid phase and then to enable doping elements to enter the interior of a ternary anode material crystal lattice through high-temperature sintering. However, the cost of the nano material is high, and the solid-phase mixing material cannot realize the uniform mixing of the host material and the doping material on the micrometer scale, so that the doping effect is poor.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
The invention also aims to provide a preparation method of the ternary cathode material based on surface layer and bulk silicon doping, wherein the nickel-cobalt-manganese hydroxide powder and a silicon source are subjected to liquid phase mixing, and silicon is doped into bulk crystal lattices through high-temperature calcination, so that SiO is used 4 4– The form of the structure occupies tetrahedral sites, and the stronger Si-O bond can stabilize lattice oxygen in a bulk phase, maintain the layered structure of the material and improve the cycle stability; at the same time, siO 4 4– The lithium ion battery has larger thermochemical radius, can widen a lithium ion transmission channel, improves the multiplying power performance of the material and reduces the cost.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a ternary cathode material based on surface and bulk silicon doping, comprising the steps of: dissolving a silicon source in a solvent, dissolving nickel-cobalt-manganese hydroxide powder in the solvent, uniformly stirring, evaporating the solvent to dryness, and drying in vacuum to obtain a precursor;
and pouring the precursor and lithium hydroxide into a high-speed mixer for mixing, and calcining after mixing to obtain the silicon-doped ternary cathode material. Specifically, the mole fractions of the silicon source and the nickel-cobalt-manganese hydroxide are 0.2-1.2% and 98.8-99.8%, respectively.
Specifically, the molar ratio of Ni, co and Mn in the nickel-cobalt-manganese hydroxide is 90:6:4.
specifically, the silicon source is one or more of tetraethyl silicate, tetrabutyl silicate and trimethylsilyl methane sulfonate.
Specifically, the molar ratio of the nickel cobalt manganese hydroxide to the lithium hydroxide is 1:1 to 1.2.
Specifically, the mixing is performed in a high speed mixer at a low speed of 200r/min for 5min, and then at a high speed of 900r/min for 15min.
Specifically, the calcination includes two stages of pre-sintering and sintering.
Specifically, the pre-sintering stage is sintered for 4 to 8 hours at 400 to 600 ℃, and the sintering stage is calcined for 8 to 15 hours at 650 to 850 ℃.
Specifically, the temperature rise rates of the pre-sintering stage and the sintering stage are respectively 5-7 ℃/min and 1-2 ℃/min.
The invention also provides a ternary cathode material based on surface layer and bulk silicon doping, and the ternary cathode material is prepared by the preparation method.
In the invention, nickel-cobalt-manganese hydroxide powder and a silicon source are mixed in a liquid phase, and silicon is doped into a bulk phase lattice by high-temperature calcination, and SiO is used 4 4– The form of the structure occupies tetrahedral sites, and the stronger Si-O bond can stabilize lattice oxygen in a bulk phase, maintain the layered structure of the material and improve the cycle stability; at the same time, siO 4 4– The material has a larger thermochemical radius, can widen a lithium ion transmission channel and improve the rate capability of the material;
the Si doping in the anode material can stabilize the material structure, stabilize the lattice oxygen in the charging and discharging process and inhibit the oxygen evolution reaction. Meanwhile, the Si doping can also inhibit the violent lattice contraction caused by the H2-H3 phase change reaction of the material in the charging and discharging processes, and inhibit the pulverization of the material in the charging and discharging processes, so that the cycle performance of the material is greatly improved.
According to the method, the ternary nickel-cobalt-manganese hydroxide precursor is subjected to surface wet treatment and then mixed and sintered with lithium salt, so that the material is modified, and uniform mixing of Si and the precursor on a micrometer scale is facilitated, so that the surface layer and the bulk phase of the NCM ternary cathode material are doped, and the material performance is improved.
The NCM ternary cathode material is applied as a high-capacity and long-service-life lithium ion battery cathode material.
The invention at least comprises the following beneficial effects:
the initial discharge specific capacity of the NCM anode material at 0.1C is 216.4mAh g –1 And the specific discharge capacity after 100 cycles of circulation under 1C is 102.3mAh g –1 The capacity retention ratio was 51.7%. When the doping molar weight of Si accounts for 0.2-1.2%, the specific discharge capacity of the first ring of the obtained positive electrode material under 0.1C is 220mAh g –1 Above, after 100 cycles under 1C, the specific discharge capacity is 190mAh g –1 The capacity retention ratio is 90% or more. The cycle performance of the cathode material is obviously improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) picture of a Si-doped high-nickel ternary material in example 1 of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) picture of a Si-doped high-nickel ternary material in example 2 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) picture of a Si-doped high-nickel ternary material in comparative example 1 of the present invention;
FIG. 4 is a Scanning Electron Microscope (SEM) picture of a Si-doped high-nickel ternary material of comparative example 2 of the present invention;
FIG. 5 is an X-ray diffraction pattern of a Si-doped high nickel ternary material of examples 1-2 of the present invention and a high nickel ternary material of comparative examples 1-2;
FIG. 6 is an electrochemical specific capacity curve of Si-doped high nickel ternary material in example 1 of the present invention;
FIG. 7 is an electrochemical specific capacity curve of Si-doped high nickel ternary material in example 2 of the present invention;
FIG. 8 is an electrochemical specific capacity curve of the Si-doped high-nickel ternary material of comparative example 1 in accordance with the present invention;
FIG. 9 is an electrochemical specific capacity curve of a high nickel ternary material of comparative example 2 of the present invention.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.
< example 1>
A precursor of an NCM ternary cathode material is nickel-cobalt-manganese hydroxide, wherein the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese hydroxide is 90 0.90 Co 0.06 Mn 0.04 (OH) 2 The diameter of the nickel-cobalt-manganese hydroxide is 5-10 mu m.
The preparation method of the Si-doped NCM ternary cathode material comprises the following steps:
(1) 5.722g of tetrabutyl silicate is dissolved in 150mL of ethanol to prepare a solution A, 202g of nickel-cobalt-manganese hydroxide is dissolved in the solution A, the mixture is stirred and dispersed for 0.5h, and then the solvent is evaporated at 80 ℃ to obtain a precursor.
(2) And pouring the precursor and 94.18g of lithium hydroxide into a high-speed mixer, mixing at the speed of 300r/min for 20min, then mixing at the speed of 600r/min for 20min, and finally mixing at the speed of 300r/min for 10min to obtain the uniformly mixed material.
(3) Putting the uniformly mixed material into a box furnace, firstly presintering for 6h at 500 ℃, then calcining for 12h at 740 ℃, wherein the heating rates in the presintering and sintering stages are respectively 5 ℃/min and 1 ℃/min, and obtaining the silicon-doped ternary cathode material after sintering; the scanning electron micrograph is shown in FIG. 1, and the X-ray diffraction pattern is shown in FIG. 5.
(4) As active material (prepared positive electrode material): conductive agent (Super P): the mass ratio of the binder (PVDF) is 8 6 The constant current charge and discharge test was performed on an electrolyte assembly battery with EC: EMC: DMC = 1.
The finished Si-doped NCM ternary cathode material is assembled into a battery, the electrochemical performance of the battery is tested, the result is shown in figure 6, and the specific discharge capacity of the first circle at 0.1 ℃ is 229.9mAh g –1 And the specific discharge capacity of the first ring under 1C is 210.8mAh g –1 And the specific discharge capacity after 100 cycles is 197.6mAh g –1 The capacity retention rate was 93.8%.
< example 2>
A precursor of an NCM ternary cathode material is nickel-cobalt-manganese hydroxide, wherein the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese hydroxide is 90 0.90 Co 0.06 Mn 0.04 (OH) 2 The diameter of the nickel-cobalt-manganese hydroxide is 5-10 mu m.
The preparation method of the Si-doped NCM ternary cathode material comprises the following steps:
(1) Dissolving 3.713g tetraethyl silicate in 150mL ethanol to prepare solution A, dissolving 202g ternary nickel-cobalt-manganese hydroxide in the solution A, stirring and dispersing for 0.5h, and evaporating the solvent at 80 ℃ to obtain a precursor;
(2) And pouring the precursor and 94.18g of lithium hydroxide into a high-speed mixer, mixing at the speed of 300r/min for 20min, then mixing at the speed of 600r/min for 20min, and finally mixing at the speed of 300r/min for 10min to obtain the uniformly mixed material.
(3) Putting the uniformly mixed material into a box furnace, firstly presintering for 7h at 450 ℃, then calcining for 14h at 700 ℃, wherein the heating rates in the presintering stage and the sintering stage are respectively 5 ℃/min and 2 ℃/min, and obtaining the Si-doped ternary cathode material after sintering; the scanning electron micrograph is shown in FIG. 2, and the X-ray diffraction micrograph is shown in FIG. 5.
(4) Uniformly mixing an active material (prepared positive electrode material), a conductive agent (Super P), a binder (PVDF) according to the mass ratio of 8 6 The constant current charge and discharge test was performed on an electrolyte assembly battery with EC: EMC: DMC = 1.
The finished Si-doped NCM ternary cathode material is assembled into a battery, the electrochemical performance of the battery is tested, the result is shown in figure 7, and the specific discharge capacity of the first ring at 0.1 ℃ is 226.4mAh g –1 And the specific discharge capacity of the first ring under 1C is 209.6mAh g –1 The discharge specific capacity after 100 cycles is 190.9mAh g –1 The capacity retention ratio was 91.1%.
< comparative example 1>
The procedure and experimental operation were the same as in example 1, compared with example 1, except that tetraethyl silicate was not added in comparative example 1, and the scanning electron micrograph thereof is shown in fig. 3, and the X-ray diffraction pattern thereof is shown in fig. 5.
The finished NCM ternary cathode material is assembled into a battery, the electrochemical performance of the battery is tested, the result is shown in figure 8, and the specific discharge capacity of the first ring at 0.1 ℃ is 216.4mAh g –1 And the first-coil discharge specific capacity under 1C is 197.8mAh g –1 And the specific discharge capacity after 100 cycles is 102.3mAh g –1 The capacity retention rate was 51.7%. The silicon is doped into the NCM ternary cathode material, so that the electrochemical performance of the NCM ternary cathode material is improved.
< comparative example 2>
The procedure and experimental procedure were as in example 1, except that in comparative example 1, 11.139g of tetraethyl silicate was added, as shown in Scanning Electron Micrograph (SEM) of FIG. 4 and as shown in X-ray diffraction pattern of FIG. 5.
The finished Si-doped NCM ternary cathode material is assembled into a battery, the electrochemical performance of the battery is tested, the result is shown in figure 9, and the specific discharge capacity of the first circle at 0.1 ℃ is 186.9mAh g –1 And the first-coil discharge specific capacity under 1C is 174.1mAh g –1 And the specific discharge capacity after 100 cycles is 137.4mAh g –1 The capacity retention rate was 78.9%. It indicates that too much doping of silicon also results in degradation of electrical properties.
While embodiments of the invention have been described above, it is not intended to be limited to the details shown, particular embodiments, but rather to those skilled in the art, and it is to be understood that the invention is capable of numerous modifications and that various changes may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.

Claims (2)

1. A preparation method of a ternary cathode material based on surface layer and bulk silicon doping is characterized by comprising the following steps: dissolving a silicon source in a solvent ethanol, and then dissolving nickel-cobalt-manganese hydroxide Ni 0.90 Co 0.06 Mn 0.04 (OH) 2 Dissolving the powder in the solvent, uniformly stirring, evaporating the solvent, and drying in vacuum to obtain a precursor;
pouring the precursor and lithium hydroxide into a high-speed mixer for mixing, and calcining after mixing to obtain a silicon-doped ternary cathode material; mixing for 20min at a low speed of 300r/min in a high speed mixer, mixing for 15 to 20min at a high speed of 600r/min, and finally mixing for 10min at a speed of 300 r/min; the calcination comprises two stages of presintering and sintering, wherein the presintering stage is used for sintering for 4 to 8 hours at 400 to 600 ℃, the sintering stage is used for calcining for 8 to 15 hours at 650 to 850 ℃, and the temperature rise rates of the presintering and the sintering stage are 5~7 ℃/min and 1~2 ℃/min respectively;
the mole fractions of the silicon source and the nickel-cobalt-manganese hydroxide are respectively 0.2 to 1.2 percent and 98.8 to 99.8 percent; the silicon source is one or more of tetraethyl silicate, tetrabutyl silicate and trimethylsilyl methane sulfonate;
the molar ratio of the nickel cobalt manganese hydroxide to the lithium hydroxide is 1:1 to 1.2.
2. A ternary cathode material based on surface layer and bulk silicon doping, which is characterized by being prepared by the preparation method of claim 1.
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