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CN114709413B - Ternary material and application thereof - Google Patents

Ternary material and application thereof Download PDF

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Publication number
CN114709413B
CN114709413B CN202210394676.8A CN202210394676A CN114709413B CN 114709413 B CN114709413 B CN 114709413B CN 202210394676 A CN202210394676 A CN 202210394676A CN 114709413 B CN114709413 B CN 114709413B
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ternary material
diffraction peak
ratio
ternary
electrochemical device
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CN114709413A (en
Inventor
杨元婴
朱呈岭
莫方杰
闫永思
杨文龙
孙化雨
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Envision Power Technology Jiangsu Co Ltd
Envision Ruitai Power Technology Shanghai Co Ltd
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Envision Power Technology Jiangsu Co Ltd
Envision Ruitai Power Technology Shanghai Co Ltd
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Complex oxides containing nickel and at least one other metal element
    • C01G53/42—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2
    • C01G53/44—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese
    • C01G53/50—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a ternary material and application thereof, wherein in an XRD result of a pole piece test, the intensity ratio of 003 diffraction peak to 104 diffraction peak is 0.8-1.0. In the ternary material, the ratio of 003 diffraction peak intensity to 104 diffraction peak intensity is in the range, so that the ternary material can exert optimal electrochemical performance, and the ternary material is not influenced by the reduction of nickel and cobalt content.

Description

Ternary material and application thereof
Technical Field
The invention belongs to the technical field of batteries, and relates to a ternary material, in particular to a ternary material and application thereof.
Background
The Ni-Co-Mn ternary layered material LiNi xCoyMn1-x-yO2 is the first choice of a power battery system with high energy density. At present, commercial ternary material batteries generally have higher Co content (y is more than or equal to 0.15) and high nickel content (x is more than or equal to 0.8). The cost can be saved and the resource can be protected by reducing the cobalt content because the Co is expensive and the Co ore is scarce; secondly, the high nickel material has poor safety and low charging voltage, the utilization rate of reversible lithium is insufficient, and the safety and the use voltage of the material can be improved by reducing the nickel content.
However, the decrease of Co content (y is less than or equal to 0.13) in the ternary material can reduce the overall conductivity of the material, and improve the diffusion barrier of lithium ions in the crystal lattice, so that serious dynamic performance deterioration is brought; the decrease in Ni content results in a decrease in the reversible specific capacity of the material.
Based on the above research, it is necessary to provide a ternary material, and on the premise of considering low cost, the lithiation degree, the surface free lithium content, the crystallinity and the lithium nickel mixed arrangement of the ternary material reach balance, so that the optimal electrochemical performance of the ternary material can be exerted.
Disclosure of Invention
The invention aims to provide a ternary material and application thereof, in particular to a low-nickel low-cobalt ternary material and application thereof, wherein the ternary material has low nickel and cobalt content, and meanwhile, the electrochemical performance of the ternary material is not influenced by the low nickel and cobalt content, so that the ternary material has good electrochemical performance.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
In a first aspect, the present invention provides a ternary material having an intensity ratio of 003 diffraction peak to 104 diffraction peak of 0.8 to 1.0 in XRD result of pole piece test.
In the ternary material, the ratio of 003 diffraction peak intensity to 104 diffraction peak intensity is in the range, so that the lithiation degree, the surface free lithium content, the crystallinity and the lithium nickel mixed arrangement of the ternary material can be balanced, the low-nickel and low-cobalt ternary material can exert optimal electrochemical performance, and the ternary material is not influenced by the reduction of nickel and cobalt content; meanwhile, the ratio of the diffraction intensity is matched with nickel and cobalt with specific contents, so that the low cost and the high safety performance can be considered.
The intensity ratio of 003 diffraction peak to 104 diffraction peak refers to the integral intensity ratio of the corresponding diffraction peak.
In the XRD result of the ternary material, the intensity ratio of 003 diffraction peak to 104 diffraction peak is 0.8 to 1.0, and may be, for example, 0.8, 0.825, 0.85, 0.875, 0.9, 0.925, 0.95, 0.975 or 1.0, but not limited to the recited values, and other non-recited values in the numerical range are still applicable.
Preferably, the composition of the ternary material comprises LiNi xCoyMn1-x-yO2, wherein x is more than or equal to 0.55 and less than or equal to 0.60,0.10 and y is more than or equal to 0.12.
The composition of the ternary material comprises LiNi xCoyMn1-x-yO2, wherein x is more than or equal to 0.55 and less than or equal to 0.60, such as 0.55, 0.56, 0.57, 0.58, 0.59 or 0.60, but the ternary material is not limited to the listed values, and other non-listed values in the numerical range still apply.
The composition of the ternary material comprises LiNi xCoyMn1-x-yO2, wherein y is more than or equal to 0.10 and less than or equal to 0.12, such as 0.10, 0.105, 0.11, 0.115 or 0.12, but not limited to the recited values, and other non-recited values in the numerical range still apply.
Preferably, the composition of the ternary material further comprises residual lithium ions.
Preferably, the residual lithium ion content is 300ppm to 800ppm, and may be 300ppm, 400ppm, 500ppm, 600ppm, 700ppm or 800ppm, for example, but is not limited to the recited values, and other non-recited values within the range of values are still applicable.
The ternary material also comprises residual lithium ions, and the existence of the residual lithium ions in a reasonable content range can improve the ion conductivity of the low-nickel low-cobalt ternary material and is beneficial to the removal and intercalation of the lithium ions.
Preferably, the ratio of the content of the residual lithium ions to the particle size D 50 of the ternary material is 150ppm/μm to 350ppm/μm, for example 150ppm/μm, 175ppm/μm, 200ppm/μm, 225ppm/μm, 250ppm/μm, 275ppm/μm, 300ppm/μm, 325ppm/μm or 350ppm/μm, but not limited to the values recited, other values not recited in the numerical range are applicable.
According to the invention, the structural stability of the ternary material can be optimized by controlling the content of residual lithium ions and the particle size D 50 of the ternary material.
Preferably, the molar ratio of lithium ions to other metal ions in the preparation raw material of the ternary material is (1.05 to 1.09): 1, for example, may be 1.05:1, 1.06:1, 1.07:1, 1.08:1 or 1.09:1, but is not limited to the recited values, and other non-recited values in the numerical range still apply.
In the preparation raw materials of the ternary material, the content of lithium ions is slightly excessive, so that the residual lithium content of the obtained low-nickel low-cobalt ternary material is within a reasonable range, and the low-nickel low-cobalt ternary material can exert optimal electrochemical performance.
The preparation method of the ternary material comprises the following steps:
and mixing the ternary material precursor and lithium salt according to the formula amount, and sintering to obtain the ternary material.
Preferably, the sintering temperature is 930 ℃ to 980 ℃, for example 930 ℃, 940 ℃, 950 ℃, 960 ℃, 970 ℃, or 980 ℃, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the sintering time is 14h to 22h, for example, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h or 22h, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In a second aspect, the present invention provides an electrochemical device comprising a ternary material as described in the first aspect.
Preferably, the composition of the positive electrode sheet of the electrochemical device includes ternary materials, conductive agents and binders in a mass ratio of (90 to 99): (0.1 to 7): 1, for example, 90:0.1:1, 95:2:1, 97:6:1 or 99:7:1, but not limited to the recited values, and other non-recited values in the numerical range are still applicable.
Preferably, the composition of the negative electrode sheet of the electrochemical device includes (90 to 99): (0.1 to 5): 2 graphite, a conductive agent and a binder, which may be, for example, 90:0.1:2, 95:3:2 or 99:5:2, but is not limited to the recited values, and other non-recited values within the numerical range are applicable.
Preferably, the electrolyte of the electrochemical device includes lithium hexafluorophosphate.
In a third aspect, the present invention provides an electronic device comprising an electrochemical apparatus as described in the second aspect.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the lithium degree, the surface free lithium content, the crystallinity and the lithium nickel mixed arrangement of the ternary material are balanced by controlling the ratio of diffraction peak intensities in the ternary material, so that the ternary material with low nickel and low cobalt can have excellent electrochemical performance, and is not influenced by the reduction of the nickel and cobalt content.
Drawings
Fig. 1 is an XRD pattern of the ternary material described in example 1.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a ternary material, wherein the ternary material comprises LiNi 0.58Co0.11Mn0.31O2 and 399ppm of residual lithium ions; the ratio of the content of the residual lithium ions to the particle size D 50 of the ternary material is 230 ppm/mu m;
XRD results of the ternary material in the pole piece test are shown in figure 1, and the intensity ratio of 003 diffraction peak to 104 diffraction peak is 0.85; wherein, 2 theta corresponding to 003 diffraction peak is 18.618 degrees, half-peak width is 0.149, 2 theta corresponding to 104 diffraction peak is 44.301 degrees, half-peak width is 0.174;
in the preparation raw materials of the ternary material, the molar ratio of lithium ions to other metal ions is 1.07:1;
the preparation method of the ternary material comprises the following steps:
and mixing the ternary material precursor and lithium carbonate according to the formula amount, and sintering for 18 hours at 950 ℃ to obtain the ternary material.
Example 2
The embodiment provides a ternary material, wherein the ternary material comprises LiNi 0.55Co0.12Mn0.33O2 and 300ppm of residual lithium ions; the ratio of the content of the residual lithium ions to the particle size D 50 of the ternary material is 150 ppm/mu m;
in the XRD result of the pole piece test, the ratio of the 003 diffraction peak intensity to the 104 diffraction peak intensity of the ternary material is 0.8;
In the preparation raw materials of the ternary material, the molar ratio of lithium ions to other metal ions is 1.05:1;
the preparation method of the ternary material comprises the following steps:
and mixing the ternary material precursor and LiOH according to the formula amount, and sintering at 930 ℃ for 22 hours to obtain the ternary material.
Example 3
The embodiment provides a ternary material, wherein the ternary material comprises LiNi 0.60Co0.10Mn0.30O2 and 800ppm of residual lithium ions; the ratio of the content of the residual lithium ions to the particle diameter D 50 of the ternary material is 350ppm/μm.
In the XRD result of the pole piece test, the ratio of the 003 diffraction peak intensity to the 104 diffraction peak intensity of the ternary material is 1.0;
In the preparation raw materials of the ternary material, the molar ratio of lithium ions to other metal ions is 1.09:1;
the preparation method of the ternary material comprises the following steps:
and mixing the ternary material precursor and lithium carbonate according to the formula amount, and sintering for 14 hours at 980 ℃ to obtain the ternary material.
The ternary materials provided in examples 4 to 6 are as shown in Table 2, except that the content of residual lithium ions is changed, and the molar ratio of lithium ions to other metal ions in the raw materials for preparation is changed accordingly, the same as that in example 1.
The ternary materials provided in examples 7 to 8 are as shown in table 3, except that the ratio of the content of the residual lithium ions to the particle diameter D 50 of the ternary material is changed, and the particle diameter D 50 of the corresponding ternary material is changed, the same as that of example 1.
The ternary materials provided in comparative example 1 and comparative example 2 are as shown in Table 4, except that the ratio of the intensities of the 003 diffraction peak and the 104 diffraction peak is changed, the same as in example 1.
Performance test:
The ternary materials obtained in the above examples and comparative examples, conductive carbon black, carbon nanotubes and polyvinylidene fluoride are mixed in a mass ratio of 97:1:0.5:1, and the mixture is prepared into slurry in an N-methylpyrrolidone solvent, and then coated on an aluminum foil, dried and rolled to obtain a positive plate; graphite, conductive carbon black, sodium carboxymethylcellulose and styrene-butadiene rubber with the mass ratio of 96:0.5:0.5:2 are coated on copper foil in an N-methylpyrrolidone solvent, and a negative plate is obtained after drying and rolling; and assembling the obtained positive plate, the polyethylene diaphragm and the lithium hexafluorophosphate electrolyte into a lithium ion battery.
The positive plate obtained by disassembling the lithium ion battery is subjected to slow scanning at 2 degrees/min through an X-ray diffractometer (model: bruce D8 Advance), the diffraction peak intensities of 003 and 104 are measured, and the ratio of the available intensities is calculated; the content of residual lithium ions in the ternary material can be measured by a titration method; the chemical formula and the particle size D 50 of the ternary material can be determined through elemental analysis and a scanning electron microscope respectively.
Gram capacity test method: charging and discharging for one week in a charging and discharging mode of 0.063A/g at 25 ℃, wherein the cut-off voltage is 2.8-4.4V, and the obtained charge/discharge capacity is divided by the usage amount of the positive electrode, namely the first charge/discharge gram capacity; the test equipment was Cheng Hong Electrical Co., ltd battery performance test System (equipment model: BTS05/10C 8D-HP).
The cyclic capacity retention test method: the lithium ion battery obtained above circulates in a charge-discharge system of 0.19A/g (calculated by the mass of the anode material) at 25 ℃, and after the circulation is completed for 800 weeks, the discharge capacity of the battery at the moment is divided by the discharge capacity of the battery at the first circle, namely the 800-circle circulation capacity retention rate of the battery; the test equipment was Cheng Hong Electrical Co., ltd battery performance test System (equipment model: BTS05/10C 8D-HP).
The test results are shown in the following table:
TABLE 1
Gram Capacity for first discharge (mAh/g) 800 Cycle capacity retention (%)
Example 1 187 95
Example 2 184 95
Example 3 183 91
TABLE 2
TABLE 3 Table 3
TABLE 4 Table 4
From the above table it can be seen that:
As is apparent from examples 1 to 8 and comparative examples 1 to 2, the ternary material of the present invention has an intensity ratio of 003 diffraction peak to 104 diffraction peak in the range of 0.8 to 1.0, and thus has excellent electrochemical properties; as can be seen from examples 1 and 4 to 8, the electrochemical properties of the ternary materials are affected by the ratio of the content of residual lithium ions in the ternary materials to the particle size D 50 of the materials.
In summary, the invention provides a low-nickel low-cobalt ternary material, which has low nickel and cobalt content, and simultaneously has good electrochemical performance without being influenced by the low nickel and cobalt content.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that fall within the technical scope of the present invention disclosed herein are within the scope of the present invention.

Claims (8)

1. A ternary material, characterized in that in the XRD result of the pole piece test, the ratio of the intensity of 003 diffraction peak to 104 diffraction peak is 0.8 to 1.0;
The ternary material comprises LiNi xCoyMn1-x-yO2 and residual lithium ions, wherein x is more than or equal to 0.55 and less than or equal to 0.60,0.10 and y is more than or equal to 0.12;
the ratio of the content of the residual lithium ions to the particle diameter D 50 of the ternary material is 150ppm/μm to 350ppm/μm.
2. The ternary material of claim 1, wherein the residual lithium ion content is 300ppm to 800ppm.
3. The ternary material according to claim 1, wherein the molar ratio of lithium ions to other metal ions in the starting material for the preparation of the ternary material is (1.05 to 1.09): 1.
4. An electrochemical device comprising the ternary material of any one of claims 1 to 3.
5. The electrochemical device according to claim 4, wherein the positive electrode sheet of the electrochemical device has a composition comprising a ternary material having a mass ratio of (90 to 99): (0.1 to 7): 1, a conductive agent and a binder.
6. The electrochemical device of claim 4 wherein the composition of the negative electrode sheet of the electrochemical device comprises (90 to 99): (0.1 to 5): 2 graphite, a conductive agent, and a binder.
7. The electrochemical device of claim 4, wherein the electrolyte of the electrochemical device comprises lithium hexafluorophosphate.
8. An electronic device, characterized in that it comprises the electrochemical apparatus according to any one of claims 4 to 7.
CN202210394676.8A 2022-04-14 2022-04-14 Ternary material and application thereof Active CN114709413B (en)

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