CN110085848A - A kind of lithium-rich manganese-based anode material and preparation method thereof - Google Patents
A kind of lithium-rich manganese-based anode material and preparation method thereof Download PDFInfo
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- CN110085848A CN110085848A CN201910411585.9A CN201910411585A CN110085848A CN 110085848 A CN110085848 A CN 110085848A CN 201910411585 A CN201910411585 A CN 201910411585A CN 110085848 A CN110085848 A CN 110085848A
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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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Abstract
The present invention provides a kind of lithium-rich manganese-based anode materials and preparation method thereof, including by MnCl2With metal chloride according to the molar ratio of each metallic element in target positive electrode at metal chloride mixed solution；The mixed solution is MnxM1‑xCl2；Wherein, one or more of M Co, Ni, Cr, 0 < x < 1；After metal chloride mixed solution ultrasonic atomizatio, spray pyrolysis is carried out, lithium-rich manganese base oxide presoma is obtained；It is sintered after lithium-rich manganese base oxide presoma is mixed with lithium salts, obtains lithium-rich manganese-based anode material.Without adding any additive into metal chloride solution in preparation method provided by the invention, that is, it can be directly used for spray pyrolysis preparation lithium-rich manganese base oxide presoma；There is good layer structure, height ratio capacity and excellent cyclical stability using lithium-rich manganese-based anode material prepared by the lithium-rich manganese base oxide presoma.
Description
Technical field
The present invention relates to field of lithium ion battery anode, in particular to a kind of lithium-rich manganese-based anode material and its preparation
Method.
Background technique
In recent years, lithium ion battery is in mobile phone, laptop, electric tool, electric car and other energy-storage systems
In be more and more widely used.The capacity of lithium ion battery largely receives the limitation of positive electrode, therefore opens
Sending out the positive electrode with high capacity, low cost a kind of is always project that researcher extremely pays close attention to.Positive lithium-rich manganese-based anode material
Expect xLi2MnO3·(1-x)LiMO2(one or more of M Co, Mn, Al etc.) practical reversible capacity reaches 250mAhg-1Or
It is higher, particularly suitable as electric vehicle (EV) or the high energy battery positive electrode of hybrid electric vehicle (HEV).
Positive electrode is prepared with process is short, strong to adaptability to raw material, process is simple, production capacity is big, raw with spray pyrolysis
Many advantages, such as high-efficient is produced, industrialized production is conducive to.Its product has spherical morphology, particle size controllable and is distributed equal
Even, the advantages that large specific surface area and product component are uniform.Spray pyrolysis has been widely used for preparing the lithium ion of different crystal forms
Cell positive material.It uses nitrate solution for raw material currently, spray pyrolysis prepares the positive electrode overwhelming majority, and needs molten
Additive (such as PVP, citric acid, urea) is added in liquid can just obtain the material with more regular spherical morphology；Another party
Face, although using nitrate solution as spinel structure positive electrode (such as LiMn prepared by raw material2O4), polyanionic anode
Material (such as Li2MSiO4(M=Mn, Fe), LiCo1/3Mn1/3Fe1/3PO4) and layered cathode material (such as LiNi1/3Co1/3Mn1/ 3O2) there is preferable chemical property, but prepared lithium-rich manganese-based anode material (such as Li [Li0.2Ni0.2Mn0.6]O2,
0.6Li2MnO3-0.4Li(Ni1/3Co1/3Mn1/3)O2) chemical property it is all poor.Due to the solubility of variety classes salt, mistake
The physicochemical properties such as saturation degree, fusing point, pyrolysis temperature have differences, and atomized drop is caused to form the machine of solid oxide composition granule
System is different, final pattern, granularity and the surface texture for influencing powder product.Powder product pattern, in terms of difference
Property will to the chemical property of subsequent prepared positive electrode generate significant impact.Currently, to using metal chloride to spray for raw material
The research that mist pyrolysis prepares lithium ion anode material is seldom, especially lack to more metal chloride spray pyrolysis prepare it is lithium-rich manganese-based just
The research of pole material.Research finds that villaumite decomposition temperature knows from experience corrosion equipment compared with the hydrogen chloride gas in nitrate height, tail gas, thus
Without further studying the possessed potential advantages on preparation high-performance positive electrode of oxide precursor prepared by villaumite.Cause
This, the potential advantages of research metal chloride spray pyrolysis preparation lithium-rich manganese base oxide presoma, to preparation high-performance richness lithium manganese
Base anode material important in inhibiting.
Summary of the invention
Based on the deficiencies of the prior art, the present invention provides a kind of lithium-rich manganese-based anode material and preparation method thereof, mesh
Be in order to use villaumite for raw material spray pyrolysis prepare lithium-rich manganese base oxide presoma, by synthesized by the presoma have it is good
The lithium-rich manganese-based anode material of good layer structure, height ratio capacity and excellent cycling stability.
In order to achieve the above object, the invention provides the following technical scheme:
(1) by MnCl2With metal chloride according to the molar ratio of each metallic element in target positive electrode at metal chlorine
Mixed salt solution；The mixed solution is MnxM1-xCl2, concentration 0.5mol/L；Wherein, one of M Co, Ni, Cr or several
Kind, 0 < x < 1；
It (2) is to carry with oxygen under the conditions of 800 DEG C by after metal chloride mixed solution ultrasonic atomizatio obtained by step (1)
Gas, flow rate of carrier gas are that 3L/min carries out spray pyrolysis, obtain lithium-rich manganese base oxide presoma, and the presoma is MnxM1-xO2；
Wherein, one or more of M Co, Ni, Cr, 0 < x < 1；
(3) it is sintered, obtains lithium-rich manganese-based after mixing lithium-rich manganese base oxide presoma obtained by step (2) with lithium salts
Positive electrode.
Preferably, when M includes Cr, the molar ratio of Cr and other metals is y:(80-y)；Wherein, 0 < y < 2.
Preferably, the lithium salts is lithium carbonate.
Preferably, the mass ratio of the presoma and lithium salts is 1:1.53.
Preferably, the temperature of the sintering is 950 DEG C, sintering time 16h.
The present invention also provides a kind of lithium-rich manganese-based anode materials, are prepared by above-mentioned any one the method, described
Lithium-rich manganese-based anode material is layer structure.
Above scheme of the invention have it is following the utility model has the advantages that
Heretofore described metal chloride solution can be directly used for spray pyrolysis preparation richness without adding any additive i.e.
Lithium manganese-base oxide presoma；Have using lithium-rich manganese-based anode material prepared by the lithium-rich manganese base oxide presoma good
Layer structure, height ratio capacity and excellent cyclical stability.In embodiment positive electrode obtained under 0.05C multiplying power for the first time
Specific discharge capacity is 309.0mAh g-1, coulombic efficiency is 78.6% for the first time.The electric discharge for the first time of 100 experiments is recycled under 1C multiplying power
Specific capacity is 206.2mAh g-1, the capacity retention ratio after circulation 100 is enclosed is 78.4%.
Method process of the invention is simple, and the structure and chemical property of synthesized lithium-rich manganese-based anode material are better than existing
Same material prepared by technology has in the high energy battery positive electrode field of electric vehicle (EV) or hybrid electric vehicle (HEV)
There is great application value.
Detailed description of the invention
Fig. 1 is gained Li in the embodiment of the present invention 11.2Ni0.13Co0.13Mn0.54O2XRD spectrum.
Fig. 2 is gained Ni in the embodiment of the present invention 10.13Co0.13Mn0.54OxAnd Li1.2Ni0.13Co0.13Mn0.54O2SEM figure
Spectrum.
Fig. 3 is gained Li in the embodiment of the present invention 11.2Ni0.13Co0.13Mn0.54O2First charge-discharge curve.
Fig. 4 is gained Li in the embodiment of the present invention 11.2Ni0.13Co0.13Mn0.54O2Cycle performance figure (2.0~4.6V, 25
Under the conditions of DEG C).
Fig. 5 is gained Li in the embodiment of the present invention 21.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2XRD diagram
Spectrum.
Fig. 6 is gained Li in the embodiment of the present invention 21.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2SEM figure
Spectrum.
Fig. 7 is gained Li in the embodiment of the present invention 21.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2For the first time
Charging and discharging curve.
Fig. 8 is gained Li in the embodiment of the present invention 21.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2Circulation
Performance map (2.0~4.6V, 25 DEG C under the conditions of).
Specific embodiment
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1
The lithium-rich manganese base oxide presoma prepared using metal chloride as raw material spray pyrolysis of the invention
Ni0.13Co0.13Mn0.54O2, comprising the following steps:
(1) by NiCl2、CoCl2And MnCl2Total metal ion is made into according to the ratio (molar ratio) of 0.13:0.13:0.54
Concentration is the metal chloride mixed solution of 0.5mol/L；
(2) Pyrolysis Experiment will be carried out after mixed solution ultrasonic atomizatio described in (1) (spray pyrolysis temperature setting is 800 DEG C)
Carrier gas (O2) flow velocity is set as 3L/min, prepare Ni0.13Co0.13Mn0.54O2Presoma, then to lithium-rich manganese base oxide forerunner
Body Ni0.13Co0.13Mn0.54O2Object phase and pattern detected.Fig. 2 is Ni0.13Co0.13Mn0.54O2SEM spectrum, it is known that gained
Product is a kind of porous solid microsphere being made of many primary particles, and spherical structure is more regular, and the partial size of particle is more equal
Even, diameter is in 1-2 microns.
(3) by lithium-rich manganese base oxide presoma Ni obtained by (2)0.13Co0.13Mn0.54O2With lithium carbonate according to 1:1.53's
Ratio mixing, in the agate mortar grind 1h after, first 500 DEG C at a temperature of pre-process 5h, reuse 950 DEG C of temperature calcinations
16h, then to gained lithium-rich manganese-based anode material Li1.2Ni0.13Co0.13Mn0.54O2Object phase, pattern and electrochemistry can be carried out
Detection.Fig. 1 is gained Li1.2Ni0.13Co0.13Mn0.54O2XRD spectrum, it is known that there are Li in product2MnO3And LiMO2Two objects
Phase, while can be seen that material has apparent layer structure, (006)/(012) and two groups of (108)/(110) peak all divide
It is fairly obvious.(003) of material/(104) peak ratio is greater than 1.2, illustrates that lithium nickel mixing phenomenon does not occur in material, sun from
Sub- ordered arrangement.The intensity of the diffraction maximum of material is all relatively strong, and rich lithium manganese crystal structure peak ten of the material between 20 °~25 °
It is clearly demarcated aobvious, illustrate that material has apparent lithium-rich manganese-based crystal phase.Fig. 2 is gained Li1.2Ni0.13Co0.13Mn0.54O2SEM spectrum,
Know that resulting materials are all the structure of a type ball-type, wherein the spherical structure that can significantly see is burnt the broken rear Asia formed
Micron level particle.Fig. 3 is gained Li1.2Ni0.13Co0.13Mn0.54O2First charge-discharge curve graph, Fig. 4 be its cycle performance
Figure, material first discharge specific capacity under 0.05C multiplying power is 292.0mAhg-1, coulombic efficiency is 82.0% for the first time.1C multiplying power
The first discharge specific capacity of lower 100 experiments of circulation is 177.4mAhg-1, circulation 100 circle after capacity retention ratio be
68.4%.
Embodiment 2
The lithium-rich manganese-based oxidation prepared after doping vario-property during spray pyrolysis using metal chloride as raw material of the invention
Object presoma Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2, comprising the following steps:
(1) by NiCl2、CoCl2And MnCl2And CrCl3According to (0.13-0.01/3): (0.13-0.01/3): (0.54-
0.01/3): 0.01 ratio (molar ratio) is made into the metal chloride mixed solution that total concentration of metal ions is 0.5mol/L；
(2) Pyrolysis Experiment will be carried out after mixed solution ultrasonic atomizatio described in (1) (spray pyrolysis temperature setting is 800 DEG C)
Carrier gas (O2) flow velocity is set as 3L/min, prepare Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2Presoma, then
To prepared lithium-rich manganese base oxide presoma Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2Object phase and pattern
It is detected.Fig. 6 is Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2SEM spectrum, it is known that be doped with Cr ion
Persursor material and the comparison of undoped persursor material, apparent variation all has occurred in pattern and structure, by original spherical shape
Structure is fully transformed to a kind of polyhedral crystal structure, and the partial size of the material after doping is more regular.
(3) by (2) resulting three kinds of lithium-rich manganese base oxide presomas Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/ 3Cr0.01O2Mixed with lithium carbonate according to the ratio of 1:1.53, in the agate mortar grind 1h after, first 500 DEG C at a temperature of
5h is pre-processed, is placed into high temperature resistance furnace, in 950 DEG C of roasting temperature 16h, then to gained lithium-rich manganese-based anode material
Li1.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2Object phase, pattern and electrochemistry can be carried out detection.Fig. 5 is institute
Obtain Li1.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2XRD spectrum, it is known that there are Li in product2MnO3And LiMO2
Two object phases, it can be observed that (006) of sample/(012) peak and (018)/(110) peak divide more than undoped raw material
Obviously, show that sample forms more typical layer structure, and the bulk strength of diffraction maximum is higher than undoped material.Simultaneously
The I (003) of sample/I (104) p-ratio is greater than 1.2, illustrates that the cation of material is orderly aligned.Fig. 6 is resulting
Li1.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2SEM spectrum, it is known that resulting materials be spherical structure do not advise
Whole and incomplete other amorphous pellets of submicron order, the more undoped material of the agglomeration of particle are declined, and one
The partial size of secondary particle is smaller.Fig. 7 is gained Li1.2Mn0.54-0.01/3Ni0.13-0.01/3Co0.13-0.01/3Cr0.01O2First charge-discharge
Curve graph, Fig. 8 are its cycle performance figure, and material first discharge specific capacity under 0.05C multiplying power is 309.0mAhg-1, library for the first time
Human relations efficiency is 78.6%.The first discharge specific capacity that 100 experiments are recycled under 1C multiplying power is 206.2mAhg-1, 100 circle of circulation
Capacity retention ratio afterwards is 78.4%.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of lithium-rich manganese-based anode material, characterized by the following steps:
(1) by MnCl2It is mixed according to the molar ratio of each metallic element in target positive electrode at metal chloride with metal chloride
Solution；The mixed solution is MnxM1-xCl2, concentration 0.5mol/L；Wherein, one or more of M Co, Ni, Cr, 0 <
X < 1；
(2) it by after metal chloride mixed solution ultrasonic atomizatio obtained by step (1), under the conditions of 800 DEG C, using oxygen as carrier gas, carries
Gas velocity is that 3L/min carries out spray pyrolysis, obtains lithium-rich manganese base oxide presoma, and the presoma is MnxM1-xO2；Wherein,
M is one or more of Co, Ni, Cr, 0 < x < 1；
(3) it is sintered after mixing lithium-rich manganese base oxide presoma obtained by step (2) with lithium salts, obtains lithium-rich manganese-based anode
Material.
2. method according to claim 1, which is characterized in that when M includes Cr, the molar ratio of Cr and other metals is y:
(80-y)；Wherein, 0 < y < 2.
3. method according to claim 1, which is characterized in that the lithium salts is lithium carbonate.
4. method according to claim 1, which is characterized in that the mass ratio of the presoma and lithium salts is 1:1.53.
5. method according to claim 1, which is characterized in that the temperature of the sintering is 950 DEG C, sintering time 16h.
6. a kind of lithium-rich manganese-based anode material, which is characterized in that it is prepared by Claims 1 to 5 any one the method,
The lithium-rich manganese-based anode material is layer structure.
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| CN116282184A (en) * | 2023-03-28 | 2023-06-23 | 湘潭大学 | Preparation method of manganese oxide positive electrode material |
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Application publication date: 20190802 |
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