CN109065852A - A kind of positive electrode and preparation method thereof - Google Patents
A kind of positive electrode and preparation method thereof Download PDFInfo
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- CN109065852A CN109065852A CN201810724733.8A CN201810724733A CN109065852A CN 109065852 A CN109065852 A CN 109065852A CN 201810724733 A CN201810724733 A CN 201810724733A CN 109065852 A CN109065852 A CN 109065852A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/50—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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- 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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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
Abstract
The invention discloses a kind of positive electrodes and preparation method thereof.The preparation method includes the following steps: the aqueous solution of nickel ion doped, ammonium paramolybdate and thioacetamide in 200-240 DEG C of progress hydro-thermal reaction；Wherein, the molar ratio of nickel ion doped, ammonium paramolybdate and thioacetamide is 100:(0.16-1.6): (2.28-22.8).Positive electrode electron conduction of the invention and high rate performance are good, and 1C discharges gram volume up to 128.6mAh/g for the first time, and discharging efficiency is up to 94.16% for the first time, and capacity retention ratio is up to 98.83% after circulation 100 is enclosed；The layer of molybdenum-disulfide uniformly coated simultaneously avoids nickel ion doped particle and contacts with the direct of electrolyte, it prevents high valence ion to the oxidation of electrolyte, and then effectively inhibits the oxygenolysis of electrolyte, improve the cycle performance of material, and preparation method reaction of the invention is mild, facilitates control.
Description
Technical field
The present invention relates to a kind of positive electrodes and preparation method thereof.
Background technique
Nickel lithium manganate cathode material operating voltage with higher (4.7V) enables it compared to other traditional positive electrodes
Higher energy density is enough provided, this is based on, in recent years, nickel lithium manganate cathode material is by the extensive of academia and industry
Concern.Nickel lithium manganate cathode material is substantially traditional spinel-type positive electrode LiMn2O4Modified material, Ni therein from
Son not only provides higher operating voltage and bigger specific capacity, can also effectively reduce Mn3+Content is effectively improved original
The high temperature cyclic performance of spinel-type positive electrode, thus a possibility that greatly improving material application.But also just because of nickel manganese
Sour lithium operating voltage is high, reacts so that electrode material is easy to happen interface oxidation with the contact surface of electrolyte, will be greatly reduced it
Cycle life.
The method that cladding can be used at present is modified nickel ion doped material surface, can avoid electrode material as far as possible
This side reaction between surface and electrolyte is expected, so as to improve the chemical property of material.However, patent CN104828878A
Graphene is added in the nickel ion doped material precursor stage, while graphene can be reacted with oxygen in high-temperature sintering process,
Part Mn can also be restored4+It is converted into Mn3+, graphene is by the effect of a large amount of consumption reduction claddings, Mn3+Generation so that material
Cycle performance is deteriorated；Patent CN106299348A is directly mixed using nickel ion doped forerunner liquid suspension and oxide suspension
Method, it is difficult to realize to mix since both of which belongs to the solid powder of indissoluble；Patent CN105226267A coating carbon
Nanotube is not in-situ preparation, but two solid phases directly stir and evenly mix the product that drying obtains, and cladding process is difficult to control.
Therefore, a kind of nickel lithium manganate cathode material that chemical property is good is researched and developed to be a problem to be solved.
Summary of the invention
The present invention is practical, and the technical problem to be solved is that in order to overcome nickel ion doped electrode material in the prior art and electricity
Solution liquid contacts and then leads to that its cycle life is low, selects the modified poor circulation of graphene, nickel ion doped forerunner's liquid suspension
Directly mixed with oxide suspension cladding process when mixing, selecting carbon nano-tube modification difficult to realize be difficult to control etc. it is scarce
It falls into, provides a kind of positive electrode and preparation method thereof.The electronic conduction of molybdenum disulfide cladding nickel ion doped material of the invention
Property and high rate performance it is good, the layer of molybdenum-disulfide uniformly coated avoids directly contacting for nickel ion doped particle and electrolyte, prevents
Only high valence ion is to the oxidation of electrolyte, and then effectively inhibits the oxygenolysis of electrolyte, improves the circulation of material
Performance, and preparation method reaction of the invention is mild, facilitates control.
The present invention solves above-mentioned technical problem by the following technical programs.
The present invention provides a kind of preparation methods of positive electrode comprising following step:
By the aqueous solution of nickel ion doped, ammonium paramolybdate and thioacetamide in 200-240 DEG C of progress hydro-thermal reaction；
Wherein, the molar ratio of the nickel ion doped, the ammonium paramolybdate and the thioacetamide is 100:(0.16-
1.6): (2.28-22.8).
In the present invention, the preparation method of the nickel ion doped may include following step:
(1) lithium source, nickel source, manganese source that atomic molar ratio is Li:Ni:Mn=(1-1.05): 0.5:1.5 are mixed with water
It is even to form the solution that solid content is 20%-30%；
(2) it is spray-dried after acquired solution being sanded, obtains presoma powder body material；
(3) the presoma powder body material is subjected to pre-burning, obtains Preburning material；
(4) Preburning material is calcined, carrying out annealing later can be obtained nickel ion doped.
Wherein, in step (1), lithium source, nickel source and manganese source can be the raw material commonly used in the art in production electrode material.It is described
Lithium source is one of lithium carbonate, lithium hydroxide, lithium acetate and lithium nitrate or a variety of.The nickel source is nickel oxalate, nickel oxide, nitre
One of sour nickel and nickel hydroxide are a variety of.The manganese source is manganese oxide, manganese acetate, manganese dioxide, mangano-manganic oxide and nitre
One of sour manganese is a variety of.
In step (1), the water can be water commonly used in the art, may be, for example, deionized water.
In step (1), the atomic molar of described Li, Ni, Mn are than being preferably 1.03:0.5:1.5.
In step (1), the solid content of the solution is preferably 25%.
In step (2), the sand milling and operate and condition can be conventional for this field, the sand milling can be used sand mill into
Row.The time of the sand milling can be conventional for this field, may be, for example, 1-3h, can also be 2h.
In step (2), the partial size of the presoma powder body material can be conventional for this field, may be, for example, 15-25um.
In step (3), the temperature of the pre-burning can be conventional for this field, such as the temperature of the pre-burning can be 350-550
DEG C, it can also be 450 DEG C.The time of the pre-burning can be conventional for this field, for example, the time of the pre-burning can be 1-3h, may be used also
For 2h.
In step (4), the temperature of the calcining can be conventional for this field, such as the temperature of the calcining can be 750-1000
DEG C, it can also be 900 DEG C.The time of the calcining can be conventional for this field, for example, the time of the calcining can be 8-20h, may be used also
For 12h.
In step (4), the temperature of the annealing can be conventional for this field, may be, for example, 650-700 DEG C, can also be 680 DEG C.
The time of the annealing can be conventional for this field, may be, for example, 4-6h, can also be 5h.
In step (4), the nickel ion doped can be spherical nickel-lithium manganate.Wherein, the partial size of the spherical nickel-lithium manganate can
For 20-30um.
It, can be before the hydro-thermal reaction, by the water to guarantee that the performance of the nickel ion doped is not affected in the present invention
The pH of solution is adjusted to 6-7.The operation for adjusting pH can be conventional for this field, such as hydrochloric acid progress can be used.
In the present invention, the temperature of the hydro-thermal reaction can be 210-230 DEG C, can also be 220 DEG C.
In the present invention, the time of the hydro-thermal reaction can be conventional for this field, may be, for example, 18-24h.
In the present invention, the hydro-thermal reaction can carry out in stainless steel cauldron, as known to those skilled in the art, the water
It needs for the reaction kettle to be sealed before thermal response.
In the present invention, as known to those skilled in the art, need to be post-processed after the hydro-thermal reaction, the post-processing
The step of may include being cooled to room temperature, by gained reaction product separation, washing, dry.
In the present invention, the molar ratio of the nickel ion doped, the ammonium paramolybdate and the thioacetamide can be 100:
(0.6-1.0): (10.0-14.5) can also be 100:0.88:12.54.
The present invention also provides a kind of molybdenum disulfide cladding nickel ion doped materials prepared by the preparation method (just
Pole material).
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the present invention
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that:
The electron conduction and high rate performance of positive electrode of the invention --- molybdenum disulfide cladding nickel ion doped material are good
Good, the 1C gram volume that discharges for the first time reaches 125.3-128.6mAh/g, and discharging efficiency reaches 90.45%-94.16% for the first time, follows
Capacity retention ratio reaches 88.53%-98.83% after ring 100 encloses；The layer of molybdenum-disulfide uniformly coated simultaneously avoids nickel ion doped
Particle is directly contacted with electrolyte, prevents high valence ion to the oxidation of electrolyte, and then effectively inhibit electrolyte
Oxygenolysis improves the cycle performance of material, and preparation method reaction of the invention is mild, facilitates control.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
Nickel ion doped (LiNi0.5Mn1.5O4) Ni in material is easy to be enriched in surface, on the one hand cause material to be easy to inhale
On the other hand water causes Ni different with the valence state of ontology in the valence state on surface, point of catalytic electrolysis liquid is easy under high potential
Solution.Molybdenum disulfide (MoS2) structure it is similar with graphene, be a kind of typical stratiform transition metal sulphur compound, with other gold
Belong to oxide compare, have the advantages that large specific surface area, adsorption capacity by force, good conductivity.In the present invention, ammonium paramolybdate and sulphur
For acetamide by hydro-thermal reaction in nickel ion doped particle surface in-situ preparation molybdenum disulfide, and then molybdenum disulfide cladding is made
Nickel ion doped material.
In following example 1-3 and comparative example 1, the partial size of spherical nickel-lithium manganate material obtained is within the scope of 20-30um.
Embodiment 1
Lithium carbonate, nickel oxide, manganese oxide are weighed respectively with molar ratio Li:Ni:Mn=1.03:0.5:1.5, are added suitable
Deionized water makes its solid content 25%.2h is sanded to above-mentioned solution using sand mill, obtained powder body material after spray-dried.
Muffle furnace 450 DEG C of pre-burnings 2h, 900 DEG C of high-temperature calcination 12h are placed on, then anneal at 680 DEG C 5h, obtains spherical nickel mangaic acid
Lithium anode material.
Weighing molar ratio is nickel ion doped: ammonium paramolybdate: thioacetamide=100:0.16:2.28 above-mentioned material is uniform
Dispersion in deionized water, uses salt acid for adjusting pH value to 6~7, is transferred to stainless steel after obtained solution stirring after stirring 5min
Reaction kettle, sealing are cooled to room temperature after 220 DEG C of processing for 24 hours, by the separation of gained reaction product, washing, drying, obtain curing
Molybdenum coats spherical nickel-lithium manganate material.
Embodiment 2
Lithium carbonate, nickel oxide, manganese oxide are weighed respectively with molar ratio Li:Ni:Mn=1.03:0.5:1.5, are added suitable
Deionized water makes its solid content 25%.2h is sanded to above-mentioned solution using sand mill, obtained powder body material after spray-dried.
Muffle furnace 450 DEG C of pre-burnings 2h, 900 DEG C of high-temperature calcination 12h are placed on, then anneal at 680 DEG C 5h, obtains spherical nickel mangaic acid
Lithium anode material.
Weighing molar ratio is nickel ion doped: ammonium paramolybdate: thioacetamide=100:0.88:12.54 above-mentioned material is equal
Even dispersion in deionized water, is used salt acid for adjusting pH value to 6~7, is transferred to after obtained solution stirring stainless after stirring 5min
Steel reaction kettle, sealing are cooled to room temperature after 220 DEG C of processing for 24 hours, by the separation of gained reaction product, washing, drying, obtain two sulphur
Change molybdenum and coats spherical nickel-lithium manganate material.
Embodiment 3
Lithium carbonate, nickel oxide, manganese oxide are weighed respectively with molar ratio Li:Ni:Mn=1.03:0.5:1.5, are added suitable
Deionized water makes its solid content 25%.2h is sanded to above-mentioned solution using sand mill, obtained powder body material after spray-dried.
Muffle furnace 450 DEG C of pre-burnings 2h, 900 DEG C of high-temperature calcination 12h are placed on, then anneal at 680 DEG C 5h, obtains spherical nickel mangaic acid
Lithium anode material.
Weighing molar ratio is nickel ion doped: ammonium paramolybdate: thioacetamide=100:1.6:22.8 above-mentioned material is uniform
Dispersion in deionized water, uses salt acid for adjusting pH value to 6~7, is transferred to stainless steel after obtained solution stirring after stirring 5min
Reaction kettle, sealing are cooled to room temperature after 220 DEG C of processing for 24 hours, by the separation of gained reaction product, washing, drying, obtain curing
Molybdenum coats spherical nickel-lithium manganate material.
Comparative example 1
Lithium carbonate, nickel oxide, manganese oxide are weighed respectively with molar ratio Li:Ni:Mn=1.03:0.5:1.5, are added suitable
Deionized water makes its solid content 25%.2h is sanded to above-mentioned solution using sand mill, obtained powder body material after spray-dried.
Muffle furnace 450 DEG C of pre-burnings 2h, 900 DEG C of high-temperature calcination 12h are placed on, then anneal at 680 DEG C 5h, obtains spherical nickel mangaic acid
Lithium anode material.
Effect example 1
The obtained positive electrode of above embodiments 1-3 and comparative example 1 is used for CR2016 type button cell, then carries out electricity
Performance test is learned, the results are shown in Table 1.By data in table 1 it is found that the electric property for the positive electrode that embodiment 1-3 is prepared more
It is excellent.
Table 1
Although specific embodiments of the present invention have been described above, it will be appreciated by those of skill in the art that this is only
For example, protection scope of the present invention is to be defined by the appended claims.Those skilled in the art without departing substantially from
Under the premise of the principle and substance of the present invention, many changes and modifications may be made, but these change and
Modification each falls within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of positive electrode, which is characterized in that its include the following steps: by nickel ion doped, ammonium paramolybdate and
The aqueous solution of thioacetamide is in 200-240 DEG C of progress hydro-thermal reaction；
Wherein, the molar ratio of the nickel ion doped, the ammonium paramolybdate and the thioacetamide is 100:(0.16-1.6):
(2.28-22.8)。
2. preparation method as described in claim 1, which is characterized in that the preparation method of the nickel ion doped includes following steps
It is rapid:
(1) lithium source, nickel source, manganese source that atomic molar ratio is Li:Ni:Mn=(1-1.05): 0.5:1.5 are uniformly mixed shape with water
The solution for being 20%-30% at solid content；
(2) it is spray-dried after acquired solution being sanded, obtains presoma powder body material；
(3) the presoma powder body material is subjected to pre-burning, obtains Preburning material；
(4) Preburning material is calcined, carrying out annealing later can be obtained nickel ion doped.
3. preparation method as claimed in claim 2, which is characterized in that in step (1), the lithium source is lithium carbonate, hydroxide
One of lithium, lithium acetate and lithium nitrate are a variety of；
In step (1), the nickel source is one of nickel oxalate, nickel oxide, nickel nitrate and nickel hydroxide or a variety of；
In step (1), the manganese source is one of manganese oxide, manganese acetate, manganese dioxide, mangano-manganic oxide and manganese nitrate or more
Kind；
In step (1), the water is deionized water；
In step (1), the atomic molar ratio of described Li, Ni, Mn are 1.03:0.5:1.5；
In step (1), the solid content of the solution is 25%；
In step (2), described be sanded is carried out using sand mill；
In step (2), the time of the sand milling is 1-3h, preferably 2h；
In step (2), the partial size of the presoma powder body material is 15-25um.
4. preparation method as claimed in claim 2, which is characterized in that in step (3), the temperature of the pre-burning is 350-550
DEG C, preferably 450 DEG C；
In step (3), the time of the pre-burning is 1-3h, preferably 2h；
In step (4), the temperature of the calcining is 750-1000 DEG C, preferably 900 DEG C；
In step (4), the time of the calcining is 8-20h, preferably 12h；
In step (4), the temperature of the annealing is 650-700 DEG C, preferably 680 DEG C；
In step (4), the time of the annealing is 4-6h, preferably 5h；
In step (4), the nickel ion doped is spherical nickel-lithium manganate, and the partial size of the spherical nickel-lithium manganate is preferably 20-
30um。
5. preparation method as described in claim 1, which is characterized in that before the hydro-thermal reaction, by the pH of the aqueous solution
It is adjusted to 6-7.
6. preparation method as claimed in claim 5, which is characterized in that adjust the pH using hydrochloric acid.
7. preparation method as described in claim 1, which is characterized in that the temperature of the hydro-thermal reaction is 210-230 DEG C, preferably
Ground is 220 DEG C；
The time of the hydro-thermal reaction is 18-24h；
The hydro-thermal reaction carries out in stainless steel cauldron.
8. preparation method as described in claim 1, which is characterized in that post-processed after the hydro-thermal reaction；It is described
The step of post-processing, which is preferably comprised, to be cooled to room temperature, by the separation of gained reaction product, washing, drying.
9. preparation method as described in claim 1, which is characterized in that the nickel ion doped, the ammonium paramolybdate and the sulphur
Molar ratio for acetamide is 100:(0.6-1.0): (10.0-14.5), preferably 100:0.88:12.54.
10. a kind of positive electrode that preparation method as claimed in any one of claims 1-9 wherein is prepared.
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Cited By (2)
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| CN112289998A (en) * | 2020-10-30 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Ternary cathode material with double-layer coating structure on surface and preparation method thereof |
| WO2023123942A1 (en) * | 2021-12-29 | 2023-07-06 | 中国科学院过程工程研究所 | Lithium-rich manganese-based positive electrode material, preparation method therefor and application thereof |
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