CN110156092A - A kind of dried persimmon shape cobaltosic oxide lithium cell cathode material and preparation method thereof - Google Patents
A kind of dried persimmon shape cobaltosic oxide lithium cell cathode material and preparation method thereof Download PDFInfo
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- CN110156092A CN110156092A CN201910509415.4A CN201910509415A CN110156092A CN 110156092 A CN110156092 A CN 110156092A CN 201910509415 A CN201910509415 A CN 201910509415A CN 110156092 A CN110156092 A CN 110156092A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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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
- 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
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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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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- 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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
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- 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
This application discloses a kind of dried persimmon shape cobaltosic oxide lithium cell cathode material and preparation method thereof, the preparation method is the following steps are included: in water by salt solubility, prepare cobalt salt solution；1,2,4 triazoles are added in cobalt salt solution, then add 3,5- dimethyl pyrazole, form light violet magenta solution；Hydrazine hydrate is added in the above solution, until obtain aubergine paste precipitating, 90 DEG C heating water bath 30 minutes, centrifuge separation, precipitating through deionized water washing three times, dehydrated alcohol wash three times, drying obtain aubergine cobalt precursor；Gained cobalt precursor is subjected to high-temperature calcination with temperature control muffle furnace, dried persimmon shape cobaltosic oxide is obtained after natural cooling.The dried persimmon shape hierarchical structure cobaltosic oxide that dried persimmon shape cobaltic-cobaltous oxide negative pole material of the invention is assembled by little particle forms.Cobaltic-cobaltous oxide negative pole material of the invention is with preferable charge/discharge capacity and good cycle performance.
Description
Technical field
The present invention relates to a kind of dried persimmon shape cobaltosic oxide lithium cell cathode materials and preparation method thereof.
Background technique
Currently, power lithium-ion battery is the bottleneck for restricting new-energy automobile development, exploitation specific capacity is high, stability is good,
The strong new type lithium ion battery of long service life, environmental suitability is extremely urgent.And the negative electrode material such as stone of current industrial application
The specific capacities such as ink, soft carbon, hard carbon are relatively low, and (graphite theoretical specific capacity is only 372mAh.-1), it is not easy fast charging and discharging, and overcharging resisting
Overdischarge ability is poor, it is difficult to meet the requirements, it would be highly desirable to develop novel cathode material for lithium ion battery.Cobaltosic oxide (Co3O4) reason
It is 890372mAh. by specific capacity-1, it is 2.5 times of graphite, and density is 3 times of graphite, i.e., volume and capacity ratio is the 7.5 of graphite
Times, can be substantially reduced the volume of large-scale lithium ion battery, chemical property is stablized again, for ideal power lithium battery negative electrode material it
One.
Cobaltosic oxide (Co3O4) it is in grey black or black powder, density size is 6.0-6.2g/cm3, molecular weight
240.80。Co3O4Belong to cubic system, the nm of lattice parameter a=0.811 has AB2O4Spinel structure, skeleton are tetrahedrons
With octahedra coplanar three-dimensional net structure, such structure is conducive to the diffusion of ion.With magnetic iron oxide Fe3O4It is heterogeneous
The isomorphous.
The patent of invention of Publication No. CN108483513A discloses a kind of preparation method of three-dimensional flower-shaped cobaltosic oxide,
Include the following steps: to weigh four hydration cobalt acetate solids and SDS in beaker, ethylene glycol and deionized water is added, stirring is straight
It is completely dissolved to solid particle, obtains solution A；The second component metals nitrate and TBAB are weighed in another beaker, second is added
Glycol stirring is completely dissolved up to solid particle, obtains solution B；Solution B is poured into solution A, continues to be added after stirring 30min
Urea, then solution is transferred in water heating kettle after persistently stirring 60min, it is placed in 180 DEG C of heating 8h in drying box；After cooling,
It takes out reaction solution to pour into centrifuge tube, centrifugation 5min is carried out with the speed of 4000rad/s, it is heavy to be first washed with deionized after centrifugation
Starch reuses dehydrated alcohol washing repeatedly, later by drying precipitate, is put into 300 DEG C of roasting 180min in Muffle furnace.
Summary of the invention
It is an object of that present invention to provide a kind of dried persimmon shape cobaltosic oxide lithium cell cathode materials and preparation method thereof.
To achieve the above object, present invention provide the technical scheme that a kind of dried persimmon shape cobaltosic oxide cathode of lithium battery
The preparation method of material, including the following steps:
Step 1: in water by salt solubility, cobalt salt solution is made；
Step 2: under agitation, the cobalt salt solution is diluted 10 times, 1,2,4 triazoles are then first added, add 3,
5- dimethyl pyrazole forms the first solution；
Step 3: under agitation, hydrazine hydrate is added in the first solution of Xiang Suoshu, until obtaining paste；
Step 4: the heating water bath under the conditions of carrying out 70-90 DEG C to the paste is then centrifuged for separating, obtain to generate precipitating
To sediment be first washed with deionized, then washed with dehydrated alcohol, then drying obtains cobalt precursor；
Step 5: the cobalt precursor is placed in crucible, then close the lid, then carry out high-temperature calcination with temperature control muffle furnace,
Up to dried persimmon shape cobaltosic oxide after natural cooling.
Preferred technical solution are as follows: in the first step, the concentration of the cobalt salt solution is 0.1-0.5mol/L.
Preferred technical solution are as follows: the cobalt salt is cobalt nitrate, cobalt acetate or cobalt chloride.
Preferred technical solution are as follows: in second step, cobalt salt and 1,2,4 triazole molar ratios are 1:2-1:5；Cobalt salt and 3,
5- dimethyl pyrazole molar ratio is 1:1.5-1:3.
Preferred technical solution are as follows: in second step, the molar ratio of cobalt salt and hydrazine hydrate is 1:20-1:25.
Preferred technical solution are as follows: in second step and third step, speed of agitator is 180-220 r/min, reaction temperature
It is 20-25 DEG C.
Preferred technical solution are as follows: temperature condition when drying is 50-70 DEG C.
Preferred technical solution are as follows: in the 5th step, calcination temperature is 450-600 DEG C, and calcination time is 1-3 hours, is risen
Warm rate is 1-5 DEG C/minute.
To achieve the above object, present invention provide the technical scheme that a kind of dried persimmon shape cobaltosic oxide cathode of lithium battery
Material is prepared according to above-mentioned preparation method.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of the application dried persimmon shape cobaltosic oxide cell negative electrode material.
Fig. 2 is the XRD spectra of the application dried persimmon shape cobaltosic oxide cell negative electrode material.
Fig. 3 is the cycle performance of the application dried persimmon shape cobaltosic oxide cell negative electrode material.
Since above-mentioned technical proposal is used, the present invention has the advantage, that compared with prior art
Dried persimmon shape cobaltic-cobaltous oxide negative pole material produced by the present invention is aoxidized by the dried persimmon shape hierarchical structure four of little particle assembling
Three cobalts composition, has excellent charge/discharge capacity and good cycle performance.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
A kind of embodiment one: dried persimmon shape cobaltosic oxide lithium cell cathode material and preparation method thereof
A kind of preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material, including the following steps:
Step 1, by salt solubility in water, prepare cobalt salt solution；
Cobalt salt solution is diluted 10 times, 1,2,4 triazoles is added, then add 3,5- diformazan by step 2, under agitation
Base pyrazoles forms light violet magenta solution；Speed of agitator is 200r/min, and reaction temperature is 22.5 DEG C.
Step 3, in above-mentioned formation aubergine complex solution, hydrazine hydrate is added under agitation, until obtain purple
Red paste；Speed of agitator is 200r/min, and reaction temperature is 22.5 DEG C.
Step 4, aubergine paste through 90 DEG C heating water bath 30 minutes, obtain purple red precipitate.Centrifuge separation, precipitating are used
Deionized water is washed three times, and drying obtains aubergine cobalt precursor three times for dehydrated alcohol washing；
Step 5, gained aubergine cobalt precursor are placed in crucible (capping), carry out high-temperature calcination with temperature control muffle furnace, naturally cold
But dried persimmon shape cobaltosic oxide is obtained afterwards.
Preferred embodiment are as follows: the concentration of the cobalt salt solution in step 1 is 0.3mol/L.
Cobalt salt solution in step 1 is cobalt nitrate aqueous solution.
Cobalt salt in step 2 and 1,2,4 triazole molar ratios are 1:3.5；Cobalt salt and 3,5- dimethyl pyrazole molar ratio are
1:2.25。
The molar ratio of cobalt salt and hydrazine hydrate is 1:22.5 in step 3.
Drying temperature in step 4 is 60 DEG C.
Crucible (capping) when calcining in step 5, temperature are 525 DEG C, and the time is 2 hours, and heating rate is 3 DEG C/minute.
The stereoscan photograph of dried persimmon shape cobaltosic oxide cell negative electrode material made from the present embodiment is as shown in Figure 1；Persimmon
The XRD spectra of pie cobaltosic oxide cell negative electrode material is as shown in Figure 2；Dried persimmon shape cobaltosic oxide cell negative electrode material follows
Ring performance is as shown in Figure 3.
A kind of embodiment two: dried persimmon shape cobaltosic oxide lithium cell cathode material and preparation method thereof
A kind of preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material, including the following steps:
Step 1: in water by salt solubility, cobalt salt solution is made；
Step 2: under agitation, the cobalt salt solution is diluted 10 times, 1,2,4 triazoles are then first added, add 3,
5- dimethyl pyrazole forms the first solution；
Step 3: under agitation, hydrazine hydrate is added in the first solution of Xiang Suoshu, until obtaining paste；
Step 4: the heating water bath under the conditions of carrying out 80 DEG C to the paste is then centrifuged for separating, obtain to generate precipitating
Sediment is first washed with deionized, then is washed with dehydrated alcohol, and then drying obtains cobalt precursor；
Step 5: the cobalt precursor is placed in crucible, then close the lid, then carry out high-temperature calcination with temperature control muffle furnace,
Up to dried persimmon shape cobaltosic oxide after natural cooling.
Preferred embodiment are as follows: in the first step, the concentration of the cobalt salt solution is 0.1mol/L.
Preferred embodiment are as follows: the cobalt salt is cobalt acetate.
Preferred embodiment are as follows: in second step, cobalt salt and 1,2,4 triazole molar ratios are 1:2；Cobalt salt and 3,5- bis-
Methylpyrazole molar ratio is 1:1.5.
Preferred embodiment are as follows: in second step, the molar ratio of cobalt salt and hydrazine hydrate is 1:20.
Preferred embodiment are as follows: in second step and third step, speed of agitator 180r/min, reaction temperature 25
℃。
Preferred embodiment are as follows: temperature condition when drying is 50 DEG C.
Preferred embodiment are as follows: in the 5th step, calcination temperature is 450 DEG C, and calcination time is 3 hours, heating rate
It is 1 DEG C/minute.
A kind of dried persimmon shape cobaltosic oxide lithium cell cathode material, is prepared according to above-mentioned preparation method.
A kind of embodiment three: dried persimmon shape cobaltosic oxide lithium cell cathode material and preparation method thereof
A kind of preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material, including the following steps:
Step 1: in water by salt solubility, cobalt salt solution is made；
Step 2: under agitation, the cobalt salt solution is diluted 10 times, 1,2,4 triazoles are then first added, add 3,
5- dimethyl pyrazole forms the first solution；
Step 3: under agitation, hydrazine hydrate is added in the first solution of Xiang Suoshu, until obtaining paste；
Step 4: the heating water bath under the conditions of carrying out 70 DEG C to the paste is then centrifuged for separating, obtain to generate precipitating
Sediment is first washed with deionized, then is washed with dehydrated alcohol, and then drying obtains cobalt precursor；
Step 5: the cobalt precursor is placed in crucible, then close the lid, then carry out high-temperature calcination with temperature control muffle furnace,
Up to dried persimmon shape cobaltosic oxide after natural cooling.
Preferred embodiment are as follows: in the first step, the concentration of the cobalt salt solution is 0.5mol/L.
Preferred embodiment are as follows: the cobalt salt is cobalt chloride.
Preferred embodiment are as follows: in second step, cobalt salt and 1,2,4 triazole molar ratios are 1:5；Cobalt salt and 3,5- bis-
Methylpyrazole molar ratio is 1:3.
Preferred embodiment are as follows: in second step, the molar ratio of cobalt salt and hydrazine hydrate is 1:25.
Preferred embodiment are as follows: in second step and third step, speed of agitator is 220 r/min, reaction temperature 20
℃。
Preferred embodiment are as follows: temperature condition when drying is 70 DEG C.
Preferred embodiment are as follows: in the 5th step, calcination temperature is 600 DEG C, and calcination time is 1 hour, heating rate
It is 5 DEG C/minute.
A kind of dried persimmon shape cobaltosic oxide lithium cell cathode material, is prepared according to above-mentioned preparation method.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (9)
1. a kind of preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material, it is characterised in that: include the following steps:
Step 1: in water by salt solubility, cobalt salt solution is made；
Step 2: under agitation, the cobalt salt solution is diluted 10 times, 1,2,4 triazoles are then first added, add 3,
5- dimethyl pyrazole forms the first solution；
Step 3: under agitation, hydrazine hydrate is added in the first solution of Xiang Suoshu, until obtaining paste；
Step 4: the heating water bath under the conditions of carrying out 70-90 DEG C to the paste is then centrifuged for separating, obtain to generate precipitating
To sediment be first washed with deionized, then washed with dehydrated alcohol, then drying obtains cobalt precursor；
Step 5: the cobalt precursor is placed in crucible, then close the lid, then carry out high-temperature calcination with temperature control muffle furnace,
Up to dried persimmon shape cobaltosic oxide after natural cooling.
2. the preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material according to claim 1, it is characterised in that:
In the first step, the concentration of the cobalt salt solution is 0.1-0.5mol/L.
3. the preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material according to claim 1, it is characterised in that:
The cobalt salt is cobalt nitrate, cobalt acetate or cobalt chloride.
4. the preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material according to claim 1, it is characterised in that:
In second step, cobalt salt and 1,2,4 triazole molar ratios are 1:2-1:5；Cobalt salt and 3,5- dimethyl pyrazole molar ratio are 1:
1.5-1:3。
5. the preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material according to claim 1, it is characterised in that:
In second step, the molar ratio of cobalt salt and hydrazine hydrate is 1:20-1:25.
6. the preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material according to claim 1, it is characterised in that:
In second step and third step, speed of agitator is 180-220 r/min, and reaction temperature is 20-25 DEG C.
7. the preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material according to claim 1, it is characterised in that:
Temperature condition when drying is 50-70 DEG C.
8. the preparation method of dried persimmon shape cobaltosic oxide lithium cell cathode material according to claim 1, it is characterised in that:
In the 5th step, calcination temperature is 450-600 DEG C, and calcination time is 1-3 hours, and heating rate is 1-5 DEG C/minute.
9. a kind of dried persimmon shape cobaltosic oxide lithium cell cathode material, it is characterised in that: according to any right in claim 1-8
It is required that the preparation method is prepared.
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Cited By (1)
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| CN114082396A (en) * | 2021-09-28 | 2022-02-25 | 淮阴师范学院 | Magnetic persimmon cake-shaped cerium ferrite/cerium dioxide composite adsorbent and preparation method thereof |
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