CN106784797A - The preparation method of tertiary cathode material - Google Patents
The preparation method of tertiary cathode material Download PDFInfo
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- CN106784797A CN106784797A CN201710050233.6A CN201710050233A CN106784797A CN 106784797 A CN106784797 A CN 106784797A CN 201710050233 A CN201710050233 A CN 201710050233A CN 106784797 A CN106784797 A CN 106784797A
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- Prior art keywords
- water
- preparation
- soluble
- cathode material
- tertiary cathode
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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
- H01M4/36—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
-
- 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 preparation method of tertiary cathode material, including step：A, water-soluble lithium salts is mixed and dissolved with water-soluble transition metal salt, obtain mixed solution；B, heating mixed solution so that mixed solution evaporates and triggers burning, acquisition presoma；C, presoma is carried out to carry out high-temperature roasting after low temperature presintering again, obtain tertiary cathode material.The burn operation control that the preparation method of tertiary cathode material of the invention prepares raw material to presoma is carried out in air ambient, compared with burning assisting sol gel method of the prior art, can not only avoid producing pollution to the high temperature furnace needed for subsequent high temperature treatment, will not also be exploded because of high temperature furnace burner hearth finite volume simultaneously, improve process safety；Meanwhile, the preparation method experiment condition is easy to get, simple to operate, safe, low for equipment requirements, products therefrom excellent electrochemical performance, to produce the preferred feedstock of lithium battery, with very strong practical value.
Description
Technical field
The invention belongs to cell positive material technical field, specifically, it is related to a kind of suitable for the three of lithium ion battery
The preparation method of first positive electrode.
Background technology
Positive electrode is one of the bottleneck problem for restricting current lithium ion battery, and the size of positive electrode specific capacity is directly determined
Determine the specific capacity of lithium battery, influence its practical use, therefore the positive electrode for preparing for the lithium ion of excellent
Battery is extremely important, and the preparation method of the positive electrode for choosing is the approach of the positive electrode for having obtained.
At present, tertiary cathode material is used as a kind of good LiCoO2Substitute, it has also become the focus of development ＆ production.For
Tertiary cathode material, existing preparation method mainly has solid reaction process, coprecipitation, sol-gal process, burning assisting sol
Gel method, sputtering method etc..But the drawbacks of above-mentioned existing preparation method has certain, such as, solid reaction process is because of its raw material
It is mixed the uneven chemical property so as to cause final product not good enough；Coprecipitation condition is harsh to need control reaction
PH value and carried out under protective atmosphere, presoma needs further to mix lithium after preparing, exist processing step it is more long lack
Point；Sputtering method is the new advanced method of comparing, but higher to equipment requirement.
Sol-gal process is a kind of preparation method simple and easy to apply, and obtained tertiary cathode material mixing uniformity is good；
Burning assisting sol gel method is a kind of improved method on sol-gal process, and its difference is to add the auxiliary such as alcohols
Incendiary agent；Sol-gal process is all by soluble lithium salt, soluble mistake with the essence of burning assisting sol gel method as being
Cross dissolving metal salts and be prepared into well mixed collosol and gel in a solvent, collosol and gel is dried afterwards, then in high temperature furnace
Tertiary cathode material is prepared in calcining；But in both approaches, there are following problems：It is molten when being calcined in high temperature furnace
Glue gel occurs burning may produce pollution to high temperature furnace, because high temperature furnace burner hearth finite volume probably explodes, to life
Product brings hidden danger.
The content of the invention
To solve the problems, such as above-mentioned prior art, the invention provides a kind of preparation method of tertiary cathode material,
The preparation method safe operation and process is simple.
In order to reach foregoing invention purpose, present invention employs following technical scheme：
A kind of preparation method of tertiary cathode material, including step：A, by water-soluble lithium salts and water-soluble transition metal salt
Mix and dissolve, obtain mixed solution；B, the heating mixed solution, so that the mixed solution evaporates and triggers burning, obtain
Obtain presoma；C, the presoma is carried out to carry out high-temperature roasting after low temperature presintering again, obtain tertiary cathode material.
Further, in the step A, combustion adjuvant is also included in the mixed solution.
Further, the combustion adjuvant is triethanolamine.
Further, the ratio between the combustion adjuvant and amount of material of the water-soluble lithium salts are more than 1:1.
Further, the cation of the water-soluble transition metal salt is Ni2+、Co2+、Mn2+, anion is selected from Cl-、
NO3 -、SO4 2-、CH3COO-In at least one.
Further, in the water-soluble transition metal salt, Ni2+、Co2+And Mn2+The ratio between the amount of material be x:1-x-
y:y；Wherein, the ＜ y ＜ 1 of 0 ＜ x ＜ 1,0.
Further, the anion of the water-soluble lithium salts is selected from Cl-、NO3 -、SO4 2-、CH3COO-In at least one.
Further, the ratio between the water-soluble lithium salts and amount of material of the water-soluble transition metal salt are 0.7:1~
1.1:1。
Further, in the step C, the temperature of the low temperature presintering is 450 DEG C~550 DEG C, and the time is 1h~3h；
The temperature of the high-temperature roasting is 850 DEG C~950 DEG C, and the time is 8h~24h.
Further, in the step A, for dissolving the water-soluble lithium salts with the water-soluble transition metal salt
Solvent is water and/or alcohol.
Beneficial effects of the present invention：
(1) the burn operation control that the preparation method of tertiary cathode material of the invention prepares raw material to presoma
Carried out in air ambient, compared with burning assisting sol gel method of the prior art, can not only avoided to subsequent high temperature
High temperature furnace needed for treatment produces pollution, while will not also be exploded because of high temperature furnace burner hearth finite volume, improves technique peace
Quan Xing；
(2) the preparation method experiment condition of tertiary cathode material of the invention be easy to get, it is simple to operate, safe,
It is low for equipment requirements, products therefrom excellent electrochemical performance, to produce the preferred feedstock of lithium battery, with very strong practical valency
Value；
(3) preparation method of tertiary cathode material of the invention preferably uses combustion-supporting during prepared by presoma
Agent, on the one hand can ensure the heat energy of burning has more preferable crystallinity by product, so that the particle of product is smaller, is conducive to carrying
The specific surface area of product high；On the other hand preferably triethanolamine as combustion adjuvant, its simultaneously or chelating agent, mistake in product can be made
Cross that Metal Distribution is more uniform, be conducive to the raising of product chemical property.
Brief description of the drawings
By the following description carried out with reference to accompanying drawing, above and other aspect of embodiments of the invention, feature and advantage
Will become clearer, in accompanying drawing：
Fig. 1 is the XRD piece of the tertiary cathode material of embodiments in accordance with the present invention 1；
Fig. 2 is the SEM pictures of the tertiary cathode material of embodiments in accordance with the present invention 1；
Fig. 3 is the XRD piece of the tertiary cathode material of embodiments in accordance with the present invention 2；
Fig. 4 is the SEM pictures of the tertiary cathode material of embodiments in accordance with the present invention 2.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to describing embodiments of the invention in detail.However, it is possible to come real in many different forms
Apply the present invention, and the present invention should not be construed as limited to the specific embodiment that illustrates here.Conversely, there is provided these implementations
Example is in order to explain principle of the invention and its practical application, so that others skilled in the art are it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
The invention provides a kind of preparation method of the tertiary cathode material suitable for lithium ion battery, including following steps
Suddenly：
Step S1, water-soluble lithium salts is mixed and dissolved with water-soluble transition metal salt, obtain mixed solution.
In this application, pre-prepared tertiary cathode material is LiNixCo1-x-yMnyO2(the ＜ y ＜ 1 of 0 ＜ x ＜ 1,0), therefore
Water-soluble transition metal salt is the mixture of water soluble nickel salt, water soluble cobaltous salt and water-soluble manganese salt herein, meanwhile, it is water-soluble
Anion in lithium salts, water soluble nickel salt, water soluble cobaltous salt and water-soluble manganese salt may be selected from Cl-、NO3 -、SO4 2-、CH3COO-
In at least one.
Specifically, water soluble nickel salt, water soluble cobaltous salt, water-soluble manganese salt are x according to the ratio between the amount of material:1-x-y:Y enters
Row mixing, while the ratio between amount of material of water-soluble lithium salts and water-soluble transition metal salt is 0.7:1~1.1:1.
It is water or alcohol or the mixing liquid of the two for dissolving water-soluble lithium salts with the solvent of water-soluble transition metal salt.
Preferably, combustion adjuvant is also included in mixed solution, combustion adjuvant is preferably triethanolamine；When using triethanolamine as helping
During combustion agent, on the one hand can promote follow-up burning, it is ensured that the heat energy of burning allows the final tertiary cathode material for obtaining with more
Good crystallinity, so that product particles are smaller, is conducive to improving the specific surface area of product；Another aspect triethanolamine or one kind
Chelating agent, can chelate the Ni in mixed solution2+、Co2+、Mn2+, so that transition in the final tertiary cathode material product for obtaining
Metal Distribution is more uniform, is conducive to the raising of product chemical property.
Specifically, when mixed solution includes combustion adjuvant, the ratio between amount of material of control combustion adjuvant and water-soluble lithium salts
More than 1:1.
Step S2, heating mixed solution, so that mixed solution evaporates and triggers burning, obtain presoma.
Specifically, to mixed solution heating evaporation first, when moisture therein nearly all pervaporation run out of it is full-time, this
When mixed solution can become sticky spawn, continuation is heated to it and can smoldered, and can be kept the state of smoldering or be used naked light
It is ignited, through different degrees of burning, obtains presoma.
Step S3, presoma is carried out to carry out high-temperature roasting after low temperature presintering again, obtain tertiary cathode material.
Specifically, presoma is carried out into attrition grinding first, then carried out at 450 DEG C~550 DEG C low temperature presintering 1h~
3h, then high-temperature roasting 8h~24h is carried out at 850 DEG C~950 DEG C.
With water soluble nickel salt as four water nickel acetates, water soluble cobaltous salt be four water cobalt acetates, water-soluble manganese salt be four water acetic acid
Manganese, water-soluble lithium salts are for as a example by lithium nitrate, its chemical reaction is as shown in formula (1)：
xNi(CH3COO)2·4H2O+yMn(CH3COO)2·4H2O+(1-x-y)Co(CH3COO)2·4H2O+LiNO3→
LiNixCo1-x-yMnyO2+CO2↑+H2O↑+NO2↑ (1)
More specifically, after after presoma cooling, presoma is placed in vibrator and is ground, abrasive media ball
The middle ball of big ball, a diameter of 1cm including a diameter of 2cm and be directly the bead of 0.7cm, and control big ball, middle ball, small
Three kinds of mass ratios of medium ball of ball are 2:3:1；15min is ground in the case where vibration frequency is 1500 times/min.
Preferably, low temperature presintering and high-temperature roasting are carried out to presoma can be carried out in the high temperature furnaces such as Muffle furnace, typically
It is preferred that corundum crucible is contained by the presoma of attrition grinding.
Hereinafter above-mentioned preparation method of the invention will be embodied by specific embodiment；In order to contrast in each embodiment not
Same condition, lists the conditional parameter of embodiment 1-5 in table form；Meanwhile, the tertiary cathode material obtained to each embodiment
The first discharge specific capacity of material is tested, and is listed in table 1.
Although it will be appreciated that can be used term " first ", " second " etc. to describe various proportionate relationships herein,
These proportionate relationships should not be limited by these terms.These terms are only used for a proportionate relationship and another proportionate relationship
Make a distinction.
The conditional parameter and performance comparison of the embodiment 1-5 of table 1
X-ray diffraction test (abbreviation XRD) has been carried out to the tertiary cathode material that embodiment 1 and embodiment 2 are obtained respectively
With sem test (abbreviation SEM), difference is as Figure 1-Figure 4.As can be seen that embodiment 1 and implementation from Fig. 1 and Fig. 3
Diffractive features peak in two tertiary cathode material samples that example 2 is obtained can belong to the α-NaFeO in space group R-3m2
Type layer structure.Diffraction locations and document report (Chung-Hsin Lu, Yu-Kai Lin.Microemulsion
preparation and electrochemical characteristics of LiNi1/3Co1/3Mn1/3O2powders
[J].Journal of Power Sources,2009,189(1):40-44) match, diffraction maximum is more sharp, illustrate crystallization
Degree is preferable.(006)/(012) and the peak division of (108)/(110) two pairs are larger, it was demonstrated that the layer structure that material has had.According to
XRD data calculate two cell parameters of tertiary cathode material sample that embodiment 1 and embodiment 2 are obtained, two samples
C/a values are larger, and c/a values higher are represented has more preferable six sides layer structure.I003/I104 shows Li in tertiary cathode material
With the mixing degree of Ni, I003/I104 is bigger, and mixing is fewer, and the I003/I104 of two samples is more than 1.4, I003/I104
>Illustrate that mixing degree is very low when 1.2.Figure it is seen that grain diameter is 1 μm or so of submicron order, in irregular many
Face body and ball shape structure, surface are smooth；Figure 4, it is seen that particle is 2 μm or so the micro particles of particle diameter, in irregular
Polyhedral structure, surface is smooth, there is caking agglomeration；Tertiary cathode material sample in comparison diagram 2 and Fig. 4, Fig. 2 has
Smaller grain diameter, caking agglomeration is less, and this is to add triethanolamine, triethanolamine in raw material due to embodiment 1
And acetate is during heat resolve, carbon dioxide, vapor are produced, while triethanolamine decomposes the heat for producing inhibiting
The reunion of grain and become big, smaller particle and bigger specific surface area, with more preferable electrolyte effect of impregnation.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where the spirit and scope of the present invention limited by claim and its equivalent are not departed from, can carry out herein form and
Various change in details.
Claims (10)
1. a kind of preparation method of tertiary cathode material, it is characterised in that including step：
A, water-soluble lithium salts is mixed and dissolved with water-soluble transition metal salt, obtain mixed solution；
B, the heating mixed solution, so that the mixed solution evaporates and triggers burning, obtain presoma；
C, the presoma is carried out to carry out high-temperature roasting after low temperature presintering again, obtain tertiary cathode material.
2. preparation method according to claim 1, it is characterised in that in the step A, also wrapped in the mixed solution
Include combustion adjuvant.
3. preparation method according to claim 2, it is characterised in that the combustion adjuvant is triethanolamine.
4. preparation method according to claim 2, it is characterised in that the material of the combustion adjuvant and the water-soluble lithium salts
The ratio between amount be more than 1:1.
5. preparation method according to claim 1, it is characterised in that the cation of the water-soluble transition metal salt is Ni2 +、Co2+、Mn2+, anion is selected from Cl-、NO3 -、SO4 2-、CH3COO-In at least one.
6. preparation method according to claim 5, it is characterised in that in the water-soluble transition metal salt, Ni2+、Co2+
And Mn2+The ratio between the amount of material be x:1-x-y:y；Wherein, the ＜ y ＜ 1 of 0 ＜ x ＜ 1,0.
7. preparation method according to claim 1, it is characterised in that the anion of the water-soluble lithium salts is selected from Cl-、
NO3 -、SO4 2-、CH3COO-In at least one.
8. according to any described preparation method in claim 1,5,6 or 7, it is characterised in that the water-soluble lithium salts with it is described
The ratio between amount of material of water-soluble transition metal salt is 0.7:1~1.1:1.
9. preparation method according to claim 1, it is characterised in that in the step C, the temperature of the low temperature presintering
It it is 450 DEG C~550 DEG C, the time is 1h~3h；The temperature of the high-temperature roasting is 850 DEG C~950 DEG C, and the time is 8h~24h.
10. preparation method according to claim 1, it is characterised in that described water-soluble for dissolving in the step A
Property lithium salts and the water-soluble transition metal salt solvent be water and/or alcohol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110112410A (en) * | 2019-05-29 | 2019-08-09 | 新乡学院 | A kind of modification lithium-ion battery anode material and preparation method thereof |
| CN112467101A (en) * | 2020-11-04 | 2021-03-09 | 双登集团股份有限公司 | Ternary lithium ion storage battery positive electrode material and preparation method thereof |
| CN115000380A (en) * | 2022-06-27 | 2022-09-02 | 中国科学院青海盐湖研究所 | High nickel ternary positive electrode material, CeO 2 Self-coated high-nickel ternary positive electrode material and preparation method thereof |
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| CN110112410A (en) * | 2019-05-29 | 2019-08-09 | 新乡学院 | A kind of modification lithium-ion battery anode material and preparation method thereof |
| CN112467101A (en) * | 2020-11-04 | 2021-03-09 | 双登集团股份有限公司 | Ternary lithium ion storage battery positive electrode material and preparation method thereof |
| CN115000380A (en) * | 2022-06-27 | 2022-09-02 | 中国科学院青海盐湖研究所 | High nickel ternary positive electrode material, CeO 2 Self-coated high-nickel ternary positive electrode material and preparation method thereof |
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Application publication date: 20170531 |