CN106981654A - A kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped - Google Patents
A kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped Download PDFInfo
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- CN106981654A CN106981654A CN201710206123.4A CN201710206123A CN106981654A CN 106981654 A CN106981654 A CN 106981654A CN 201710206123 A CN201710206123 A CN 201710206123A CN 106981654 A CN106981654 A CN 106981654A
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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
- 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
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- 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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- 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
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Abstract
The present invention relates to a kind of preparation method for synthesizing high-voltage lithium-battery cathode material hollow ball shape nickel ion doped, belong to chemical cell technical field, it is by manganese source of hydrated manganese sulfate, nickel sulfate hexahydrate is nickel source, using ammonium hydrogen carbonate as precipitating reagent, hollow ball shape nickel manganese presoma is obtained using coprecipitation method synthesis, stir, dry after presoma is mixed with soluble lithium salt solution, by mixture sintering, obtain the LNMO positive electrodes of a diameter of 600 2000nm hollow ball shape.Present invention process is simple and convenient to operate, environment-friendly, and raw material sources enrich, it is easy to mass production.
Description
Technical field
The present invention relates to a kind of preparation method of anode active material of lithium ion battery hollow ball shape nickel ion doped.Belong to lithium
Ion battery technology field.
Background technology
Nickel ion doped LiNi0.5Mn1.5O4It is on the Research foundation of LiMn2O4, to be taken by Ni parts for spinel structure
A kind of electrode material developed for Mn, as the positive electrode of lithium ion battery, it has 4.7V high voltages, three-dimensional lithium ion
Transmission channel, up to 650Wh/kg energy densities make it be paid close attention to by numerous researchers, it is considered to be following lithium-ion electric
Most one of positive electrode of future and attraction in the development of pond.But LiNi0.5Mn1.5O4Do positive electrode and still suffer from deficiency, than
Such as there is very important capacity fade problem in cyclic process at 55 DEG C of temperature ＞, working can send out under high voltages with electrolyte
Raw serious side reaction, causes structure and chemical stability to be deteriorated, causes capacity attenuation.Which has limited LiNi0.5Mn1.5O4Material
Commercialized development.
The discovery of comprehensive numerous researchers understands that the preparation method and pattern of spinel-type nickel ion doped material are to composition
The Electrochemical Performances of battery are very big.Current nickel ion doped preparation method mainly has high temperature solid-state method, coprecipitation etc. a variety of
Method.High temperature solid-state method in actual production due to the advantages of method is simple and convenient to operate, being used widely, but high temperature is solid
Phase method is because of the inhomogeneities of batch mixing, and the material particle size of formation is big and uneven；And persursor material is prepared with coprecipitation,
After presoma is mixed with lithium source again nickel ion doped material is prepared by special high-temperature heat treatment mode.This method particle diameter
It is homogeneous, and this method easily realization in large-scale production.In addition, spherical structure has density high, the big grade of specific surface area is dashed forward
Go out feature, be conducive to preparing the good cell positive material of long lifespan, performance.
In numerous open methods, it is most using hydrothermal reaction kettle come the material of synthesizing spherical, but hydrothermal reaction kettle yield
It is relatively low, it is unfavorable for large-scale production.In the method for persursor material is prepared with coprecipitation, most researchers are with hydroxide
Thing, organic salt or polymer assistance etc. make precipitating reagent and prepare presoma in the middle of mixing, although synthetic material performance is compared with other method
It is significantly improved, but raw material are complicated, and synthesis technique is cumbersome, is unfavorable for large-scale production.In addition, spherical nickel-lithium manganate
Preparation method is more, and such as a kind of preparation method of the spherical high-voltage lithium nickel manganate anode materials of CN 103066275 is using co-precipitation
Method prepares presoma, and two-step sintering prepares spherical nickel-lithium manganate, but this method need to use poisonous hydrazine hydrate, and two-step sintering
Between need to cool down, crush, technique is relatively complicated, and product is solid spherical or class ball-type.A kind of spherical nickels of CN 103579607
The preparation method of manganate cathode material for lithium is relatively simple, but product is using spherical mangano-manganic oxide as template, and generation is medicine ball
Shape or class ball-type.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped
Preparation method.The preparation method is simple and environmentally-friendly without using hydrothermal reaction kettle, it is easy to accomplish large-scale production.
The technical solution adopted by the present invention is：
A kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped, it comprises the following steps：
(1) by MnSO4•H2O、NiSO4•6H2O is scattered in organic solvent, stirs 30-90min, obtains the scattered of nickel manganese salt
Liquid；
(2) carbonate is distributed in deionized water, stirs 10-30min, obtain carbonate solution；
(3) carbonate solution is slowly dropped in the dispersion liquid of nickel manganese salt, persistently stirs 30-120min, obtain grass green nickel
The carbonate deposition of manganese；
(4) will（3）The precipitation of gained carries out filtration washing, collects sediment, and drying precipitate is handled；
(5) dried precipitation and soluble lithium salt solution are stirred, are evaporated；Milled after drying, wait to mill uniformly
After be sintered, obtain hollow ball shape lithium ion anode material nickel ion doped.
It is currently preferred, step（1）Described in organic solvent for absolute ethyl alcohol and deionized water mixed liquor, it is anhydrous
Volume fraction >=50% of ethanol, the concentration of manganese salt is 0.075-0.1875mol/L, and the concentration of nickel salt is 0.025-
0.0625mol/L。
Currently preferred, the carbonate described in step (2) is ammonium hydrogen carbonate, and ammonium bicarbonate concentration is 2.5 × 10-4~
6.25×10-4mol/L。
Currently preferred, detergent is deionized water and absolute ethyl alcohol in step (4), is cleaned 3-5 times.
Currently preferred, drying process temperature is 50-80 DEG C in step (4), and drying time is 4-8h.
Currently preferred, soluble lithium salt described in step (5) is Li2CO3、CH3COOLi, LiCl or LiOH H2O。
Currently preferred, soluble lithium salt solution described in step (5) is molten for the aqueous solution or ethanol of soluble lithium salt
Liquid, the concentration of soluble lithium salt is 0.0525-0.131mol/L.
Currently preferred, sintering processes are divided into two sections in step (5), and the temperature of first paragraph is 400-500 DEG C, during sintering
Between be 2-5h, be warming up to afterwards at 600-1000 DEG C and sinter 8-15h, room temperature is down to naturally.
The high-voltage lithium-battery cathode material hollow ball shape nickel ion doped prepared according to above technical scheme is spinel-type
Crystal structure（PDF#80-2162）, correspondence cell parameter is a=8.173, b=8.173, c=8.173.
Hollow ball surface is in flakey, and scale size is less than or equal to 200nm, and hollow ball outer dia is 600-2000nm,
Inside diameter is 400-1800nm.
Beneficial effects of the present invention are as follows：
The present invention is prepared for high-voltage lithium-battery cathode material hollow ball shape nickel ion doped using simple method, obtains nanometer sheet
Layer tiny balloon, simple with synthetic method, raw material sources enrich, and cost is low, the advantages of being adapted to large-scale industrial production.Will
Its as lithium ion battery positive electrode, with higher specific discharge capacity, good cyclical stability.While hollow ball shape
Material structure be conducive to fully contacting for electrolyte and electrode material, shorten the diffusion length of lithium ion, improve material
Specific capacity and high rate performance.
Brief description of the drawings
Fig. 1 is the XRD diffraction patterns according to the gained hollow ball nickel ion doped sample of the embodiment of the present invention 1；
Fig. 2 is the stereoscan photograph according to the gained hollow ball nickel ion doped sample of the embodiment of the present invention 1.
Embodiment
With reference to specific embodiment, the present invention is described in more detail.These embodiments are merely to illustrate the present invention,
But it is not limited to the scope of the present invention.In addition, after specific embodiment set forth in the present invention has been read, those skilled in the art can
To make an amendment and change to the present invention, but these equivalent form of values are equally belonged in the application patent book limited range.
Manganese sulfate, nickel sulfate are commercial products, purchased from Tianjin BASF Chemical Co., Ltd..
Embodiment 1
A kind of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped, preparation process is as follows：
（1）By 3.375mmol manganese sulfates, 1.125mmol nickel sulfates be uniformly scattered in 30ml absolute ethyl alcohols and 60ml go from
In sub- water mixed liquid, 50min is stirred, the dispersion liquid of manganese sulfate nickel is obtained；
（2）225mmol ammonium hydrogen carbonate is uniformly scattered in 60ml deionized waters, 30min is stirred, obtains ammonium hydrogen carbonate molten
Liquid；
（3）Will（2）The ammonium bicarbonate soln of system is slowly dropped to（1）Mixed liquor in, continue stir 60min, obtain grass green
The nickel manganese carbonate deposition of color；
（4）Above-mentioned precipitation is subjected to suction filtration, and washed 3 times with deionized water and absolute ethyl alcohol repeatedly, collects and is done at precipitation, 60 DEG C
Dry 5h；
（5）2.362mmol lithium hydroxides are dissolved in deionized water, dried precipitation and lithium hydroxide solution are stirred
After 30min, it is warming up to 80 DEG C and continues to stir, untill moisture evaporation is finished, be placed in afterwards in air dry oven and carry out air blast
Dry；
（6）Dried mixture is warming up to 400 DEG C with 3 DEG C/min heating rate by room temperature, 3h is sintered, afterwards with 3
DEG C/min heating rate to 800 DEG C, after sintering 10h, naturally cool to room temperature, obtain hollow ball shape nickel ion doped.
Fig. 1 is the XRD spectrum of the hollow ball shape nickel ion doped prepared according to the embodiment of the present invention 1.As shown in Figure 1, it is made
Standby product is spinel type crystal structure（JCPDS#80-2162）, corresponding cell parameter is a=8.147, b=8.147, c
=8.147, occur without other miscellaneous peaks, show to prepare for pure phase nickel lithium manganate cathode material.
Fig. 2 is the stereoscan photograph according to the products therefrom of embodiment 1, and material is uniform hollow ball as can be seen from Figure
Shape structure.
Embodiment 2
A kind of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped, preparation process is as follows：
（1）Be the same as Example 1
（2）Be the same as Example 1
（3）Be the same as Example 1
（4）Be the same as Example 1
（5）1.181mmol lithium carbonate is dissolved in absolute ethyl alcohol, dried precipitation and Lithium carbonate solution are stirred into 30min
Afterwards, 50 DEG C of continuation stirring is warming up to, untill ethanol volatilization is finished, is placed in afterwards in air dry oven and carries out forced air drying；
（6）Dried mixture is warming up to 400 DEG C with 3 DEG C/min heating rate by room temperature, 3h is sintered, afterwards with 3
DEG C/min heating rate to 700 DEG C, after sintering 8h, naturally cool to room temperature.Obtain hollow ball shape nickel ion doped.
Hollow ball shape nickel ion doped prepared by this method is used as anode material for lithium-ion batteries, and specific energy is high,
Specific surface area is big, effectively increases the electrochemistry cyclic reversibility and stability of lithium ion battery.
Embodiment 3
A kind of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped, preparation process is as follows：
（1）2.25mmol manganese sulfates, 0.75mmol nickel sulfates are uniformly scattered in 10ml absolute ethyl alcohols and 20ml deionizations
In water mixed liquid, 40min is stirred, the dispersion liquid of manganese sulfate nickel is obtained；
（2）15mmol ammonium hydrogen carbonate is uniformly scattered in 20ml deionized waters, 30min is stirred, obtains ammonium bicarbonate soln；
（3）Be the same as Example 1；
（4）Be the same as Example 1；
（5）1.575mmol lithium acetate is dissolved in deionized water, dried precipitation and lithium acetate solution are stirred into 50min
Afterwards, 70 DEG C of continuation stirring is warming up to, untill moisture evaporation is finished, is placed in afterwards in air dry oven and carries out forced air drying；
（6）Dried mixture is warming up to 500 DEG C with 3 DEG C/min heating rate by room temperature, 3h is sintered, afterwards with 3
DEG C/min heating rate to 900 DEG C, after sintering 8h, naturally cool to temperature.Obtain hollow ball shape nickel ion doped.
Hollow ball shape nickel ion doped prepared by this method is used as anode material for lithium-ion batteries, and specific energy is high,
Specific surface area is big, effectively increases the electrochemistry cyclic reversibility and stability of lithium ion battery.
Claims (7)
1. a kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped, it is characterised in that：Including following
Step：
(1) by MnSO4•H2O、NiSO4•6H2O is scattered in organic solvent, stirs 30-90min, obtains the scattered of nickel manganese salt
Liquid；
(2) carbonate is distributed in deionized water, stirs 10-30min, obtain carbonate solution；
(3) carbonate solution is slowly dropped in the dispersion liquid of nickel manganese salt, persistently stirs 30-120min, obtain grass green nickel
The carbonate deposition of manganese；
(4) will（3）The precipitation of gained carries out filtration washing, collects sediment, and drying precipitate is handled；
(5) dried precipitation and soluble lithium salt solution are stirred, are evaporated；Milled after drying, wait to mill uniformly
After be sintered, obtain hollow ball shape lithium ion anode material nickel ion doped.
2. a kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped according to claim 1,
It is characterised by, step（1）Described in organic solvent be the mixed liquor of absolute ethyl alcohol and deionized water, the volume integral of absolute ethyl alcohol
Number >=50%, the concentration of manganese salt is 0.075-0.1875mol/L, and the concentration of nickel salt is 0.025-0.0625mol/L.
3. a kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped according to claim 1,
Characterized in that, the carbonate described in step (2) is preferably to be ammonium hydrogen carbonate, ammonium bicarbonate concentration is 2.5 × 10-4~6.25
×10-4mol/L。
4. a kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped according to claim 1,
Characterized in that, detergent is deionized water and absolute ethyl alcohol in step (4), clean 3-5 times；Drying process temperature is 50-80
DEG C, drying time is 4-8h.
5. a kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped according to claim 1,
Characterized in that, soluble lithium salt described in step (5) is Li2CO3、CH3COOLi, LiCl or LiOH H2O。
6. a kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped according to claim 1,
Characterized in that, soluble lithium salt solution described in step (5) is the aqueous solution or ethanol solution of soluble lithium salt, soluble lithium
The concentration of salt is 0.0525-0.131mol/L.
7. a kind of preparation method of high-voltage lithium-battery cathode material hollow ball shape nickel ion doped according to claim 1,
Characterized in that, sintering processes described in step (5) are divided into two sections, the temperature of first paragraph is 400-500 DEG C, and sintering time is
2-5h, is warming up under 600-1000 ° and sinters 8-15h, room temperature is down to naturally afterwards.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108649217A (en) * | 2018-05-09 | 2018-10-12 | 哈尔滨工业大学（威海） | A kind of preparation method of high-voltage lithium-battery cathode material bat mixing nickel ion doped |
| CN108847476A (en) * | 2018-06-07 | 2018-11-20 | 哈尔滨工业大学（威海） | Preparation method of zinc ion battery anode |
| CN108987743A (en) * | 2018-09-04 | 2018-12-11 | 江南大学 | Ternary cathode material of lithium ion battery and preparation method thereof with hollow structure |
| CN109686972A (en) * | 2018-12-12 | 2019-04-26 | 无锡晶石新型能源股份有限公司 | A kind of preparation method of high magnification hollow sphere lithium nickelate positive electrode |
| CN111434616A (en) * | 2019-12-26 | 2020-07-21 | 蜂巢能源科技有限公司 | Hollow structure carbonate binary precursor and preparation method and application thereof |
| CN111613788A (en) * | 2020-06-05 | 2020-09-01 | 哈尔滨工业大学（威海） | Hollow spherical lithium nickel manganese oxide positive electrode material and preparation method thereof |
| CN113809301A (en) * | 2021-09-17 | 2021-12-17 | 中国海洋大学 | High-voltage nitrogen-doped nickel lithium manganate electrode material with yolk structure and lithium storage application thereof |
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| CN103413929A (en) * | 2013-07-30 | 2013-11-27 | 南京航空航天大学 | Preparation method for spherical Ni1/4Mn3/4CO3 precursor and LiNi0.5Mn1.5O4 |
| CN103474650A (en) * | 2013-10-11 | 2013-12-25 | 哈尔滨工业大学 | Method for preparing hollow high voltage nickel manganese acid lithium anode material |
| CN105428628A (en) * | 2015-12-28 | 2016-03-23 | 安徽工业大学 | Preparation method of porous spherical high-voltage lithium ion battery positive electrode material |
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| CN103413929A (en) * | 2013-07-30 | 2013-11-27 | 南京航空航天大学 | Preparation method for spherical Ni1/4Mn3/4CO3 precursor and LiNi0.5Mn1.5O4 |
| CN103474650A (en) * | 2013-10-11 | 2013-12-25 | 哈尔滨工业大学 | Method for preparing hollow high voltage nickel manganese acid lithium anode material |
| CN105428628A (en) * | 2015-12-28 | 2016-03-23 | 安徽工业大学 | Preparation method of porous spherical high-voltage lithium ion battery positive electrode material |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108649217A (en) * | 2018-05-09 | 2018-10-12 | 哈尔滨工业大学（威海） | A kind of preparation method of high-voltage lithium-battery cathode material bat mixing nickel ion doped |
| CN108649217B (en) * | 2018-05-09 | 2021-09-28 | 哈尔滨工业大学（威海） | Preparation method of high-voltage lithium battery anode material bat mixed lithium nickel manganese oxide |
| CN108847476A (en) * | 2018-06-07 | 2018-11-20 | 哈尔滨工业大学（威海） | Preparation method of zinc ion battery anode |
| CN108987743A (en) * | 2018-09-04 | 2018-12-11 | 江南大学 | Ternary cathode material of lithium ion battery and preparation method thereof with hollow structure |
| CN109686972A (en) * | 2018-12-12 | 2019-04-26 | 无锡晶石新型能源股份有限公司 | A kind of preparation method of high magnification hollow sphere lithium nickelate positive electrode |
| CN111434616A (en) * | 2019-12-26 | 2020-07-21 | 蜂巢能源科技有限公司 | Hollow structure carbonate binary precursor and preparation method and application thereof |
| CN111434616B (en) * | 2019-12-26 | 2022-12-20 | 蜂巢能源科技有限公司 | Hollow structure carbonate binary precursor and preparation method and application thereof |
| CN111613788A (en) * | 2020-06-05 | 2020-09-01 | 哈尔滨工业大学（威海） | Hollow spherical lithium nickel manganese oxide positive electrode material and preparation method thereof |
| CN113809301A (en) * | 2021-09-17 | 2021-12-17 | 中国海洋大学 | High-voltage nitrogen-doped nickel lithium manganate electrode material with yolk structure and lithium storage application thereof |
| CN113809301B (en) * | 2021-09-17 | 2023-03-10 | 中国海洋大学 | High-voltage nitrogen-doped nickel lithium manganate electrode material with yolk-like structure and lithium storage application thereof |
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