CN105932247A - Preparation method of nickel ferrite-coated lithium nickel manganese oxide positive electrode material - Google Patents
Preparation method of nickel ferrite-coated lithium nickel manganese oxide positive electrode material Download PDFInfo
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- 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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- 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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Abstract
The invention discloses a preparation method of a nickel ferrite-coated lithium nickel manganese oxide positive electrode material, and belongs to the technical field of preparation of lithium-ion battery materials. The preparation method of the positive electrode material comprises the following specific steps of: mixing the materials of a nickel salt, a manganese salt and a lithium salt to prepare a lithium nickel manganese oxide precursor through a sol-gel method; carrying out pre-sintering and high-temperature sintering to prepare the lithium nickel manganese oxide positive electrode material; dissolving selected nickel source and iron source into deionized water for in-situ deposition coating of lithium nickel manganese oxide; and finally carrying out high-temperature sintering to obtain the nickel ferrite-coated lithium nickel manganese oxide positive electrode material. Surface coating is carried out on the nickel ferrite-coated lithium nickel manganese oxide positive electrode material by nickel ferrite; direct contact of an electrolyte and the lithium nickel manganese oxide positive electrode material is reduced; the interface side reaction between the electrolyte and the lithium nickel manganese oxide is avoided; dissolution of manganese ions is reduced; and the stability of a spinel lithium nickel manganese oxide material structure is ensured, so that the cycle performance of the material is improved.
Description
[technical field]
The present invention relates to lithium ion battery material preparing technical field, be specifically related to a kind of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material
Preparation method.
[background technology]
Lithium ion battery is to be acknowledged as the most potential accumulation power supply at present, and the performance of lithium ion battery depends primarily on
Electrode material, wherein positive pole is as the reversible deintercalation of lithium ion time battery operated and the place of insertion, and therefore positive pole is to affect battery to hold
The key of amount, researching and developing high performance positive electrode the most just becomes the key point of current lithium ion battery development.At present,
The LiCoO of commercialization2Good cycle but specific capacity is low, price is high, environmental pollution is relatively big, this have impact on undoubtedly its
Industrial extensive application, therefore people more and more sight is tended to cheap, aboundresources, the manganese systems of excellent performance
Material, wherein spinel-type nickel ion doped (LiNi0.5Mn1.5O4) positive electrode be increasingly becoming people research focus.Although nickel manganese
Acid lithium has high working voltage (4.7V) and energy density can be up to 690Wh.Kg-1Etc. advantage, but in actual application,
Nickel ion doped there is also some problems.Especially in high voltage range, carbonate electrolyte is difficult to keep stable, electrode material and
Interfacial reaction between electrolyte will cause serious capacity attenuation.And material is in cyclic process, under electrolyte effect, material
In material, the dissolving of manganese will cause the loss of active material, accelerate material capacity decay.At present, both at home and abroad for nickel ion doped positive pole
The optimization of material processes, and is concentrated mainly on the improvement aspect of its combination property: (cladding) is modified on (1) surface；(2) doping.Grind
Study carefully discovery, at one layer of active material of nickel ion doped Surface coating, it is to avoid electrolyte directly contacts with nickel ion doped, effectively reduces
Some unnecessary interfacial reactions, reduce manganese and dissolve, it is ensured that the stability of spinel structure thus improve following of nickel ion doped
Ring performance.At present, study more nickel ion doped covering material and mainly have oxide, metal etc., such as ZnO, SiO2、MgO、
LaZO3、Al2O3、SnO2、ZrO2、FePO4, Ni etc., but the battery of the nickel ion doped of these claddings or doping preparation at present
Discharge performance is the most relatively unstable, fails to comply with the demand in market.And at present modification for nickel ion doped is also being inquired into further
In.
On the basis of these are coated with, the present invention intends by nickel ion doped material surface is coated with one layer of oxide nickel ferrite based magnetic loaded (NiFe2O4)。
Nickel ferrite based magnetic loaded clad, as the protective layer of nickel ion doped, can improve the cycle performance of nickel ion doped.
[summary of the invention]
It is an object of the invention to: for the problem of above-mentioned existence, it is provided that the system of a kind of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material
Preparation Method, described method is simple to operation, and the actual gram volume not only increasing nickel ion doped plays, and effectively reduces
The impedance of battery, improves the discharge platform voltage of the cycle life of nickel ion doped battery, capability retention and battery.
To achieve these goals, the technical solution used in the present invention is as follows:
The preparation method of a kind of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, comprises the following steps:
(1) weigh a certain amount of nickel salt, manganese salt and lithium salts and be dissolved in deionized water, add chelating agent, add in the water bath with thermostatic control of 80 DEG C
Thermal agitation, until generating dope, i.e. nickel ion doped presoma, the consumption of chelating agent is the 1～2.5% of the compound by weight of manganese；
(2), after the presoma of step (1) being dried, it is ground into powder and is crossed the standard screen of 100 mesh, the powder after then sieving
End is put into air atmosphere in Muffle furnace and is carried out pre-sintered 1～2h, and sintering temperature is 400～600 DEG C；
(3) being sintered at 800～1000 DEG C of air atmospheres by the pre-sintered product of step (2), temperature retention time is 2～10h, obtains nickel mangaic acid
Lithium anode material；
(4) weigh nickel salt and molysite that mol ratio is 1:2, be dissolved in nickel salt and molysite gross weight 5～the deionized water of 8 times, be dissolved in from
Sub-water, is stirred continuously formation homogeneous solution；
(5) regulating the pH value of solution toward addition buffer solution in step (4) is 8～10, at once adds nickel manganese produced above in solution
Acid lithium anode material is also stirred continuously, and obtains suspension mixed solution；
(6) take step (5) gained suspension mixed solution, after 80 ± 5 DEG C of oven dryings, be broken into powder, obtain nickel ferrite based magnetic loaded cladding nickel manganese
The presoma of acid lithium；
(7) by step 6) precursor powder for preparing, roasting 2～4h in 400～600 DEG C of air atmospheres, then use deionized water
Wash, filter, be dried, i.e. obtain the nickel lithium manganate cathode material of final required nickel ferrite based magnetic loaded cladding.
Further, the mole of described lithium salts and nickel salt and the ratio that ratio is 1:2, wherein nickel salt and manganese salt of manganese salt integral molar quantity
Example is a:(2-a), and 0 ＜ a≤1, nickel salt not can exceed that 1:1 with the ratio of manganese salt, and being primarily due to too much nickel salt can affect mangaic acid
The spinel structure of lithium, further results in the deterioration of cell properties of material.
Further, the nickel salt of described step (1) and step (4) is all the one in nickel nitrate, nickel acetate.
Further, in described step (1), the compound of manganese is the one in manganese acetate, manganese dioxide, manganese carbonate.
Further, the lithium salts in described step (1) is the mixture of one or more in lithium acetate, lithium carbonate, lithium citrate.
Further, the chelating agent in described step (1) is the mixture of one or more in oxalic acid, citric acid or gluconic acid,
Manganese ion in the compound of manganese is chelated by chelating agent, manganese ion can be avoided to precipitate, make each raw material the most anti-when heating water bath
Should.
Further, the buffer solution in described step (4) be concentration be 0.5～2mol/L ammonium hydrogen carbonate or ammoniacal liquor in one or two
The mixed solution planted, it is ensured that nickel ion doped is stable in the environment of alkalescence, it is to avoid the dissolving of nickel ion doped material, makes molysite and nickel
Salt is in the occupy-place of nickel ion doped surface, and the in-situ deposition for follow-up nickel ferrite based magnetic loaded provides carrier.
Further, the molysite in described step (4) is the one in ferric nitrate, ferrous oxalate.
Further, nickel ferrite based magnetic loaded consumption is nickel ion doped weight 2%～the 6% of described cladding nickel ion doped, too much nickel ferrite based magnetic loaded is anti-
And the performance of nickel ion doped material property can be affected, very few nickel ferrite based magnetic loaded is not enough to again be coated with nickel ion doped particle surface, therefore controls
The consumption of nickel ferrite based magnetic loaded processed can play the chemical property of nickel ion doped to greatest extent.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows:
(1) present invention uses nickel ferrite based magnetic loaded to be coated with nickel lithium manganate cathode material, is possible not only to improve positive electrode gram volume and plays, and
Can effectively reduce the impedance of battery, improve the discharge platform of the cycle life of nickel ion doped battery, capability retention and battery
Voltage.
(2) present invention is during preparing nickel ion doped, uses chelating agent can effectively prevent the manganese ion in manganese salt from sinking in the solution
Precipitation goes out, and makes the manganese ion can under solution state fully and other raw material reactions.
(3) present invention uses during preparation nickel ferrite based magnetic loaded cladding nickel ion doped, uses buffer solution that solution ph is adjusted to alkali
Property, it is ensured that nickel ion doped is stable in the environment of alkalescence, it is to avoid the dissolving of nickel ion doped material, makes molysite and nickel salt at nickel manganese
Acid lithium surface occupy-place, the in-situ deposition for follow-up nickel ferrite based magnetic loaded provides carrier.
(4) present invention effectively controls the content of nickel ferrite based magnetic loaded, improves the performance of the electrochemical energy energy of nickel ion doped to greatest extent.
[accompanying drawing explanation]
Fig. 1 is the XRD comparison diagram of the present invention and comparative example positive electrode.
Fig. 2 is the cyclic discharge capacity comparison diagram of the present invention and comparative example positive electrode.
Fig. 3 is the AC impedance figure of the present invention and comparative example positive electrode.
[detailed description of the invention]
Below by way of specific embodiment and verification the verifying results, the invention will be further described.
One, embodiment is made:
Embodiment 1
The preparation method of a kind of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, comprises the following steps:
(1) it is that 1:0.1:1.9 weighs a certain amount of lithium acetate, nickel acetate and manganese carbonate and is dissolved in deionized water according to mol ratio, adds grass
Acid, as chelating agent, adds thermal agitation in the water bath with thermostatic control of 80 DEG C, until generating dope, i.e. nickel ion doped presoma, oxalic acid
Consumption be 1.0%；
(2), after the presoma of step (1) being dried, it is ground into powder and is crossed the standard screen of 100 mesh, the powder after then sieving
End is put into air atmosphere in Muffle furnace and is carried out pre-sintered 1h, and sintering temperature is 400 DEG C；
(3) being sintered at 800 DEG C of air atmospheres by the pre-sintered product of step (2), temperature retention time is 10h, obtains nickel ion doped positive pole material
Material；
(4) weigh nickel acetate and ferrous oxalate that mol ratio is 1:2, be dissolved in nickel acetate and the deionization of ferrous oxalate gross weight 5 times
Water, is stirred continuously formation homogeneous solution；
(5) pH value regulating solution as buffer solution toward addition ammonium hydrogen carbonate in step (4) is 8, at once makes more than addition in solution
Nickel lithium manganate cathode material and be stirred continuously, obtain suspension mixed solution；
(6) take step (5) gained suspension mixed solution, after 75 DEG C of oven dryings, be broken into powder, obtain nickel ferrite based magnetic loaded cladding nickel mangaic acid
The presoma of lithium；
(7) precursor powder that step (6) is prepared, roasting 4h in 400 DEG C of air atmospheres, then carry out being washed with deionized,
Filter, be dried, i.e. obtain the nickel lithium manganate cathode material of final required nickel ferrite based magnetic loaded cladding.
Embodiment 2
The preparation method of a kind of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, comprises the following steps:
(1) it is that 1:1:1 weighs a certain amount of lithium carbonate, nickel nitrate and manganese carbonate and is dissolved in deionized water according to mol ratio, adds glucose
Acid, as chelating agent, adds thermal agitation in the water bath with thermostatic control of 80 DEG C, until generating dope, i.e. nickel ion doped presoma glucose
The 2.5% of the compound by weight that consumption is manganese of acid；
(2), after the presoma of step (1) being dried, it is ground into powder and is crossed the standard screen of 100 mesh, the powder after then sieving
End is put into air atmosphere in Muffle furnace and is carried out pre-sintered 2h, and sintering temperature is 600 DEG C；
(3) being sintered at 1000 DEG C of air atmospheres by the pre-sintered product of step (2), temperature retention time is 2h, obtains nickel ion doped positive pole material
Material；
(4) weigh nickel nitrate and ferric nitrate that mol ratio is 1:2, be dissolved in nickel nitrate and the deionized water of ferric nitrate gross weight 8 times,
It is stirred continuously formation homogeneous solution；
(5) it is 10 toward step (4) adding ammoniacal liquor as the pH value of buffer solution regulation solution, at once produced above toward solution adds
Nickel lithium manganate cathode material and be stirred continuously, obtain suspension mixed solution；
(6) take step (5) gained suspension mixed solution, after 85 DEG C of oven dryings, be broken into powder, obtain nickel ferrite based magnetic loaded cladding nickel mangaic acid
The presoma of lithium；
(7) precursor powder that step (6) is prepared, roasting 2h in 600 DEG C of air atmospheres, then carry out being washed with deionized,
Filter, be dried, i.e. obtain the nickel lithium manganate cathode material of final required nickel ferrite based magnetic loaded cladding.
Embodiment 3
The preparation method of a kind of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, comprises the following steps:
(1) it is that 1:0.5:1.5 weighs a certain amount of lithium citrate, nickel nitrate and manganese dioxide and is dissolved in deionized water according to mol ratio, adds
Enter gluconic acid as chelating agent, in the water bath with thermostatic control of 80 DEG C, add thermal agitation, until generating dope, i.e. nickel ion doped forerunner
Body, the consumption of gluconic acid is the 1～2.5% of the compound by weight of manganese；
(2), after the presoma of step (1) being dried, it is ground into powder and is crossed the standard screen of 100 mesh, the powder after then sieving
End is put into air atmosphere in Muffle furnace and is carried out pre-sintered 1.5h, and sintering temperature is 500 DEG C；
(3) being sintered at 900 DEG C of air atmospheres by the pre-sintered product of step (2), temperature retention time is 6h, obtains nickel ion doped positive pole material
Material；
(4) weigh nickel nitrate and ferric nitrate that mol ratio is 1:2, be dissolved in nickel nitrate and the deionized water of ferric nitrate gross weight 6.5 times,
It is stirred continuously formation homogeneous solution；
(5) it is 9 toward step (4) adding ammoniacal liquor as the pH value of buffer solution regulation solution, at once produced above toward solution adds
Nickel lithium manganate cathode material is also stirred continuously, and obtains suspension mixed solution；
(6) take step (5) gained suspension mixed solution, after 80 DEG C of oven dryings, be broken into powder, obtain nickel ferrite based magnetic loaded cladding nickel mangaic acid
The presoma of lithium；
(7) precursor powder that step (6) is prepared, roasting 3h in 500 DEG C of air atmospheres, then carry out being washed with deionized,
Filter, be dried, i.e. obtain the nickel lithium manganate cathode material of final required nickel ferrite based magnetic loaded cladding.
Two, compliance test result:
The preparation method of comparative example: the nickel ion doped positive pole material prepared according to step (1)～the step (3) of the embodiment of the present invention 3
Material.
The preparation method of the present invention: prepare nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material according to embodiment 1～embodiment 3.
For ease of the comparative analysis of comparative example Yu material of the present invention, other battery production methods, test equipment and and operating process equal
Unanimously, the results are shown in Table shown in 1 and Fig. 1～3 of concrete compliance test result.
Table 1 nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material and the chemical property comparative analysis of pure nickel LiMn2O4
| Gram volume mAh/g | Impedance/Ω | Cycle-index (1.0C) | Capability retention | Discharge voltage plateau/V | |
| Comparative example | 126 | 280 | 150 | 93.00% | 4.6～4.7 |
| Embodiment 1 | 128 | 150 | 150 | 97.00% | 4.7～4.8 |
| Embodiment 2 | 129 | 155 | 150 | 98.50% | 4.7～4.8 |
| Embodiment 3 | 128 | 162 | 150 | 97.60% | 4.7～4.8 |
As can be seen from Table 1: the electrochemical impedance of pure nickel LiMn2O4 is big, and capability retention is low, and gram volume plays and compares
Difference；And nickel ion doped Surface coating nickel ferrite based magnetic loaded of the present invention, the conductance on the surface that can be effectively increased positive electrode reduces battery
Impedance, improves the performance to greatest extent of material gram volume simultaneously, and after circulation 150 weeks, capability retention is also than pure nickel
LiMn2O4 improves 4～6%, therefore can be greatly promoted the material electrification of nickel ion doped in the nickel ferrite based magnetic loaded that nickel ion doped Surface coating is appropriate
Learn performance.
Claims (9)
1. the preparation method of a nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: comprise the following steps:
(1) weigh nickel salt, the compound of manganese and lithium salts and be dissolved in deionized water, add chelating agent, heat in the water bath with thermostatic control of 80 DEG C
Stirring, until generating dope, i.e. nickel ion doped presoma, the consumption of chelating agent is the 1～2.5% of the compound by weight of manganese；
(2), after the presoma of step (1) being dried, it is ground into powder and is crossed the standard screen of 100 mesh, the powder after then sieving
End is put into air atmosphere in Muffle furnace and is carried out pre-sintered 1～2h, and sintering temperature is 400～600 DEG C；
(3) being sintered at 800～1000 DEG C of air atmospheres by the pre-sintered product of step (2), temperature retention time is 2～10h, obtains nickel mangaic acid
Lithium anode material；
(4) weigh nickel salt and molysite that mol ratio is 1:2, be dissolved in nickel salt and molysite gross weight 5～the deionized water of 8 times, be stirred continuously
Form homogeneous solution；
(5) regulating the pH value of solution toward addition buffer solution in the solution in step (4) is 8～10, at once makes more than addition in solution
Nickel lithium manganate cathode material and be stirred continuously, obtain suspension mixed solution；
(6) step 5 is taken) gained suspension mixed solution, after 80 ± 5 DEG C of oven dryings, it is broken into powder, obtains nickel ferrite based magnetic loaded cladding nickel manganese
The presoma of acid lithium；
(7) by step 6) precursor powder for preparing, roasting 2～4h in 400～600 DEG C of air atmospheres, then use deionized water
Wash, filter, be dried, i.e. obtain the nickel lithium manganate cathode material of final required nickel ferrite based magnetic loaded cladding.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
Stating the ratio of the mole of lithium salts and nickel salt and manganese salt integral molar quantity in step (1) is 1:2, wherein nickel salt and the mol ratio of manganese salt
Example is a:(2-a), and 0 ＜ a≤1.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
The nickel salt stating step (1) and step (4) is all the one in nickel nitrate, nickel acetate.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
Stating the compound of manganese in step (1) is the one in manganese acetate, manganese dioxide, manganese carbonate.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
Stating the lithium salts in step (1) is the mixture of one or more in lithium acetate, lithium carbonate, lithium citrate.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
Stating the chelating agent in step (1) is the mixture of one or more in oxalic acid, citric acid or gluconic acid.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
State the buffer solution in step (4) be concentration be 0.5～2mol/L ammonium hydrogen carbonate or ammoniacal liquor in one or both mixed solution.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
Stating the molysite in step (4) is the one in ferric nitrate, ferrous oxalate.
A kind of preparation method of nickel ferrite based magnetic loaded cladding nickel lithium manganate cathode material, it is characterised in that: institute
State nickel ferrite based magnetic loaded consumption is nickel ion doped weight 2%～the 6% of cladding nickel ion doped.
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| CN109950496A (en) * | 2019-03-29 | 2019-06-28 | 荆门市格林美新材料有限公司 | Nickel cobalt lithium aluminate tertiary cathode material and preparation method are covered in a kind of double-contracting |
| CN110112387A (en) * | 2019-05-07 | 2019-08-09 | 湖南金富力新能源股份有限公司 | A kind of positive electrode and preparation method thereof that Asia titanium-oxide-coated is modified |
| CN110247039A (en) * | 2019-06-17 | 2019-09-17 | 启东启澳新材料科技发展有限公司 | A kind of nickel lithium manganate cathode material preparation method coating strontium titanate base conductive coating |
| CN111883749A (en) * | 2020-06-29 | 2020-11-03 | 安徽南都华铂新材料科技有限公司 | Method for preparing transition metal oxide composite electrode for lithium battery |
| CN112838208A (en) * | 2021-01-09 | 2021-05-25 | 厦门厦钨新能源材料股份有限公司 | Preparation method and application of lithium ion battery anode material |
| CN114314546A (en) * | 2021-12-21 | 2022-04-12 | 万向一二三股份公司 | Phosphate anode material and preparation method thereof |
| EP3984959A1 (en) * | 2020-10-16 | 2022-04-20 | Prime Planet Energy & Solutions, Inc. | Positive electrode active material and secondary battery provided with positive electrode active material |
| CN114824267A (en) * | 2022-03-29 | 2022-07-29 | 蜂巢能源科技股份有限公司 | Layered lithium nickel manganese oxide positive electrode material and preparation method and application thereof |
| CN117466346A (en) * | 2023-12-28 | 2024-01-30 | 深圳中芯能科技有限公司 | Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
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| CN114314546A (en) * | 2021-12-21 | 2022-04-12 | 万向一二三股份公司 | Phosphate anode material and preparation method thereof |
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