CN106910878A - A kind of spherical 5V spinel nickels lithium manganate material and preparation method thereof - Google Patents
A kind of spherical 5V spinel nickels lithium manganate material and preparation method thereof Download PDFInfo
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- CN106910878A CN106910878A CN201710195004.3A CN201710195004A CN106910878A CN 106910878 A CN106910878 A CN 106910878A CN 201710195004 A CN201710195004 A CN 201710195004A CN 106910878 A CN106910878 A CN 106910878A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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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- H—ELECTRICITY
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- 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
- H01M4/52—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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- 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
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- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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Abstract
The invention discloses a kind of preparation method of spherical 5V spinel nickels lithium manganate material, comprise the following steps：Lithium salts, nickel salt, manganese salt, binding agent are dissolved in deionized water, material I is obtained；Wherein, elemental mole ratios meet Li：Ni：Mn=(1~1.05)：0.5：1.5, the quality of binding agent is the 5~10% of lithium salts, nickel salt and manganese salt quality sum；By material I be spray-dried after in air atmosphere 800~900 DEG C next time be calcined 4~12h；Then product is stirred with acetate in ionized water；It is spray-dried again, in 450~550 DEG C of 6~12h of after baking, obtains final product spherical 5V spinel nickels lithium manganate material.The preparation method combines the advantage of existing liquid phase method and solid phase method, eliminates the step of liquid phase method is necessary to precipitate lithium source, nickel source, manganese source, and solid phase method element can be overcome to mix uneven defect.
Description
Technical field
The present invention relates to lithium ion secondary battery anode material field, more particularly to a kind of spherical 5V spinel nickels LiMn2O4
Material and preparation method thereof.
Background technology
Lithium ion battery has that open-circuit voltage is high, energy density big, long service life, memory-less effect, it is pollution-free and from
The advantages of discharging small, is the best battery system of current combination property, is also applicable battery system widest in area.By ten
The fast development of several years, lithium ion battery industrial chain has reached its maturity in China, its technical performance, maturity and industrialization
Considerable scale is reached, will be new energy and the supporting first-selection of ev industry battery within following one period, possessed
Absolute popularization and application advantage and huge development space.It is well known that the performance of lithium ion battery depend primarily on lithium from
The structure and performance of sub- battery material.Lithium ion battery material mainly includes positive electrode, negative material, barrier film and electrolyte,
Wherein positive electrode directly determines the performances such as the energy density and service life of lithium ion battery, is performance of lithium ion battery
Key influence factor.
5V spinel-types nickel ion doped grows up on the basis of lithium manganate having spinel structure in positive electrode, with mangaic acid
Lithium is equally have three-dimensional lithium ion tunnel, and reversible specific capacity is 146.7mAh/g, almost identical with LiMn2O4, but voltage platform
It is 4.7V or so, the 4V voltage platforms than LiMn2O4 will be higher by more than 15%.The materials application will make in lithium-ion-power cell
The energy density of battery system obtains larger raising, and amount of monomer of being connected under identical group of output voltage is reduced, and is favorably improved electricity
The reliability of pond group, is that energy density is high, good rate capability lithium-ion-power cell key raw material for development.
At present, the preparation method of 5V spinel-types nickel ion doped mainly has two kinds, and one is liquid phase method：First by co-precipitation
Generation spherical nickel-manganese presoma, is then mixed into lithium source high-temperature roasting and prepares final products；Two is solid phase method：First lithium
Source, nickel source, manganese source are well mixed, and then high-temperature roasting prepares final products.But liquid phase method technology controlling and process is complicated, is produced into
This height；The mixing of solid phase method element is uneven, and homogeneity of product and stability are poor, and granule-morphology is irregular, influences Product processing
Performance.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides a kind of preparation side of spherical 5V spinel nickels lithium manganate material
Method, combines the advantage of existing liquid phase method and solid phase method, eliminates precipitation lithium source, nickel source, the step of manganese source necessary to liquid phase method
Suddenly, and solid phase method element can be overcome to mix uneven defect.
Therefore, technical scheme is as follows：
A kind of preparation method of spherical 5V spinel nickels lithium manganate material, comprises the following steps：
1) lithium salts, nickel salt, manganese salt, binding agent are dissolved in deionized water, obtain material I；The binding agent is solvable
In the polymer of water；Meanwhile, lithium salts, nickel salt, manganese salt are water-soluble；
Wherein, elemental mole ratios meet Li：Ni：Mn=(1~1.05)：0.5：1.5, the quality of the binding agent is lithium
The 5~10% of salt, nickel salt and manganese salt quality sum；
2) the material I is spray-dried, drying temperature is 240~280 DEG C, obtains material II；
3) the material II is once calcined in air atmosphere, sintering temperature is 800~900 DEG C, roasting time
It is 4~12h, obtains material III；
4) by the material III and acetate, add in deionized water, high-speed stirred is well mixed, and obtains material IV；
Wherein, the quality of the acetate is the 2~5% of material III mass；
5) the material IV is spray-dried, drying temperature is 240~280 DEG C, obtains material V；
6) the material V is carried out into after baking in air atmosphere, sintering temperature is 450~550 DEG C, and roasting time is
6~12h, obtains final product the spherical 5V spinel nickels lithium manganate material.
Further：Step 1) lithium salts be lithium nitrate.
Further, step 1) nickel salt be nickel nitrate.
Further, step 1) manganese salt be manganese nitrate.
Further, step 1) binding agent be polyethylene glycol or polyvinylpyrrolidone.
Further, step 4) acetate be zinc acetate, copper acetate, magnesium acetate or aluminum acetate.
The beneficial effects of the invention are as follows：Step 1) entered from the mode of lithium salts, nickel salt, manganese salt and binding agent co-dissolve
OK, both can guarantee that each element was well mixed, eliminate again has the co-precipitation step of high request in liquid phase method to technique.In secondary roasting
It is in order in 5V spinel nickel LiMn2O4 Surface coating layer of substance, to completely cut off electrolyte to coat material using acetate before burning
Corrode, suppress the dissolving of manganese, improve cycle performance.Zinc acetate used, copper acetate, magnesium acetate or aluminum acetate in this patent
The uniformity that water ensure that cladding is dissolved in, the zinc of generation, Cu oxide can effectively completely cut off electrolyte after roasting, reach raising
The purpose of 5V spinel nickel LiMn2O4 cycle performances.
Brief description of the drawings
The process chart of the preparation method of the spherical 5V spinel nickels lithium manganate material that Fig. 1 is provided for the present invention；
Fig. 2 is the SEM photograph that embodiment 1 is obtained product.
Specific embodiment
Technical scheme is described in detail with reference to embodiments.
Embodiment 1
A kind of preparation method of spherical 5V spinel nickels lithium manganate material, comprises the following steps：
1) it is above-mentioned three kinds of material masses and 5% by 1mol lithium nitrates, 0.5mol nickel nitrates, 1.5mol manganese nitrates and quality
Polyethylene glycol be dissolved in deionized water, obtain material I；
2) the material I is spray-dried, drying temperature is 240 DEG C, obtains material II；
3) material II is once calcined in roasting kiln, air atmosphere, sintering temperature is 800 DEG C, roasting time
It is 12h, obtains material III；
4) in material III and quality being added into deionized water for the copper acetate of material III mass 2%, high-speed stirred mixing
Uniformly, material IV is obtained；
5) material IV is spray-dried, drying temperature is 240 DEG C, obtains material V；
6) material V is carried out into after baking in roasting kiln, air atmosphere, sintering temperature is 450 DEG C, and roasting time is
12h, obtains final product the spherical 5V spinel nickels lithium manganate material.
Fig. 2 is the SEM photograph that the present embodiment 1 is obtained product, and as seen from the figure, this Project Product is spherical in shape to be uniformly distributed, should
Pattern is conducive to the lifting of Product processing performance.
Embodiment 2
A kind of preparation method of spherical 5V spinel nickels lithium manganate material, comprises the following steps：
1) by 1mol lithium nitrates, 0.5mol nickel nitrates, 1.5mol manganese nitrates and quality be above-mentioned three kinds of material masses and
10% polyethylene glycol is dissolved in deionized water, obtains material I；
2) the material I is spray-dried, drying temperature is 280 DEG C, obtains material II；
3) material II is once calcined in roasting kiln, air atmosphere, sintering temperature is 900 DEG C, roasting time
It is 4h, obtains material III；
4) in material III and quality being added into deionized water for the magnesium acetate of material III mass 5%, high-speed stirred mixing
Uniformly, material IV is obtained；
5) material IV is spray-dried, drying temperature is 240 DEG C, obtains material V；
6) material V is carried out into after baking in roasting kiln, air atmosphere, sintering temperature is 550 DEG C, and roasting time is
6h, obtains final product the spherical 5V spinel nickels lithium manganate material.
Embodiment 3
A kind of preparation method of spherical 5V spinel nickels lithium manganate material, comprises the following steps：
1) by 1.05mol lithium nitrates, 0.5mol nickel nitrates, 1.5mol manganese nitrates and quality be above-mentioned three kinds of material masses and
10% polyvinylpyrrolidone is dissolved in deionized water, obtains material I；
2) the material I is spray-dried, drying temperature is 240 DEG C, obtains material II；
3) material II is once calcined in roasting kiln, air atmosphere, sintering temperature is 800 DEG C, roasting time
It is 12h, obtains material III；
4) in material III and quality being added into deionized water for the zinc acetate of material III mass 2%, high-speed stirred mixing
Uniformly, material IV is obtained；
5) material IV is spray-dried, drying temperature is 240 DEG C, obtains material V；
6) material V is carried out into after baking in roasting kiln, air atmosphere, sintering temperature is 450 DEG C, and roasting time is
12h, obtains final product the spherical 5V spinel nickels lithium manganate material.
Embodiment 4
A kind of preparation method of spherical 5V spinel nickels lithium manganate material, comprises the following steps：
1) by 1.05mol lithium nitrates, 0.5mol nickel nitrates, 1.5mol manganese nitrates and quality be above-mentioned three kinds of material masses and
5% polyvinylpyrrolidone is dissolved in deionized water, obtains material I；
2) the material I is spray-dried, drying temperature is 280 DEG C, obtains material II；
3) material II is once calcined in roasting kiln, air atmosphere, sintering temperature is 900 DEG C, roasting time
It is 4h, obtains material III；
4) in material III and quality being added into deionized water for the aluminum acetate of material III mass 5%, high-speed stirred mixing
Uniformly, material IV is obtained；
5) material IV is spray-dried, drying temperature is 240 DEG C, obtains material V；
6) material V is carried out into after baking in roasting kiln, air atmosphere, sintering temperature is 550 DEG C, and roasting time is
6h, obtains final product the spherical 5V spinel nickels lithium manganate material.
Experimental conditions：
Table 1 is listed and is made button cell first using lithium ion secondary battery anode material obtained in embodiment 1~4
Cycle charge-discharge specific capacity.The test condition of button cell is LR 2032,0.1C, 3.0~4.9V, vs.Li+/ Li, uses
Charging/discharging apparatus are blue electricity discharge and recharge instrument.
The charge-discharge property contrast table of table 1
The 5V spinel nickels lithium manganate material as obtained in data in table can be seen that the present invention, specific capacity is higher, forthright again
Energy and good cycle.Therefore had good prospects in lithium-ion-power cell field.
Claims (6)
1. a kind of preparation method of spherical 5V spinel nickels lithium manganate material, it is characterised in that comprise the following steps：
1) lithium salts, nickel salt, manganese salt, binding agent are dissolved in deionized water, obtain material I；The binding agent is water-soluble
Polymer；
Wherein, elemental mole ratios meet Li：Ni：Mn=(1~1.05)：0.5：1.5, the quality of the binding agent is lithium salts, nickel
The 5~10% of salt and manganese salt quality sum；
2) the material I is spray-dried, drying temperature is 240~280 DEG C, obtains material II；
3) the material II is once calcined in air atmosphere, sintering temperature be 800~900 DEG C, roasting time be 4~
12h, obtains material III；
4) by the material III and acetate, add in deionized water, high-speed stirred is well mixed, and obtains material IV；Wherein,
The quality of the acetate is the 2~5% of material III mass；
5) the material IV is spray-dried, drying temperature is 240~280 DEG C, obtains material V；
6) the material V being carried out into after baking in air atmosphere, sintering temperature is 450~550 DEG C, roasting time is 6~
12h, obtains final product the spherical 5V spinel nickels lithium manganate material.
2. as claimed in claim 1 spherical 5V spinel nickels lithium manganate material preparation method, it is characterised in that：Step 1) it is described
Lithium salts is lithium nitrate.
3. as claimed in claim 1 spherical 5V spinel nickels lithium manganate material preparation method, it is characterised in that：Step 1) it is described
Nickel salt is nickel nitrate.
4. as claimed in claim 1 spherical 5V spinel nickels lithium manganate material preparation method, it is characterised in that：Step 1) it is described
Manganese salt is manganese nitrate.
5. as claimed in claim 1 spherical 5V spinel nickels lithium manganate material preparation method, it is characterised in that：Step 1) it is described
Binding agent is polyethylene glycol or polyvinylpyrrolidone.
6. as claimed in claim 1 spherical 5V spinel nickels lithium manganate material preparation method, it is characterised in that：Step 4) it is described
Acetate is zinc acetate, copper acetate, magnesium acetate or aluminum acetate.
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| CN201710195004.3A CN106910878A (en) | 2017-03-29 | 2017-03-29 | A kind of spherical 5V spinel nickels lithium manganate material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113707875A (en) * | 2021-08-24 | 2021-11-26 | 蜂巢能源科技有限公司 | Spinel type lithium nickel manganese oxide, preparation method thereof and lithium ion battery |
| CN113937256A (en) * | 2020-07-14 | 2022-01-14 | 天津国安盟固利新材料科技股份有限公司 | Method for coating lithium nickel manganese oxide cathode material by spraying |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787254A (en) * | 2004-12-09 | 2006-06-14 | 比亚迪股份有限公司 | Lithium ion cell positive electrode actived material and preparation method thereof |
| CN105304896A (en) * | 2015-10-26 | 2016-02-03 | 华南理工大学 | Preparation method of zinc-oxide-coated lithium nickel manganese oxide positive electrode material |
-
2017
- 2017-03-29 CN CN201710195004.3A patent/CN106910878A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787254A (en) * | 2004-12-09 | 2006-06-14 | 比亚迪股份有限公司 | Lithium ion cell positive electrode actived material and preparation method thereof |
| CN105304896A (en) * | 2015-10-26 | 2016-02-03 | 华南理工大学 | Preparation method of zinc-oxide-coated lithium nickel manganese oxide positive electrode material |
Non-Patent Citations (1)
| Title |
|---|
| TIM RISTHAUS等: ""Synthesis of spinel LiNi0.5Mn1.5O4 with secondary plate morphology as cathode material for lithium ion batteries"", 《JOURNAL OF POWER SOURCES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113937256A (en) * | 2020-07-14 | 2022-01-14 | 天津国安盟固利新材料科技股份有限公司 | Method for coating lithium nickel manganese oxide cathode material by spraying |
| CN113707875A (en) * | 2021-08-24 | 2021-11-26 | 蜂巢能源科技有限公司 | Spinel type lithium nickel manganese oxide, preparation method thereof and lithium ion battery |
| CN113707875B (en) * | 2021-08-24 | 2023-03-07 | 蜂巢能源科技有限公司 | Spinel type lithium nickel manganese oxide, preparation method thereof and lithium ion battery |
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Application publication date: 20170630 |