CN106082360B - A kind of lithium ion battery negative material of flower-shaped high power capacity and preparation method and application - Google Patents
A kind of lithium ion battery negative material of flower-shaped high power capacity and preparation method and application Download PDFInfo
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Abstract
The present invention discloses a kind of lithium ion battery negative material of flower-shaped high power capacity and preparation method and application, belongs to energy new material technology field.The preparation method comprises the following steps：First the nickel salt of solubility and divalent iron salt are completely dissolved in a solvent, add protective agent；Uniformly after mixing, heated at 180 DEG C~200 DEG C and obtain within 10~20 hours dirty-green precipitation, finally rinsed green precipitate, drying, obtain nickel ferrite based magnetic loaded.Gained ferrous acid nickel by powder is uniform flower-shaped particle, is uniformly dispersed, well-crystallized, electrochemical performance, first charge-discharge efficiency is high, specific capacity high (first up to more than 1400mAh/g, current commercialized graphite theoretical capacity is 372mAh/g), good cycle.The preparation method technique is simple, cost is cheap, suitable for industrialized production, and emphasis solves the problems, such as that efficiency is low first, irreversible capacity loss is big and electric conductivity is poor existing for Ni-based ferrite.
Description
Technical field
The invention belongs to energy new material technology field, more particularly to a kind of negative electrode of lithium ion battery material of flower-shaped high power capacity
Material and preparation method and application.
Background technology
Lithium ion battery have operating voltage height, high-energy-density, long lifespan, good cycle, memory-less effect and
The advantages that environmental pollution is small, it is widely used in portable electric appts, implantable medical device, electric automobile etc..It is negative
Main body of the pole material as storage lithium, is the important part of lithium ion battery.The negative pole of current commercialized lithium ion battery
Material is mainly graphite, can be in graphite surface during high rate charge-discharge although it has preferable cycle performance
Li dendrite is produced, potential safety hazard be present, and graphite material theoretical capacity low (372mAh/g) and lithium ion diffusion coefficient are small etc.
Shortcoming, it is difficult to meet the needs of high performance lithium ion battery.In order to further improve the energy density of lithium ion battery, using the longevity
Life etc., develop new, cheap, height ratio capacity negative material has turned into the focus of Study on Li-ion batteries.
In recent years, the double transition metal oxides of iron-based spinel-type as lithium ion battery negative material by more and more
Concern.Compared with traditional carbon material, the double transition metal oxides of iron-based spinel-type have height ratio capacity, it is safe and reliable,
The advantages that resource is extensive, synthetic material is cheap, it is set to have as in terms of high performance lithium ionic cell cathode material of new generation
There are tremendous expansion potentiality.
Among transition metal oxide, due to NiFe2O4With 915mAhg-1Theoretical specific capacity, and resource is rich
Richness, cost is relatively low, it is environmentally friendly the advantages that, NiFe2O4It is considered as a kind of negative electrode of lithium ion battery material of great application prospect
Material.
Although nickel ferrite based magnetic loaded has the advantages of many as lithium cell negative pole material, there is also obvious in the application process of reality
The problem of：NiFe2O4Material has that electrical conductivity is low, Volume Changes are big during charge and discharge cycles in itself, causes the stable circulation of difference
Property, chemical property is undesirable.
The content of the invention
The shortcomings that in order to overcome prior art, is to provide a kind of flower-shaped high power capacity with deficiency, primary and foremost purpose of the invention
The preparation method of lithium ion battery negative material.The preparation method technique is simple, cost is cheap, suitable for industrialized production, weight
Point solves the problems, such as that efficiency is low first, irreversible capacity loss is big and electric conductivity is poor existing for Ni-based ferrite.
Another object of the present invention is in the lithium-ion electric for being to provide the flower-shaped high power capacity obtained by above-mentioned preparation method
Pond negative material.
It is still another object of the present invention to provide the application of the lithium ion battery negative material of above-mentioned flower-shaped high power capacity.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of the lithium ion battery negative material of flower-shaped high power capacity, comprises the following steps：
First the nickel salt of solubility and divalent iron salt are completely dissolved in a solvent, add protective agent；Uniformly after mixing,
Heated at 180 DEG C~200 DEG C and obtain within 10~20 hours dirty-green precipitation, finally rinsed green precipitate, drying, obtain nickel ferrite based magnetic loaded,
The lithium ion battery negative material of i.e. flower-shaped high power capacity.Gained ferrous acid nickel by powder is uniform flower-shaped particle, good dispersion, specific volume
Amount is high, good cycle.
Described soluble nickel salt is at least one of nickel chloride, nickel nitrate, nickel acetate and nickel sulfate；
Described divalent iron salt is at least one of frerrous chloride, ferrous nitrate, ferrous acetate and ferrous sulfate；
The concentration of the nickel ion of described soluble nickel salt is 0.01~0.1 mol/L；
The concentration of the ferrous ion of described divalent iron salt is 0.02~0.2 mol/L；
Nickel ion is pressed in described soluble nickel salt and divalent iron salt：Ferrous ion=1：2 (mol ratio) ratios are mixed
Close；
Described solvent is the mixed solution of deionized water and ethylene glycol, and ratio is volume ratio 1:1.
Described protective agent is polyvinylpyrrolidone (PVP) or urea；Its dosage is controlled in molysite and nickel salt total moles
The 0.24% of amount；
Described polyvinylpyrrolidone (PVP) is preferably PVP-K30.
Described heating is carried out in high pressure sealing tank.
Described flushing is to use absolute ethyl alcohol and deionized water centrifugal elutriation.
The condition of described drying is preferably 50~80 DEG C of dryings 5~10 hours.
A kind of lithium ion battery negative material of flower-shaped high power capacity, is prepared by above-mentioned preparation method.
Application of the lithium ion battery negative material of described flower-shaped high power capacity in lithium ion battery preparation field.
The present invention is had the following advantages and effect relative to prior art：
The present invention uses hydrothermal template process, has prepared the flower-shaped ferrous acid nickel material of nano particle accumulation, and product is scattered equal
Even, well-crystallized, electrochemical performance, first charge-discharge efficiency is high, and specific capacity is high (first up to more than 1400mAh/g, at present
Commercialized graphite theoretical capacity is 372mAh/g), good cycle.
Brief description of the drawings
Fig. 1 is the XRD spectrum of the nickel ferrite based magnetic loaded of the gained of embodiment 1.
Fig. 2 is the XRD spectrum of the nickel ferrite based magnetic loaded of the gained of embodiment 2.
Fig. 3 is the XRD spectrum of the nickel ferrite based magnetic loaded of the gained of embodiment 3.
Fig. 4 is the stereoscan photograph of the Flied emission nickel ferrite based magnetic loaded of the gained of embodiment 1.
Fig. 5 is the stereoscan photograph of the Flied emission nickel ferrite based magnetic loaded of the gained of embodiment 2.
Fig. 6 is the stereoscan photograph of the Flied emission nickel ferrite based magnetic loaded of the gained of embodiment 3.
Fig. 7 is the charge-discharge performance figure of the gained nickel ferrite based magnetic loaded of embodiment 1.
Fig. 8 is the charge-discharge performance figure of the gained nickel ferrite based magnetic loaded of embodiment 2.
Fig. 9 is the charge-discharge performance figure of the gained nickel ferrite based magnetic loaded of embodiment 3.
Figure 10 is process chart.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
In following case study on implementation, working electrode is cut into Φ 12mm circular piece for the alloy firm that deposition is prepared,
It is pour lithium slice to electrode, electrolyte is by LiPF that solute is 1mol/L6/ solvent is EC (ethylene carbonate)+DMC
(dimethy carbonate)+EMC (ethylene carbonate) (mass ratio 1:1:1) solution allocation forms, and barrier film is
Microporous polypropylene membrane Celgard-2300, CR2025 type button cells are assembled into the glove box full of argon gas.Battery charge and discharge
Electric (Land) battery test system of indigo plant that electrical testing is produced using Wuhan Jin Nuo Electronics Co., Ltd.s.In battery charging and discharging system
Using constant current charge-discharge test, charging and discharging currents 1mA, charging/discharging voltage scope control is between 0.01~2.5V.
Embodiment 1：
0.291g six water nickel nitrate (Ni (NO are weighed respectively3)2·6H2O), 0.576g six water ferrous nitrate (Fe
(NO3)2·6H2O) mixed dissolution is in 50mL ethylene glycol and the 50mL aqueous solution, and wherein the molar concentration of nickel nitrate is rubbed for 0.01
You/liter, the molar concentration of ferrous nitrate be 0.02 mol/L, and the mol ratio of nickel ion and ferrous ion is 1：2, treat completely
0.29g (0.0073mmol) polyvinylpyrrolidones are added after dissolving to stir 0.5 hour as protective agent, the mixed liquor of gained.
Then homogeneous mixture solotion is poured into 200mL high pressure sealing tank, obtaining within 20 hours dirty-green in 180 degrees Centigrade sinks
Form sediment, filter out dirty-green precipitation, with several times of absolute ethyl alcohol and deionized water rinsing, 50 degrees Celsius of dryings 6 hours, finally obtain iron
Sour nickel.The process chart of preparation is as shown in Figure 10.Side noted earlier is pressed as negative material using material made from embodiment 1
Method is assembled into CR2025 button cells.
Fig. 1 is the XRD spectrum of ferrous acid nickel by powder.The collection of illustrative plates matches with nickel ferrite based magnetic loaded standard card JCPDSno.10-0325,
There is no NiO, Fe2O3Deng the diffraction maximum of impurity, it is pure nickel ferrite based magnetic loaded to illustrate product.Fig. 4 is that the ESEM of nickel ferrite based magnetic loaded powder shines
Piece, the nickel ferrite based magnetic loaded for showing synthesis is uniform spheric granules, and flower-shaped a length of 2~4 μm of average diameter, good dispersion, Fig. 7 is nickel ferrite based magnetic loaded
Powder makes the charge-discharge performance figure of lithium ion battery negative material, and can obtain new ferrous acid Ni nanopowders material by figure makees
High for lithium cell cathode material specific capacity, specific capacity first is 1633mAh/g, and initial charge specific capacity is 1157mAh/g, first
Secondary cycle efficieny is 70.85%.Circulation 20 weeks, specific capacity is also maintained at more than 700mAh/g, good cycle.The flower of the present invention
Shape lithium ion battery ferrous acid nickel negative material has good efficiency first and stable circulation performance.
Embodiment 2：
2.63g nickel sulfate hexahydrate (NiSO is weighed respectively4·6H2O), 5.76g six water ferrous nitrate (Fe (NO3)2·
6H2O) mixed dissolution is in 50mL ethylene glycol and the 50mL aqueous solution, and the wherein molar concentration of nickel sulfate is 0.1 mol/L, nitre
Sour ferrous molar concentration be 0.2 mol/L, and the mol ratio of nickel ion and ferrous ion is 1：2, add until completely dissolved
2.90g (0.073mmol) polyvinylpyrrolidones stir 0.5 hour as protective agent, the mixed liquor of gained.Then uniformly mixed
Close solution to pour into 200mL high pressure sealing tank, obtain within 15 hours dirty-green precipitation in 200 degrees Centigrade, filter out dark green
Color precipitates, and with several times of absolute ethyl alcohol and deionized water rinsing, 50 degrees Celsius of dryings 6 hours, finally obtains nickel ferrite based magnetic loaded.Using implementation
Material made from example 2 is assembled into CR2025 button cells as negative material by method noted earlier.
Fig. 2 is the XRD spectrum of nickel ferrite based magnetic loaded powder.The collection of illustrative plates matches with nickel ferrite based magnetic loaded standard card JCPDSno.10-0325,
There is no NiO, Fe2O3Deng the diffraction maximum of impurity, it is pure nickel ferrite based magnetic loaded to illustrate product.Fig. 5 is that the ESEM of nickel ferrite based magnetic loaded powder shines
Piece, the nickel ferrite based magnetic loaded for showing synthesis is uniform spheric granules, and flower-shaped a length of 2~4 μm of average diameter, good dispersion, Fig. 8 is nickel ferrite based magnetic loaded
Powder makes the charge-discharge performance figure of lithium ion battery negative material, and can obtain new zinc ferrite nano-powder material by figure makees
High for lithium cell cathode material specific capacity, specific capacity first is 1613mAh/g, and initial charge specific capacity is 1151mAh/g, first
Secondary cycle efficieny is 71.36%.By 20 weeks, specific capacity was also maintained at more than 700mAh/g, good cycle.The present invention's is new
The flower-shaped lithium ion battery ferrous acid nickel negative material of type has good efficiency first and stable circulation performance.
Embodiment 3
2.91g six water nickel nitrate (Ni (NO are weighed respectively3)2·6H2O), 5.56g ferrous sulfate heptahydrate (FeSO4·
7H2O) mixed dissolution is in 50mL ethylene glycol and the 50mL aqueous solution, and the wherein molar concentration of nickel nitrate is 0.1 mol/L, sulphur
Sour ferrous molar concentration be 0.2 mol/L, and the mol ratio of nickel ion and ferrous ion is 1：2, add until completely dissolved
2.90g (0.073mmol) polyvinylpyrrolidones stir 0.5 hour as protective agent, the mixed liquor of gained.Then uniformly mixed
Close solution to pour into 200mL high pressure sealing tank, obtain within 10 hours dirty-green precipitation in 190 degrees Centigrade, filter out dark green
Color precipitates, and with several times of absolute ethyl alcohol and deionized water rinsing, 50 degrees Celsius of dryings 6 hours, finally obtains nickel ferrite based magnetic loaded.Using implementation
Material made from example 3 is assembled into CR2025 button cells as negative material by method noted earlier.
Fig. 3 is the XRD spectrum of nickel ferrite based magnetic loaded powder.The collection of illustrative plates matches with nickel ferrite based magnetic loaded standard card JCPDSno.10-0325,
There is no NiO, Fe2O3Deng the diffraction maximum of impurity, it is pure nickel ferrite based magnetic loaded to illustrate product.Fig. 6 is that the ESEM of nickel ferrite based magnetic loaded powder shines
Piece, the nickel ferrite based magnetic loaded for showing synthesis is uniform spheric granules, and flower-shaped a length of 2~4 μm of average diameter, good dispersion, Fig. 9 is nickel ferrite based magnetic loaded
Powder makes the charge-discharge performance figure of lithium ion battery negative material, and can obtain new zinc ferrite nano-powder material by figure makees
High for lithium cell cathode material specific capacity, specific capacity first is 1479mAh/g, and initial charge specific capacity is 1116mAh/g, first
Secondary cycle efficieny is 75.46%.By 20 weeks, specific capacity was also maintained at more than 700mAh/g, good cycle.The present invention's is new
The flower-shaped lithium ion battery ferrous acid nickel negative material of type has good efficiency first and stable circulation performance.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the lithium ion battery negative material of flower-shaped high power capacity, it is characterised in that comprise the following steps：
First the nickel salt of solubility and divalent iron salt are completely dissolved in a solvent, add protective agent；Uniformly after mixing, 180
DEG C~200 DEG C at heat 10~20 hours obtain dirty-green precipitation, finally rinse green precipitate, drying, obtain nickel ferrite based magnetic loaded, that is, spend
The lithium ion battery negative material of shape high power capacity；
Described protective agent is polyvinylpyrrolidone or urea.
2. the preparation method of the lithium ion battery negative material of flower-shaped high power capacity according to claim 1, it is characterised in that：
Described soluble nickel salt is at least one of nickel chloride, nickel nitrate, nickel acetate and nickel sulfate.
3. the preparation method of the lithium ion battery negative material of flower-shaped high power capacity according to claim 1, it is characterised in that：
Described divalent iron salt is at least one of frerrous chloride, ferrous nitrate, ferrous acetate and ferrous sulfate.
4. the preparation method of the lithium ion battery negative material of flower-shaped high power capacity according to claim 1, it is characterised in that：
The concentration of the nickel ion of described soluble nickel salt is 0.01~0.1 mol/L；
The concentration of the ferrous ion of described divalent iron salt is 0.02~0.2 mol/L.
5. the preparation method of the lithium ion battery negative material of flower-shaped high power capacity according to claim 1, it is characterised in that：
Nickel ion in molar ratio in described soluble nickel salt and divalent iron salt：Ferrous ion=1：2 ratios mix.
6. the preparation method of the lithium ion battery negative material of flower-shaped high power capacity according to claim 1, it is characterised in that：
Described solvent is the mixed solution of deionized water and ethylene glycol, and ratio is volume ratio 1:1.
7. the preparation method of the lithium ion battery negative material of flower-shaped high power capacity according to claim 1, it is characterised in that：
Described protectant dosage controls 0.24% in molysite and nickel salt integral molar quantity.
8. the preparation method of the lithium ion battery negative material of flower-shaped high power capacity according to claim 1, it is characterised in that：
The condition of described drying is 50~80 DEG C and dried 5~10 hours.
9. a kind of lithium ion battery negative material of flower-shaped high power capacity, it is characterised in that by described in any one of claim 1~8
Preparation method be prepared.
10. the lithium ion battery negative material of the flower-shaped high power capacity described in claim 9 is in lithium ion battery preparation field
Using.
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| CN107204422A (en) * | 2017-06-13 | 2017-09-26 | 四川大学 | A kind of preparation method of carbon/nickel ferrite based magnetic loaded nanometer composite fiber material |
| CN107452952B (en) * | 2017-08-16 | 2019-10-08 | 华南师范大学 | A kind of composite material and preparation method and application of nickel ferrite based magnetic loaded and silicon |
| CN107308922A (en) * | 2017-08-28 | 2017-11-03 | 华南师范大学 | A kind of water process is with Ni-based from growth three-dimensional material and preparation method thereof |
| CN108110227A (en) * | 2017-11-20 | 2018-06-01 | 南开大学 | Lithium-sulfur battery composite cathode material of nickel ferrite based magnetic loaded polar support and preparation method thereof |
| CN109585825A (en) * | 2018-11-28 | 2019-04-05 | 成都理工大学 | The Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material and preparation method thereof |
| CN112467069A (en) * | 2020-12-11 | 2021-03-09 | 燕山大学 | Battery negative electrode material and preparation method and application thereof |
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