CN106784660A - Nickel foam as interlayer Se TiO2/ NFF lithium selenium secondary cells and preparation method thereof - Google Patents
Nickel foam as interlayer Se TiO2/ NFF lithium selenium secondary cells and preparation method thereof Download PDFInfo
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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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Abstract
A kind of nickel foam as interlayer Se TiO2/ NFF lithium selenium secondary cells and preparation method thereof, belong to technical field of lithium ion.It is that 0.2~0.4g vinylpyrrolidones are dissolved in 6~8mL ethanol, adds 2~4mL glacial acetic acid and 1~5mL butyl titanates, 12~24h of stirring obtains spinning solution;Then the spinning under the high voltage of 15~20KV, then 6~12h pre-oxidation under the conditions of 400~700 DEG C by spinning product, obtains the TiO of 80~100nm of diameter2Nanofiber;2~8h is ground after mixing with mass ratio 1: 1 with Se particles, 6~12h is calcined after compressing tablet under the conditions of argon gas, 200~260 DEG C, Se particles is entered into TiO2Nanofiber it is mesoporous in, obtain Se TiO2Nanofiber;It is mixed with conductive agent, binding agent according to the ratio of mass ratio 8: 1: 1, gained slurry is coated on aluminium foil, obtain Se TiO2Positive electrode;In Se TiO2Between positive electrode and barrier film add NFF interlayers, lithium piece as to electrode assembling half-cell, so as to obtain Se TiO of the nickel foam of the present invention as interlayer2/ NFF lithium selenium secondary cells, with capacity higher, the circulating ratio performance of stabilization.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of nickel foam as interlayer Se-TiO2/NFF
Lithium selenium secondary cell and preparation method thereof.
Background technology
High-energy-density, long circulation life and low cost are the developing direction of batteries of electric automobile.Lithium-sulfur cell is because having
Theoretical Mass specific energy (2567Wh/kg), volume and capacity ratio (3467mAh/cm very high3) and low cost be considered as most have should
One of high-specific energy battery system of future generation with prospect.But the relatively low high rate performance for causing battery of the electric conductivity of sulphur is not high,
And many sulphions dissolve in ethers electrolyte and cause shuttle effect, cause the stable circulation performance of battery poor.For many years,
It is modified that people are such as consolidated on sulphur, electrolyte and barrier film by various effort, and the electrification of lithium-sulfur cell is improved to a certain extent
Performance is learned, but itself insulating properties of its essential problem such as sulphur is not resolved.
Selenium is located at same main group with sulphur in the periodic table of elements, and selenium is expected to turn into following substitute of lithium-sulfur cell.Although
The specific discharge capacity of selenium (675mAh/g) is lower than sulphur (1672mAh/g), but on volume and capacity ratio selenium (3253mAh/cm) with
Quite, due to receiving the limitation in battery pack space, volume and capacity ratio is more important with specific discharge capacity for sulphur (3467mAh/cm).
The electronic conductivity (1 × 10 of selenium-3S/m) than sulphur (5 × 10-28S/m it is) much higher, it means that active material in electrode material
Load capacity is expected to far above sulfur-based positive electrode, and selenium has a utilization rate higher than sulphur, more preferable electro-chemical activity, with lithium ion quickly
React, so as to realize actual specific energy higher.Therefore, selenium is expected to turn into the positive pole for being specifically applied to build high-energy battery
Material, including domestic electronic appliances and means of transport.
However, selenium equally can also experience decay and the coulombic efficiency of the capacity caused by the dissolving of many selenides as sulphur
Reduction.In order to improve the performance of battery, people take many measures, and a kind of strategy is the selenium material for synthesizing different shape structure
Material, such as the nanoporous or nano-fiber material of selenium.Another strategy is that selenium is fixed in porous matrix to pass through to inhale
Receive material and chase many selenides.Worn additionally, also increasing by a layer interlayer between electrode slice and barrier film and equally can also play suppression
The effect of shuttle effect.
During the present invention is positioned over electrode slice and barrier film using nickel foam (NFF) as interlayer first, and use TiO2As
The matrix of lithium selenium cell, obtains cycle performance and all good lithium selenium secondary cell of high rate performance.
The content of the invention
It is an object of the invention to provide a kind of a kind of simple nickel foam of novel preparation process as interlayer Se-
TiO2/ NFF lithium selenium secondary cells and preparation method thereof, described its step of preparation method is as follows:
1) TiO is prepared2Nanofiber
0.2~0.4g vinylpyrrolidones are dissolved in 6~8mL ethanol, 2~4mL glacial acetic acid and 1~5mL metatitanic acids is added
Four butyl esters, 12~24h of stirring obtains spinning solution;Then the spinning under the high voltage of 15~20KV, then by spinning product 400
6~12h pre-oxidation, obtains the TiO of 80~100nm of diameter under the conditions of~700 DEG C2Nanofiber;
2) Se-TiO is prepared2Positive electrode
By step 1) TiO for preparing2Nanofiber and Se particles are with mass ratio 1:2~8h, compressing tablet are ground after 1 mixing
6~12h is calcined under the conditions of argon gas, 200~260 DEG C afterwards, Se particles is entered into TiO2Nanofiber it is mesoporous in, obtain
Se-TiO2Nanofiber;By obtained Se-TiO2Nanofiber, conductive agent (super P, conductive black), binding agent (SA, sea
Mosanom) according to mass ratio 8:1:1 ratio mixing, gained slurry is coated on aluminium foil, obtains Se-TiO2Positive electrode;
3) Se-TiO is prepared2/ NFF lithium selenium secondary cells
By nickel foam compressing tablet into the disk of 10~20 μm of thickness, with 2M salt acid elutions, then carried out with deionized water and ethanol
Rinse, obtain NFF interlayers:
In Se-TiO2NFF interlayers are added between positive electrode and barrier film (Celgard 2300), lithium piece is used as to electrode group
Dress half-cell, so as to obtain Se-TiO of the nickel foam of the present invention as interlayer2/ NFF lithium selenium secondary cells.
A kind of nickel foam of the present invention as interlayer Se-TiO2/ NFF lithium selenium secondary cells, it is characterised in that be
Prepared by the above method.
The beneficial effects of the invention are as follows:
(1) Se-TiO for preparing2Nanofiber pattern is homogeneous, and purity is high, reproducible.
(2) raw material for using are prepared cheap and easy to get, low cost, without expensive device.
(3) process is simple, favorable reproducibility can be not only used for experimental implementation, can industrially mass produce again.
(4) anode material for lithium-ion batteries Se-TiO prepared by the present invention2/ NFF has capacity higher, the circulation of stabilization
High rate performance.
Brief description of the drawings
In order to illustrate more clearly of the technical scheme in the present invention and its performance of material is prepared, correlation is given below
Diagram.
Fig. 1 is NFF interlayer and Se/TiO prepared by embodiment 12The scanning electron microscope (SEM) photograph (SEM) of nanofiber.Figure (a) is 40
The scanning electron microscope (SEM) photograph (SEM) of NFF under μm scale, it can be seen that NFF is pore space structure.Figure (b) is Se/TiO under 1 μm of scale2Receive
The scanning electron microscope (SEM) photograph (SEM) of rice fiber, it can be clearly seen that Se/TiO2The diameter of nanofiber about 100~120nm, it is overall
Even thickness, soilless sticking.
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates that embodiment 1 prepares material.Wherein curve 3 is the Se/TiO for preparing2Receive
The collection of illustrative plates of rice fiber, curve 1 and curve 2 are respectively Se and TiO2XRD spectrum.Contrast show that the x- of prepared material is penetrated
Line diffraction (XRD) collection of illustrative plates free from admixture peak occurs, that is, prove that the material for preparing is the Se-TiO of pure phase2。
Fig. 3 is Se-TiO prepared by embodiment 12Used as positive electrode, NFF is placed in positive electrode and barrier film as interlayer
Between (Celgard 2300), lithium piece is schemed as the CV to electrode, the half-cell of making, in first lap discharge process, Se quilts
Many selenides are reduced into, many selenides are further reduced into Li2The process of Se, there is an oxidation peak wider at 2.3V, right
Answer Li2Transformations of the Se to many selenides and Se.Two pairs of new redox peaks are occurred in that simultaneously, wherein 1.7V/2.0V is TiO2
The peak of offer;And 1.4V/1.9V is the peak of the redox reaction for generating new, that is, the Li for producing2Se there occurs reversible with nickel
Redox reaction generate Ni3Se2, 1.9V correspond to Li2Se to Ni3Se2Transformation, 1.4V correspond to Ni3Se2To Li2Se
Transformation.This new redox reaction restrained effectively the loss of capacity, improve the performance of battery.
Fig. 4 is Se-TiO prepared by embodiment 12Used as positive electrode, NFF is placed in positive electrode and barrier film as interlayer
Between (Celgard 2300), lithium piece is used as to electrode, the cycle performance figure of the half-cell of making.There are 2 curves, curve in figure
1 represents coulombic efficiency, and curve 2 represents specific discharge capacity.It is seen that under 0.5C (337.5mAh/g) current density,
After being circulated by 200 times, specific discharge capacity keeps still reaching 597mAh/g, and coulombic efficiency close to 100%, shows material
Material has preferable cyclical stability.
Fig. 5 is Se-TiO prepared by embodiment 12Used as positive electrode, NFF is placed in positive electrode and barrier film as interlayer
Between (Celgard 2300), lithium piece is used as to electrode, the big circulation performance map of the half-cell of making.There are 2 songs in figure
Line, curve 1 represents coulombic efficiency, and curve 2 represents specific discharge capacity.It can be seen that in the big of 30C (20250mA/g)
Under current density charge-discharge test, by 500 circulations, the specific discharge capacity capacity of material remains to be maintained at 178mAh/g, and
And coulombic efficiency is close to 100%, illustrate that material has preferable cyclical stability and excellent high rate during charging-discharging.
Fig. 6 is Se-TiO prepared by embodiment 12Used as positive electrode, NFF is placed in positive electrode and barrier film as interlayer
Between (Celgard 2300), used as to electrode, the half-cell of making is respectively in 0.5C, 1C, 2C, 5C, 10C, 20C, 30C for lithium piece
Discharge test high rate performance figure under different current densities.It can be seen that material is followed under the test of each current density
Ring stabilization, and under the high current of 30C, the specific capacity of material can still reach 303mAh/g, it was demonstrated that material has more excellent
Elegant high rate performance.
Fig. 7 is Se-TiO prepared by embodiment 22Used as positive electrode, NFF is placed in positive electrode and barrier film as interlayer
Between (Celgard 2300), lithium piece is used as to electrode, the cycle performance figure of the half-cell of making.There are two curves in figure, it is bent
Line 1 is Se-TiO2/ NFF materials, curve 2 is Se-TiO2Material.Curve 2 is as a comparison.It is seen that curve 2 exists
Under 0.5C (337.5mAh/g) current density, after being circulated by 100 times, specific discharge capacity is only 124mAh/g, and curve 1 is passed through
100 times circulation specific discharge capacity can still reach 597mAh/g.Illustrate that NFF interlayers can absorb many selenides, suppress capacity
Loss.
Fig. 8 be embodiment 3 prepare Se as positive electrode, NFF is placed in positive electrode and barrier film as interlayer
Between (Celgard 2300), lithium piece is used as to electrode, the cycle performance figure of the half-cell of making.There are two curves in figure, it is bent
Line 1 is Se-TiO2/ NFF materials, curve 2 is Se/NFF materials.Curve 2 is as a comparison.It is seen that curve 2 exists
Under 0.5C (337.5mAh/g) current density, after being circulated by 100 times, specific discharge capacity only remains 152mAh/g, and curve 1 is passed through
100 times circulation specific discharge capacity can still reach 597mAh/g.Illustrate TiO2Solid selenium can be played a part of, so as to inhibit
Shuttle effect.
Fig. 9 be embodiment 4 prepare Se as positive electrode, NFF is placed in positive electrode and barrier film as interlayer
Between (Celgard 2300), lithium piece is used as to electrode, the cycle performance figure of the half-cell of making.There are two curves in figure, it is bent
Line 1 is Se-TiO2/ NFF materials, curve 2 is Se materials.Curve 2 is as a comparison.It is seen that curve 2 is in 0.5C
Under (337.5mAh/g) current density, after being circulated by 100 times, specific discharge capacity only remains 38mAh/g, and curve 1 is through 100 times
Circulation specific discharge capacity can still reach 597mAh/g.Illustrate TiO2Solid selenium can be played a part of, NFF interlayers can absorb
Many selenides, the two is the shuttle effect that mutually collaboration suppresses in lithium selenium cell, and then improves the chemical property of battery.
Specific embodiment
Embodiment 1:
1) 0.35g vinylpyrrolidones are dissolved in 6.5mL ethanol, add 2mL glacial acetic acid and 1.5mL butyl titanates, stir
12h is mixed as spinning solution, spinning solution is sucked and is fixed on syringe clip upper in manifold with the syringe of 10mL
Aluminium foil is placed to receive material in end, the underface of syringe, the distance controlling from syringe tip to aluminium foil in 20cm or so, so
The spinning under the high voltage of about 18KV afterwards, obtains white filiform and is laid in aluminium foil surface.The white filiform that will be obtained takes out,
10h pre-oxidation, as TiO are carried out at 550 DEG C2Nanofiber.The TiO that will be prepared2Nanofiber and Se particles are with mass ratio
1:1 grinding 5h, is placed in the reactor full of argon gas after compressing tablet, 260 DEG C of roasting 10h, Se is entered TiO2It is mesoporous in, obtain
Se-TiO2Nanofiber.The Se-TiO that will be obtained2Material, conductive agent (super P, i.e. conductive black), binding agent (SA, i.e. sea
Mosanom) according to mass ratio 8:1:1 mixing, gained slurry is coated on aluminium foil (thickness of slurry is 0.02mm), is placed in 120 DEG C
Vacuum drying oven 10h, obtains Se-TiO2Electrode material.The disk of diameter 12mm thickness 20um will be cut into after nickel foam compressing tablet, uses 2M
Salt acid elution, then be rinsed with deionized water and ethanol.With Se-TiO2Used as positive electrode, assembled battery is full of argon gas
Glove box in carry out, with Se-TiO2It is positive electrode, NFF is placed in positive electrode and barrier film (Celgard as interlayer
2300) it is that, to electrode, electrolyte is double (chloroform) the sulfimide lithium salts of 1mol/L and 1,2- dimethoxy with lithium piece between
Ethane and 1,3- dioxies defend ring with volume ratio 1:The mixed solution of 1 composition, is packaged, and has obtained nickel foam of the present invention
As the Se-TiO of interlayer2/ NFF secondary cells.
The cycle performance of battery curve of preparation is respectively as shown in figure 4, charging and discharging currents density is 0.5C.Big circulation
Energy curve is as shown in figure 5, charging and discharging currents density is 30C, it can be seen that the cycle performance of battery is preferable.High rate performance figure is as schemed
Shown in 6, charging and discharging currents density is 0.5C, 1C, 2C, 5C, 10C, 20C, 30C, shows that battery has preferably high rate performance.
Raw material described in this example can have been bought from commercial channel.
Embodiment 2:
Embodiment 2 is not add NFF interlayers in assembled battery with the difference part of embodiment 1, due to no interlayer
Many selenides are absorbed, its electrochemical cycle stability and high rate performance are relatively low, see Fig. 7.
Embodiment 3:
Embodiment 3 is not prepare TiO with the difference part of embodiment 12Nanofiber, that is, directly by Se simple substance
Electrode material is made with SP, SA smear, NFF interlayers is added during assembled battery, due to no TiO2Gu selenium, electrochemical cycle stability
Property and high rate performance are relatively low, see Fig. 8.
Embodiment 4:
Embodiment 4 is to use Se simple substance direct smears with the difference part of embodiment 1, and is not also had in assembled battery
NFF interlayers are added, due to both not consolidating selenium, do not have interlayer to absorb many selenides again, electrochemical cycle stability and high rate performance are minimum,
See Fig. 9.
Claims (3)
1. a kind of nickel foam as interlayer Se-TiO2The preparation method of/NFF lithium selenium secondary cells, its step is as follows:
1) TiO is prepared2Nanofiber
0.2~0.4g vinylpyrrolidones are dissolved in 6~8mL ethanol, 2~4mL glacial acetic acid and the fourth of 1~5mL metatitanic acids four is added
Ester, 12~24h of stirring obtains spinning solution;Then the spinning under the high voltage of 15~20KV, then by spinning product 400~
6~12h pre-oxidation, obtains the TiO of 80~100nm of diameter under the conditions of 700 DEG C2Nanofiber;
2) Se-TiO is prepared2Positive electrode
By step 1) TiO for preparing2Nanofiber and Se particles are with mass ratio 1:1 mixing after grind 2~8h, after compressing tablet
Argon gas, 6~12h is calcined under the conditions of 200~260 DEG C, Se particles is entered into TiO2Nanofiber it is mesoporous in, obtain Se-TiO2
Nanofiber;By obtained Se-TiO2Nanofiber, conductive agent, binding agent are according to mass ratio 8:1:1 ratio mixing, gained
Slurry is coated on aluminium foil, obtains Se-TiO2Positive electrode;
3) Se-TiO is prepared2/ NFF lithium selenium secondary cells
By nickel foam compressing tablet into the disk of 10~20 μm of thickness, with 2M salt acid elutions, then it is rinsed with deionized water and ethanol,
Obtain NFF interlayers;In Se-TiO2NFF interlayers are added between positive electrode and barrier film, lithium piece as to electrode assembling half-cell,
So as to obtain Se-TiO of the nickel foam as interlayer2/ NFF lithium selenium secondary cells.
2. a kind of nickel foam as claimed in claim 1 as interlayer Se-TiO2The preparation method of/NFF lithium selenium secondary cells,
It is characterized in that:Described conductive agent is conductive black, and described binding agent is sodium alginate.
3. a kind of nickel foam as interlayer Se-TiO2/ NFF lithium selenium secondary cells, it is characterised in that:It is by claim 1 or 2
Described method is prepared.
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Cited By (1)
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CN111180711A (en) * | 2020-01-22 | 2020-05-19 | 河北大学 | Preparation method of graphene-coated oxide-selenium composite aluminum battery positive electrode material |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN111180711A (en) * | 2020-01-22 | 2020-05-19 | 河北大学 | Preparation method of graphene-coated oxide-selenium composite aluminum battery positive electrode material |
CN111180711B (en) * | 2020-01-22 | 2022-11-22 | 河北大学 | Preparation method of graphene-coated oxide-selenium composite aluminum battery positive electrode material |
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