CN109888239A - A kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery and preparation method thereof and a kind of sodium-ion battery - Google Patents
A kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery and preparation method thereof and a kind of sodium-ion battery Download PDFInfo
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- CN109888239A CN109888239A CN201910174877.5A CN201910174877A CN109888239A CN 109888239 A CN109888239 A CN 109888239A CN 201910174877 A CN201910174877 A CN 201910174877A CN 109888239 A CN109888239 A CN 109888239A
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Abstract
The invention discloses a kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery and preparation method thereof and a kind of sodium-ion batteries, nickel source, polymethyl methacrylate and polyacrylonitrile are added to N, in dinethylformamide, uniform solution is obtained after stirring at room temperature；Uniform solution is taken out with syringe, is put into electrostatic spinning machine；It sets certain voltage, after flow velocity, uniform slurries is spun into nanofiber；The fiber that will have been spun, in air low temperature calcination for a period of time, then high-temperature calcination；Calcined material cures are finally obtained into one-dimensional N doping curing nickel porous fibre with sulphur powder.The present invention uses electrostatic spinning technique, and the curing nickel nano particle that polyacrylonitrile (nitrogenous) is evenly coated as carbon skeleton slows down it and generated volume expansion and improves electric conductivity in cyclic process.When high-temperature calcination simultaneously, the high rate performance and cycle performance of sodium-ion battery are effectively improved.
Description
Technical field
The present invention relates to a kind of, and in particular to one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery and
Preparation method and a kind of sodium-ion battery.
Background technique
With the extensive utilization of new energy, lithium ion battery answering in terms of electronic equipment, electric car and power grid energy storage
With also more and more extensive.And the shortage and Gao Chengben of lithium source, lithium ion battery can not be made to meet the needs of current again.And metallic sodium
Possess property similar with lithium, and at low cost, content is high, therefore high performance sodium-ion battery be hopeful very much to substitute lithium from
Sub- battery.
Currently, transient metal sulfide such as curing nickel, molybdenum disulfide, stannic disulfide etc. is in anode material of lithium-ion battery
Application in have received widespread attention.Especially curing nickel composite material has 873mAh g-1High theoretical specific capacity,
There are very big potentiality to be used as anode material of lithium-ion battery.But curing nickel electric conductivity is poor, and ratio can be generated in cyclic process
Biggish bulk effect leads to the rapid decay and certain risk of performance, largely limits answering for curing nickel
With.Therefore, the feasible method that can be effectively improved electric conductivity and bulk effect is searched out, so that high-performance is obtained, safe two
Nickel sulfide anode material of lithium-ion battery is vital.
Summary of the invention
Problem to be solved by this invention is: it is negative to provide a kind of one-dimensional N doping curing nickel porous fibre sodium-ion battery
Pole material and preparation method thereof and a kind of sodium-ion battery, by the way that curing nickel particles to be dispersed in nitrogenous polypropylene
In nitrile carbon skeleton, it has been able to suppress the Volumetric expansion of curing nickel particles, and has effectively improved leading for entire negative electrode material
Electrically, good cyclical stability and high rate performance are obtained.It is environmentally protective for the production method of electrostatic spinning, simple process,
Yield is high, and is easily achieved commercialization.
The present invention in order to solve the above problem provided by technical solution are as follows: a kind of one-dimensional N doping curing nickel porous fibre
Anode material of lithium-ion battery, it is characterised in that: including porous nano-fibre skeleton and curing nickel nano particle；Two sulphur
Change surface and inside that nickel nano particle is evenly dispersed in porous nano-fibre skeleton.
Preferably, the curing nickel nano particle is crystal, chemical formula NiS2, belong to cubic system, cell parameter a
=b=c=5.67, α=β=γ=90 °.
Preferably, the partial size of the curing nickel nano particle is 5nm~10nm, the NiS2The diameter of/C porous fibre
For 400nm~600nm.
A kind of preparation method of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery, the method packet
Include following steps,
A), 80 DEG C of required solvent N,N-dimethylformamide are dried；
B), nickel source, pore creating material and polyacrylonitrile are added in n,N-Dimethylformamide, stirring 20h to uniform slurries；
C), uniform slurries are extracted with the syringe of 5ml, are placed in electrostatic spinning machine and are carried out spinning；
D), the fiber for finishing spinning is placed in tube furnace, under air conditions, with the heating rate liter of 1~4 DEG C/min
Temperature keeps the temperature 2~4h to 300 DEG C~400 DEG C；
E), fast with the heating of 1~4 DEG C/min under the conditions of argon gas by sample putting tube formula furnace calcine in step d)
Rate is warming up to 1000 DEG C~1200 DEG C, keeps the temperature 2~4h；
F), sample calcine in step e) is mixed with sulphur powder, in placement tube furnace, under the conditions of argon gas, with 1~4 DEG C/
The heating rate of min is warming up to 400~600 DEG C, keeps the temperature 1~3h to get the negative electrode material；
G), the one-dimensional N doping NiS that will be prepared2/ C porous fibre is assembled into sodium-ion battery, and tests its sodium ion
Battery performance.
Preferably, nickel source is nickel acetylacetonate in the step b), and pore creating material is polymethyl methacrylate, described poly- third
Contain nitrogen source in alkene nitrile, the nickel source: pore creating material: mass ratio=1 of polyacrylonitrile~5:1~10:1.
Preferably, electrospinning parameters in the step c) are as follows: spinning temperature is 25 DEG C~35 DEG C, and spray speed is 0.05ml/
Min~0.2ml/min, voltage are 20kv~26kv, and positive and negative anodes spacing is 20cm~30cm.
Preferably, sample and the doping mass ratio of sulphur powder are 1:3 in the step f).
A kind of sodium-ion battery, including a kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery.
Compared with prior art, the invention has the advantages that the present invention is using nitrogenous polyacrylonitrile as carbon source, without additional
N doping；Using nickel acetylacetonate as nickel source, using polymethyl methacrylate as pore creating material, using sulphur powder as sulphur source；Raw material exists
N,N-Dimethylformamide has good dissolubility, and the curing nickel particles as active material is made to be evenly dispersed in carbon nanometer
On fiber.This nitrogenous porous fibrous structure can greatly improve the electric conductivity and Particle Delivery performance of material, while again can be very
The volume expansion of good inhibition curing nickel particles, obtains good chemical property.In 0.1A g-1Current density under, electricity
Tankage is up to 510mAh g-1, recycled by 100 circles, battery can still keep 430mAh g-1Capacity, cyclical stability
Very well.In addition, the production technology of electrostatic spinning is relatively simple, yield is high, is easy to be commercialized.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.
Fig. 1 is that present invention specific implementation preparation process obtains the X-ray diffractogram of product.
Fig. 2 is that present invention specific implementation preparation process obtains the field emission scanning electron microscope figure of product.
Fig. 3 is that present invention specific implementation preparation process obtains the transmission electron microscope electron microscope of product.
Fig. 4 is the electrochemistry cycle performance figure of electrode material prepared by present invention specific implementation preparation process.
Fig. 5 is the electrochemistry high rate performance figure of electrode material prepared by present invention specific implementation preparation process.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with accompanying drawings and embodiments, how the present invention is applied whereby
Technological means solves technical problem and reaches the realization process of technical effect to fully understand and implement.
Embodiment 1
A kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery, it is characterised in that: including porous
Nanofibrous Scaffolds and curing nickel nano particle；The curing nickel nano particle is evenly dispersed in porous nano-fibre bone
The surface and inside of frame；
The curing nickel nano particle is crystal, chemical formula NiS2, belong to cubic system, cell parameter a=b=c
=5.67, α=β=γ=90 °.
The partial size of the curing nickel nano particle is 5nm~10nm, the NiS2The diameter of/C porous fibre is 400nm
~600nm.
A kind of preparation method of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery, the method packet
Include following steps,
A), 80 DEG C of required solvent N,N-dimethylformamide are dried；
B), nickel source, pore creating material and polyacrylonitrile are added in n,N-Dimethylformamide, stirring 20h to uniform slurries；
C), uniform slurries are extracted with the syringe of 5ml, are placed in electrostatic spinning machine and are carried out spinning；
D), the fiber for finishing spinning is placed in tube furnace, under air conditions, with the heating rate liter of 1~4 DEG C/min
Temperature keeps the temperature 2~4h to 300 DEG C~400 DEG C；
E), fast with the heating of 1~4 DEG C/min under the conditions of argon gas by sample putting tube formula furnace calcine in step d)
Rate is warming up to 1000 DEG C~1200 DEG C, keeps the temperature 2~4h；
F), sample calcine in step e) is mixed with sulphur powder, in placement tube furnace, under the conditions of argon gas, with 1~4 DEG C/
The heating rate of min is warming up to 400~600 DEG C, keeps the temperature 1~3h to get the negative electrode material；
G), the one-dimensional N doping NiS that will be prepared2/ C porous fibre is assembled into sodium-ion battery, and tests its sodium ion
Battery performance.
Nickel source is nickel acetylacetonate in the step b), and pore creating material is polymethyl methacrylate, in the polyacrylonitrile
Containing nitrogen source, the nickel source: pore creating material: mass ratio=1 of polyacrylonitrile~5:1~10:1.
Electrospinning parameters in the step c) are as follows: spinning temperature be 25 DEG C~35 DEG C, spray speed be 0.05ml/min~
0.2ml/min, voltage are 20kv~26kv, and positive and negative anodes spacing is 20cm~30cm.
Sample and the doping mass ratio of sulphur powder are 1:3 in the step f).
A kind of sodium-ion battery, including a kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery.
Embodiment 2
1. preprocessing process；
10ml n,N-Dimethylformamide is first taken to put in an oven, 80 DEG C of dry 12h；Take 1g polyacrylonitrile, the poly- first of 0.5g
Base methyl acrylate and 1g nickel acetylacetonate are added in dried 10ml n,N-Dimethylformamide solution, stir 12h,
Obtain uniform slurries.
2. electrostatic spinning process；
Uniform slurries are extracted with 5ml syringe, are put into electrostatic spinning machine, and adjustment positive and negative anodes spacing is 15cm, setting electricity
Pressure is 26kv, and slurries spray speed is 0.08ml/min.Spinning machine temperature is adjusted to 30 DEG C.
3. stable and poration process；
The fiber of spinning is placed in the tube furnace of air atmosphere, is warming up to 350 with the heating rate of 2 DEG C/min
DEG C, keep the temperature 2h, cooled to room temperature after fully reacting；Fibrous material after stabilization is placed on to the tube furnace of argon atmosphere again
In, 1200 DEG C are warming up to the heating rate of 2 DEG C/min, keeps the temperature 2h, cooled to room temperature after fully reacting.
4. sulfidation
Calcined black powder and sulphur powder mixed grinding (1:3) are placed in the tube furnace of argon atmosphere, with 2 DEG C/
The heating rate of min is warming up to 500 DEG C, keeps the temperature 2h, cooled to room temperature after fully reacting.Obtain one-dimensional N doping
NiS2/ C porous fibre anode material of lithium-ion battery.
5. performance test process；
It will obtain powder and be prepared into button-shaped sodium-ion battery, specific steps are as follows: by active material powder, conductive agent
(Super P) and binder (carboxymethyl cellulose CMC) are made so that a small amount of deionized water is added after the mass ratio grinding uniformly of 8:1:1
Slurry is applied on copper foil by slurry with coating device, then by it in a vacuum drying oven with 100 DEG C of heat preservation 18h.Then it will dry
Good electrode slice is cut into the electrode slice that diameter is 12mm with slicer, with metallic sodium is finally to electricity in glove box by electrode slice
Pole is assembled into sodium ion button cell.It is taken out after being placed one day in glove box, carries out electro-chemical test with blue electric system.
The beneficial effects of the present invention are: the present invention is using nitrogenous polyacrylonitrile as carbon source, without additional N doping；With second
Acyl acetone nickel is nickel source, using polymethyl methacrylate as pore creating material, using sulphur powder as sulphur source；Raw material is in N, N- dimethyl methyl
Amide has good dissolubility, is evenly dispersed in the curing nickel particles as active material on carbon nano-fiber.It is this
Nitrogenous porous fibrous structure can greatly improve the electric conductivity and Particle Delivery performance of material, while can inhibit two sulphur well again
The volume expansion for changing nickel particles, obtains good chemical property.In 0.1A g-1Current density under, battery capacity is up to
510mAh g-1, recycled by 100 circles, battery can still keep 430mAh g-1Capacity, cyclical stability is fine.In addition,
The production technology of electrostatic spinning is relatively simple, and yield is high, is easy to be commercialized.
Only highly preferred embodiment of the present invention is described above, but is not to be construed as limiting the scope of the invention.This
Invention is not only limited to above embodiments, and specific structure is allowed to vary.All protection models in independent claims of the present invention
Interior made various change is enclosed to all fall in the scope of protection of the present invention.
Claims (8)
1. a kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery, it is characterised in that: received including porous
Rice fiber skeleton and curing nickel nano particle；The curing nickel nano particle is evenly dispersed in porous nano-fibre skeleton
Surface and inside.
2. a kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery according to claim 1,
Be characterized in that: the curing nickel nano particle is crystal, chemical formula NiS2, belong to cubic system, cell parameter a=b=c
=5.67, α=β=γ=90 °.
3. a kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery according to claim 1,
Be characterized in that: the partial size of the curing nickel nano particle is 5nm~10nm, the NiS2The diameter of/C porous fibre is
400nm~600nm.
4. a kind of preparation method of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery, it is characterised in that:
It the described method comprises the following steps,
A), 80 DEG C of required solvent N,N-dimethylformamide are dried；
B), nickel source, pore creating material and polyacrylonitrile are added in n,N-Dimethylformamide, stirring 20h to uniform slurries；
C), uniform slurries are extracted with the syringe of 5ml, are placed in electrostatic spinning machine and are carried out spinning；
D), the fiber for finishing spinning is placed in tube furnace, under air conditions, is warming up to the heating rate of 1~4 DEG C/min
300 DEG C~400 DEG C, keep the temperature 2~4h；
E), by the sample putting tube formula furnace calcined in step d), under the conditions of argon gas, with the heating rate liter of 1~4 DEG C/min
Temperature keeps the temperature 2~4h to 1000 DEG C~1200 DEG C；
F), the sample calcined in step e) is mixed with sulphur powder, is placed in tube furnace, under the conditions of argon gas, with 1~4 DEG C/min
Heating rate be warming up to 400~600 DEG C, keep the temperature 1~3h to get the negative electrode material；
G), the one-dimensional N doping NiS that will be prepared2/ C porous fibre is assembled into sodium-ion battery, and tests its sodium-ion battery
Energy.
5. a kind of system of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery according to claim 4
Preparation Method, it is characterised in that: nickel source is nickel acetylacetonate in the step b), and pore creating material is polymethyl methacrylate, described
Contain nitrogen source in polyacrylonitrile, the nickel source: pore creating material: mass ratio=1 of polyacrylonitrile~5:1~10:1.
6. a kind of system of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery according to claim 4
Preparation Method, it is characterised in that: electrospinning parameters in the step c) are as follows: spinning temperature is 25 DEG C~35 DEG C, and spray speed is
0.05ml/min~0.2ml/min, voltage are 20kv~26kv, and positive and negative anodes spacing is 20cm~30cm.
7. a kind of system of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery according to claim 4
Preparation Method, it is characterised in that: sample and the doping mass ratio of sulphur powder are 1:3 in the step f).
8. a kind of sodium-ion battery, it is characterised in that: including a kind of one-dimensional two sulphur of N doping a method according to any one of claims 1-3
Change nickel porous fibre anode material of lithium-ion battery.
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| CN201910174877.5A CN109888239A (en) | 2019-03-08 | 2019-03-08 | A kind of one-dimensional N doping curing nickel porous fibre anode material of lithium-ion battery and preparation method thereof and a kind of sodium-ion battery |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112133886A (en) * | 2020-08-12 | 2020-12-25 | 南昌航空大学 | Preparation method and application of in-situ integrated electrode for alkali ion battery |
| CN112582618A (en) * | 2020-12-14 | 2021-03-30 | 安徽大学 | Preparation method of nickel sulfide nanosheet anchored on inner surface of nitrogen-containing hollow carbon substrate, prepared product and application of product |
| CN113036097A (en) * | 2021-02-04 | 2021-06-25 | 淮阴工学院 | Sulfur vacancy nitrogen doped carbon coated nickel sulfide composite electrode material and preparation method thereof |
| CN113036092A (en) * | 2021-03-10 | 2021-06-25 | 安徽大学 | Preparation method of flexible membrane, prepared flexible membrane and battery |
| CN113279091A (en) * | 2021-07-22 | 2021-08-20 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Porous carbon fiber, preparation method thereof and sodium ion battery |
| CN113314715A (en) * | 2021-05-20 | 2021-08-27 | 广州大学 | Nickel sulfide composite material and preparation method and application thereof |
| CN114142025A (en) * | 2021-11-26 | 2022-03-04 | 桂林理工大学 | Bimetal sulfide @ porous carbon fiber composite material, preparation method thereof and application thereof in sodium ion battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112133886A (en) * | 2020-08-12 | 2020-12-25 | 南昌航空大学 | Preparation method and application of in-situ integrated electrode for alkali ion battery |
| CN112582618A (en) * | 2020-12-14 | 2021-03-30 | 安徽大学 | Preparation method of nickel sulfide nanosheet anchored on inner surface of nitrogen-containing hollow carbon substrate, prepared product and application of product |
| CN113036097A (en) * | 2021-02-04 | 2021-06-25 | 淮阴工学院 | Sulfur vacancy nitrogen doped carbon coated nickel sulfide composite electrode material and preparation method thereof |
| CN113036092A (en) * | 2021-03-10 | 2021-06-25 | 安徽大学 | Preparation method of flexible membrane, prepared flexible membrane and battery |
| CN113036092B (en) * | 2021-03-10 | 2022-06-21 | 安徽大学 | Preparation method of flexible membrane, prepared flexible membrane and battery |
| CN113314715A (en) * | 2021-05-20 | 2021-08-27 | 广州大学 | Nickel sulfide composite material and preparation method and application thereof |
| CN113279091A (en) * | 2021-07-22 | 2021-08-20 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Porous carbon fiber, preparation method thereof and sodium ion battery |
| CN114142025A (en) * | 2021-11-26 | 2022-03-04 | 桂林理工大学 | Bimetal sulfide @ porous carbon fiber composite material, preparation method thereof and application thereof in sodium ion battery |
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