CN106252636A - A kind of lithium ion battery hollow NiO/C nanofiber anode material and preparation method thereof - Google Patents
A kind of lithium ion battery hollow NiO/C nanofiber anode material and preparation method thereof Download PDFInfo
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- CN106252636A CN106252636A CN201610881725.5A CN201610881725A CN106252636A CN 106252636 A CN106252636 A CN 106252636A CN 201610881725 A CN201610881725 A CN 201610881725A CN 106252636 A CN106252636 A CN 106252636A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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Abstract
The invention discloses a kind of lithium ion battery hollow NiO/C nanofiber anode material and preparation method thereof, this composite nano fiber prepares through heat treatment method after using electrostatic spinning technique, synthesis technique is simple, gained average fibre diameter is 180nm, the hollow nickel oxide nanosphere formed is evenly distributed in carbon nano-fiber inside and surface, and the diameter Distribution of hollow ball is 8～40nm.This material is used for preparing negative pole piece of battery, has good rate capability, an advantage that security performance is high.
Description
Technical field
The present invention relates to a kind of new type lithium ion battery hollow NiO/C nanofiber anode material and preparation method thereof, belong to
In technical field of lithium ion.
Technical background
Owing to lithium ion battery has high energy density, excellent cyclical stability and good environment friendly,
The most universal in the mobile electronic devices such as mobile phone, notebook computer and digital camera.In recent years in order to reduce energy danger
Machine and environmental pollution, lithium ion battery starts to set foot in large-scale energy storage and power-equipment, develops energy density height, has extended cycle life
The electrode material of the new type lithium ion battery good with security performance is extremely urgent.The negative material security performance to lithium ion battery
Play a key effect.Graphite is the commercialization lithium cell negative pole material of current main flow, as lithium battery most widely used on market
Negative material, the theoretical specific capacity of graphite is only 372mA h g-1, including native graphite, CNT etc..Due to graphite itself
The restriction of architectural characteristic, the development of graphite cathode material also encounters bottleneck, such as specific capacity and has arrived at the limit, can not meet
Lasting large current discharging capability etc. required by large-sized power battery, thus limit their actual application.Therefore ratio is found
Capacity is of a relatively high, good cycling stability and the relatively cheap negative material of price become the research emphasis of people.
In recent decades, (～the 718mA h g because the outstanding theoretical capacity of nickel oxide-1), chemically and thermally stability, storage
Amount is abundant it is considered to be a negative material candidate the most promising.The nickel oxide material of many dissimilar nanostructureds
Studied, in order to realize the lithium ion storage of excellence.Despite many effort, the energy density of nickel oxide, high rate performance and follow
Ring stability still existing defects.Here, it is proposed that the hollow NiO cluster of a kind of novelty is combined one-dimensional carbon nano-fiber knot
Structure meets the chemical property demand of lithium ion battery as high power negative material.In the present invention, utilize the most efficiently
Electrostatic spinning technique hollow NiO cluster is combined with one-dimensional carbon nano-fiber, treated obtain hollow NiO/C nanofiber.
This material is used for preparing negative pole piece of battery, has good rate capability, an advantage that security performance is high.
Summary of the invention
It is an object of the invention to for above-mentioned technical Analysis, it is provided that a kind of Novel anode material for lithium ion battery,
Using compound to transition metal oxide hollow nanospheres and the carbon nano-fiber theory as lithium ion battery negative material, to improve
The performance of lithium ion battery negative material.
Technical scheme:
For achieving the above object, the present invention is by the following technical solutions: utilize electrostatic spinning technique by nickel salt and carbon
Fiber composite, obtains Ni/C nanofiber through subsequent heat treatment, then obtains hollow type NiO/C nanofiber, institute through peroxidating
That states hollow ball is formed as Kinkendal Effect, a diameter of 1O0～200nm of this composite nano fiber.
A kind of above-mentioned lithium ion battery hollow NiO/C nanofiber anode material and preparation method thereof, its step is as follows:
(1) preparation of spinning solution, is slowly dissolve into 30mL dimethylformamide by 3.4020g polyacrylonitrile (PAN)
(DMF) in, and stir to being completely dissolved；Then add 1.7010g tetra-water nickel acetate to continue to be stirred to be completely dissolved, obtain all
Even, transparent, stable green spinning solution；
(2) spinning solution obtained in (1) is moved in electrostatic spinning apparatus, carry out electrostatic spinning obtain polymer-
Nickel salt composite precursor fiber；
(3) the composite precursor fiber (2) collected is in atmosphere after pre-oxidation, in noble gas argon atmosphere
Under the conditions of through carbonization treatment, more in atmosphere after peroxidating, obtain hollow NiO/C composite nano fiber；
Described in step (1), in spinning solution, the mass fraction of nickel acetate is 5.07%；The mass fraction of polyacrylonitrile is
10.14%；
Described in step (2), electrostatic spinning process parameter is: voltage 25kV, sprays needle diameter 0.3mm, and solution advances speed
Rate 0.1mL/h, solidification distance is 15cm, and temperature is 20～30 DEG C, and humidity is less than 40%；
Pre-oxidizing design parameter described in step (3) is: temperature is 280 DEG C, temperature retention time 4h, heating rate is 1 DEG C/
min；
Described in step (3), carbonization treatment design parameter is: temperature is 700 DEG C, and atmosphere is argon, and temperature retention time is 2h,
Heating rate is 2 DEG C/min；
Described in step (3), oxidation processes design parameter is: temperature is 300 DEG C, and temperature retention time is 2h, and heating rate is 1
℃/min；
The invention have the advantage that and first transition metal salt and carbon source electrostatic spinning are combined into nanofiber, through overheated
Process obtains transition metal oxide hollow nanospheres and is applied to lithium ion battery industry with carbon nano-fiber composite material, this material
Material shows higher capacity and excellent cyclical stability, at 50mA g-1Electric current density under, first discharge capacity up to
1629.1mA h·g-1, after circulation 20 circle, capacity remains to be maintained at 974.3mA h g-1, compared with pure carbon nano-fiber materials,
It is higher that described NiO/C nanofiber lithium ion battery negative material has capacity, the feature that multiplying power is good and performance is more stable.
Accompanying drawing explanation
The SEM photograph of hollow NiO/C nanofiber prepared in Fig. 1: embodiment 1；
The TEM photo of hollow NiO/C nanofiber prepared in Fig. 2: embodiment 1；
The HRTEM photo of hollow NiO/C nanofiber prepared in Fig. 3: embodiment 1；
Fig. 4: the XRD photo of hollow NiO/C nanofiber prepared in embodiment 1-5；
The high rate performance curve being assembled into button cell of hollow NiO/C nanofiber prepared in Fig. 5: embodiment 1
Figure.
Detailed description of the invention
Embodiment 1
1) preparation of Ni/C composite nano fiber presoma: 3.4020g polyacrylonitrile (PAN) is slowly dissolve into 30mL bis-
In methylformamide (DMF), and stir to being completely dissolved；Then add 1.7010g tetra-water nickel acetate to continue to be stirred to completely
Dissolve, obtain uniform, transparent, stable green spinning solution, the spinning solution obtained is moved in electrostatic spinning apparatus, enters
Row electrostatic spinning obtains polymer-nickel salt composite precursor fiber；
(2) preparation of Ni/C composite nano fiber: the composite precursor fiber collected is paved on plate glass solid
Reserve, put in Muffle furnace, after calcining 4h with the heating rate of 1 DEG C/min to 280 DEG C in atmosphere, then move in tube furnace,
Under noble gas argon atmospheric condition, calcine 2h with the heating rate of 2 DEG C/min to 700 DEG C, obtain Ni/C composite Nano fine
Dimension, places in Muffle furnace, is 300 DEG C with temperature, and temperature retention time is 2h, and heating rate is 1 DEG C/min, after peroxidating,
To hollow NiO/C composite nano fiber；
As it is shown in figure 1, the SEM figure of prepared hollow NiO/C composite nano fiber, upper right corner illustration is that fibre diameter divides
Cloth, average diameter is 180nm, and lower-left figure is the enlarged drawing of fiber, it may be clearly seen that fiber surface has granule to separate out.Such as figure
Shown in 2, hollow ball is entrained in composite nano fiber equably.Fig. 3 is the HRTEM picture of hollow NiO/C composite nano fiber,
Can be seen that hollow nickel oxide nano bulb diameter is about 15nm.Above-mentioned sample is carried out the analysis of the Nomenclature Composition and Structure of Complexes, during Fig. 4 is
The XRD spectra of empty NiO/C composite nano fiber, can be observed from figure ,～the diffraction maximum that peak is graphitized carbon of 26 °, except
Outside the diffraction maximum of nickel, also diffraction maximum matches with the standard card PDF#47-1049 of nickel oxide, answers so sample is NiO/C
Close nanofiber.
Embodiment 2
Same as in Example 1, simply oxidation temperature retention time is become 0min.This composite is as lithium ion battery negative
Material, at 50mA g-1Electric current density under, initial charge capacity is up to 1048.6mA h g-1, after circulation 20 circle, capacity is still
511mA h g can be maintained at-1。
Embodiment 3
Same as in Example 1, simply oxidation temperature retention time is become 1h.This composite is as lithium ion battery negative material
Material, at 50mA g-1Electric current density under, initial charge capacity is up to 823.9mA h g-1, after circulation 100 circle, capacity remains to
It is maintained at 600.5mA h g-1。
Embodiment 4
Same as in Example 1, simply oxidation temperature retention time is become 3h.This composite is as lithium ion battery negative material
Material, at 50mA g-1Electric current density under, initial charge capacity is up to 1218.6mA h g-1, after circulation 100 circle, capacity remains to
It is maintained at 181.7mA h g-1。
Embodiment 5
Same as in Example 1, simply oxidation temperature retention time is become 4h.This composite is as lithium ion battery negative material
Material, at 50mA g-1Electric current density under, initial charge capacity is up to 1080mA h g-1, after circulation 100 circle, capacity remains to protect
Hold at 69.1mA h g-1。
Claims (4)
1. an its preparation method for lithium ion battery hollow NiO/C nanofiber anode material, its step is as follows:
(1) preparation of spinning solution, is slowly dissolve into 30mL dimethylformamide (DMF) by 3.4020g polyacrylonitrile (PAN)
In, and stir to being completely dissolved, add 1.7010g nickel acetate tetrahydrate and continue to be stirred to be completely dissolved, obtain uniform, saturating
Bright, stable green spinning solution；
(2) spinning solution obtained in (1) is moved in electrostatic spinning apparatus, carries out electrostatic spinning and obtain polymer-nickel salt
Composite precursor fiber；
(3) the composite precursor fiber (2) collected is in atmosphere after pre-oxidation, at noble gas argon atmospheric condition
Lower through carbonization treatment, more in atmosphere after peroxidating, obtain hollow NiO/C composite nano fiber.
The preparation method of a kind of lithium ion battery hollow NiO/C nanofiber anode material the most as claimed in claim 1, it is special
Levy and be: in gained NiO/C composite nano fiber, the mass fraction of nickel oxide is 30～40%.
The preparation method of a kind of lithium ion battery hollow NiO/C nanofiber anode material the most as claimed in claim 1, it is special
To levy and be: pre-oxidizing design parameter described in (3) is: temperature is 250～280 DEG C, temperature retention time 4h, heating rate is 1 DEG C/
min；Carbonization treatment design parameter is: temperature is 500～700 DEG C, and temperature retention time is 2h, and heating rate is 2 DEG C/min；At oxidation
Reason design parameter is: temperature is 300 DEG C, and temperature retention time is 1～4h, and heating rate is 1 DEG C/min.
The preparation method of a kind of lithium ion battery hollow NiO/C nanofiber anode material the most as claimed in claim 1, it is special
Levy and be: hollow type NiO is evenly distributed in carbon nano-fiber, and diameter is 8～40nm.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107956000A (en) * | 2017-12-29 | 2018-04-24 | 济南大学 | A kind of synthetic method and products obtained therefrom of NiO multistages doughnut |
| CN108346787A (en) * | 2018-01-24 | 2018-07-31 | 浙江衡远新能源科技有限公司 | Hollow carbon nano-fiber lithium cell cathode material of a kind of high power capacity TiO2-VO2 doping and preparation method thereof |
| CN108642606A (en) * | 2018-04-11 | 2018-10-12 | 西安交通大学 | Cobaltosic oxide/carbon nano-fiber composite material and its preparation method and application |
| CN109004185A (en) * | 2018-06-13 | 2018-12-14 | 福建翔丰华新能源材料有限公司 | Method for preparing independent negative electrode material of flexible lithium ion battery |
| CN109037554A (en) * | 2018-06-26 | 2018-12-18 | 长沙矿冶研究院有限责任公司 | A kind of Ni/C composite nano-fiber membrane applied to lithium-sulfur cell and preparation method thereof and lithium-sulfur cell |
| CN109589982A (en) * | 2018-12-26 | 2019-04-09 | 大连工业大学 | A kind of preparation method of nickel oxide-base composite semiconductor nanofiber |
| CN110416495A (en) * | 2019-06-26 | 2019-11-05 | 广东工业大学 | A kind of CNF- metallic compound absolute electrode material and its preparation method and application |
| CN110970628A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | Nano carbon fiber and metal composite electrode and application thereof |
| CN111092204A (en) * | 2019-12-12 | 2020-05-01 | 银隆新能源股份有限公司 | Hollow carbon fiber modified silicon-carbon material, preparation method and application thereof |
| CN111659439A (en) * | 2020-06-02 | 2020-09-15 | 南京师范大学 | Nitrogen-doped carbon nano composite material loaded with NiS/NiO heterojunction and preparation method and application thereof |
| CN114975970A (en) * | 2022-07-01 | 2022-08-30 | 长春理工大学 | Carbon nano tube/tin dioxide nano composite material and preparation method and application thereof |
| CN115893528A (en) * | 2022-11-01 | 2023-04-04 | 安徽大学 | Magnetic metal nanotube with controllable specific surface pipe diameter and preparation method and application thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107956000B (en) * | 2017-12-29 | 2019-11-08 | 济南大学 | A kind of synthetic method and products obtained therefrom of NiO multistage doughnut |
| CN107956000A (en) * | 2017-12-29 | 2018-04-24 | 济南大学 | A kind of synthetic method and products obtained therefrom of NiO multistages doughnut |
| CN108346787A (en) * | 2018-01-24 | 2018-07-31 | 浙江衡远新能源科技有限公司 | Hollow carbon nano-fiber lithium cell cathode material of a kind of high power capacity TiO2-VO2 doping and preparation method thereof |
| CN108642606A (en) * | 2018-04-11 | 2018-10-12 | 西安交通大学 | Cobaltosic oxide/carbon nano-fiber composite material and its preparation method and application |
| CN109004185A (en) * | 2018-06-13 | 2018-12-14 | 福建翔丰华新能源材料有限公司 | Method for preparing independent negative electrode material of flexible lithium ion battery |
| CN109004185B (en) * | 2018-06-13 | 2021-12-24 | 福建翔丰华新能源材料有限公司 | Method for preparing independent negative electrode material of flexible lithium ion battery |
| CN109037554A (en) * | 2018-06-26 | 2018-12-18 | 长沙矿冶研究院有限责任公司 | A kind of Ni/C composite nano-fiber membrane applied to lithium-sulfur cell and preparation method thereof and lithium-sulfur cell |
| CN110970628A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | Nano carbon fiber and metal composite electrode and application thereof |
| CN109589982B (en) * | 2018-12-26 | 2021-05-18 | 大连工业大学 | Preparation method of nickel oxide-based composite semiconductor nanofiber |
| CN109589982A (en) * | 2018-12-26 | 2019-04-09 | 大连工业大学 | A kind of preparation method of nickel oxide-base composite semiconductor nanofiber |
| CN110416495A (en) * | 2019-06-26 | 2019-11-05 | 广东工业大学 | A kind of CNF- metallic compound absolute electrode material and its preparation method and application |
| CN111092204A (en) * | 2019-12-12 | 2020-05-01 | 银隆新能源股份有限公司 | Hollow carbon fiber modified silicon-carbon material, preparation method and application thereof |
| CN111659439A (en) * | 2020-06-02 | 2020-09-15 | 南京师范大学 | Nitrogen-doped carbon nano composite material loaded with NiS/NiO heterojunction and preparation method and application thereof |
| CN111659439B (en) * | 2020-06-02 | 2023-04-07 | 南京师范大学 | Nitrogen-doped carbon nano composite material loaded with NiS/NiO heterojunction and preparation method and application thereof |
| CN114975970A (en) * | 2022-07-01 | 2022-08-30 | 长春理工大学 | Carbon nano tube/tin dioxide nano composite material and preparation method and application thereof |
| CN115893528A (en) * | 2022-11-01 | 2023-04-04 | 安徽大学 | Magnetic metal nanotube with controllable specific surface pipe diameter and preparation method and application thereof |
| CN115893528B (en) * | 2022-11-01 | 2024-02-20 | 安徽大学 | Magnetic metal nanotube with controllable specific surface pipe diameter and preparation method and application thereof |
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