CN108682802A - A method of preparing lithium cell negative pole shell-core structure nanofiber - Google Patents
A method of preparing lithium cell negative pole shell-core structure nanofiber Download PDFInfo
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- CN108682802A CN108682802A CN201810379525.9A CN201810379525A CN108682802A CN 108682802 A CN108682802 A CN 108682802A CN 201810379525 A CN201810379525 A CN 201810379525A CN 108682802 A CN108682802 A CN 108682802A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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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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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention discloses a kind of method preparing lithium cell negative pole core-shell structure nanofiber, includes following steps：（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre nuclear structure precursor solution；（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre is formd；（3）Composite nanometer fiber felt is prepared according to electrospinning parameters using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure, after 1 2h is pre-oxidized at 260 280 DEG C, be carbonized under argon gas atmosphere protection between 800 1000 DEG C 3 6h.By first configuring the precursor solution of nuclear structure and the precursor solution of shell structure, then by coaxial electrostatic spinning technology it is simple and practicable prepare Si-C composite material that is with good chemical property and can apply to lithium ion battery negative material, meet the needs used.
Description
Technical field
The present invention relates to chemical material field technology, refer in particular to a kind of preparing lithium cell negative pole shell-core structure Nanowire
The method of dimension.
Background technology
Due to its unprecedented theoretical capacity -4000mAh/g, almost decuple existing commercial graphite cathode-silicon at
For most promising lithium cell negative pole material now.In answering for the extensive energy storage such as such as electric vehicle and utility network
It uses, application prospect seems more tempting, but silicon also has the shortcomings that cycle life is of short duration simultaneously.
The volume expansion and contraction that the of short duration cycle life main contributor of silicon moves in circles when it is in cycle.In the body of silicon
When product changes, capacity, which declines, mainly has these failure mechanisms in action：First, silicon its volume in complete lithiumation is swollen
It is swollen to reach 300%, at this time caused by pressure silicon can be pressed into fine powder completely.This crushing is obviously related with capacity decline,
Because therefore active material loses with collector and is conductively connected；Second is that silicon can be disconnected with carbon conductor such as conductive black,
Based on same reason, silicon electrode film also can be peeled off easily above collector very much；Third, volume change can cause
The SEI films of silicon face are unstable.During repetitive cycling, since the volume change SEI films of silicon are forming always crack, and pass through
These cracks are ceaselessly being grown.To the last, SEI films it is too thick so that lithium ion can not spread or electrolyte by
It has been depleted to a degree totally.
For first failure mechanism, someone obtains scheme to solve the problems, such as by using the silicon of nanostructure：Because
The silicon of small size can relax those since volume is widely varied caused pressure.Although having there is some successful examples
Prove that this method is feasible, but its production technology is more complex, and the silicon of nanostructure is typically produced by CVD method, this is not only
Pressure, temperature, oxygen concentration are required, it is also necessary to the help of additional catalyst or surfactant.
Invention content
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of lithium electricity for preparing to bear
The method of pole shell-core structure nanofiber, by coaxial electrostatic spinning technology it is simple and practicable prepare with good
Chemical property and the Si-C composite material that can apply to lithium ion battery negative material.
To achieve the above object, the present invention is using following technical solution：
A method of lithium cell negative pole shell-core structure nanofiber is prepared, includes following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The mass concentration of the precursor solution of nuclear structure, silicon nano is 4%-6%, and the mass concentration of PMMA is 8%-12%；Nuclear structure
Precursor solution 6-8h has been dispersed with stirring in 50-80 DEG C of environment；
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre is formd, quality is dense
Degree is 8%-12%；The precursor solution of shell structure has been dispersed with stirring 6-8h in 50-80 DEG C of environment；
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio is 1:
2-3:Between 4, apply voltage between 10-15kV, receive distance between 9-14cm, reception device is the reception with aluminium foil
Device；Compound receive is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Rice fibrofelt, after pre-oxidizing 1-2h at 260-280 DEG C, be carbonized under argon gas atmosphere protection between 800-1000 DEG C 3-6h.
As a preferred embodiment, the volume ratio of the molten middle DMF of the mixing of the DMF and acetone and acetone is 1：1.
The present invention has clear advantage and advantageous effect compared with prior art, specifically, by above-mentioned technical proposal
Known to：
By first configuring the precursor solution of nuclear structure and the precursor solution of shell structure, then pass through coaxial electrostatic spinning technology
It is compound that silicon-carbon that is with good chemical property and can apply to lithium ion battery negative material is prepared simple and practicablely
Material meets the needs used.
Description of the drawings
Fig. 1 is the SEM figures of silicon-carbon composite fibre in the present invention；
The charge and discharge potential of different cycle-indexes divides under first charge-discharge gesture distribution map, (B) 2.75 A/g under Fig. 2 (A) C/10
Charge and discharge potential profile under Butut, the multiplying power test chart of (C) composite material, (D) different multiplying.
Specific implementation mode
Present invention is disclosed a kind of methods preparing lithium cell negative pole shell-core structure nanofiber, include following steps：
（1）By silicon nano and PMMA（Polymethyl methacrylate）It is dissolved in DMF（N,N-dimethylformamide）With acetone
Mixing it is molten in form finally obtained composite fibre nuclear structure precursor solution, the mass concentration of silicon nano is
The mass concentration of 4%-6%, PMMA are 8%-12%；The precursor solution of nuclear structure has been dispersed with stirring 6-8h in 50-80 DEG C of environment；
The molten middle DMF of mixing of the DMF and acetone and the volume ratio of acetone are 1：1.
（2）By PAN（Pantoprazole）It is dissolved in DMF, before foring the shell structure in finally obtained composite fibre
Drive liquid solution, mass concentration 8%-12%；The precursor solution of shell structure has been dispersed with stirring 6-8h in 50-80 DEG C of environment.
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio
It is 1:2-3:Between 4, apply voltage between 10-15kV, receive distance between 9-14cm, reception device is with aluminium foil
Reception device；It is prepared again according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Nanofiber mats are closed, after pre-oxidizing 1-2h at 260-280 DEG C, be carbonized under argon gas atmosphere protection between 800-1000 DEG C 3-
6h。
With multiple embodiments, invention is further described in detail below：
Embodiment 1：
A method of lithium cell negative pole shell-core structure nanofiber is prepared, includes following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The precursor solution of nuclear structure, the mass concentration that the mass concentration of silicon nano is 4%, PMMA is 9%；The presoma of nuclear structure
Solution has been dispersed with stirring 6h in 50 DEG C of environment；The molten middle DMF of mixing of the DMF and acetone and the volume ratio of acetone are 1：1.
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre, matter are formd
Measure a concentration of 9%；The precursor solution of shell structure has been dispersed with stirring 7h in 70 DEG C of environment.
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio
It is 1:Between 2, apply voltage between 10kV, receive distance between 9cm, reception device is the reception device with aluminium foil；
Composite Nano fibre is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Felt is tieed up, after pre-oxidizing 1h at 270 DEG C, be carbonized under argon gas atmosphere protection between 800 DEG C 3h.
As shown in Figure 1, in the present embodiment, the SEM of silicon-carbon composite fibre schemes（A）（B）（C）And figure（D）TEM and white
Selective electron diffraction pattern in frame shows Si nano-particle integrated distributions in fibrous inside.
The Electrochemical results of the Si-C composite material of the shell-core structure prepared using coaxial electrostatic spinning method show it
Cycle performance is not only improved in the case where keeping relatively high capacitance, and its high rate performance is also relatively good.It fills for the first time
Electric discharge is 1305/1491mAh/g=87.5%.High rate performance is good, 0.1C（0.122A/g）, capacitance is distinguished under the conditions of 1C, 12C
For：1381,1195,721mAh/g, the raw capacity that it still has 52.2% after 80 times of increase in current.By Fig. 2（C）
In it can be seen that in high magnification, cycle performance is still good.
Embodiment 2：
A method of lithium cell negative pole shell-core structure nanofiber is prepared, includes following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The precursor solution of nuclear structure, the mass concentration that the mass concentration of silicon nano is 5%, PMMA is 11%；The forerunner of nuclear structure
Liquid solution has been dispersed with stirring 7h in 55 DEG C of environment；The molten middle DMF of mixing of the DMF and acetone and the volume ratio of acetone are 1：
1。
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre, matter are formd
Measure a concentration of 12%；The precursor solution of shell structure has been dispersed with stirring 6h in 50 DEG C of environment.
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio
It is 3:Between 4, apply voltage between 11kV, receive distance between 10cm, reception device is the reception device with aluminium foil；
Composite Nano fibre is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Felt is tieed up, after pre-oxidizing 2h at 260 DEG C, be carbonized under argon gas atmosphere protection between 900 DEG C 5h.
After tested, in the present embodiment, first charge-discharge is 1197/1422mAh/g=84.2%.High rate performance is good,
0.1C（0.122A/g）, capacitance is respectively under the conditions of 1C, 12C：1281,1115,704mAh/g, when 80 times of increase in current with
Its raw capacity for still having 50.2% afterwards.
Embodiment 3：
A method of lithium cell negative pole shell-core structure nanofiber is prepared, includes following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The precursor solution of nuclear structure, the mass concentration that the mass concentration of silicon nano is 6%, PMMA is 12%；The forerunner of nuclear structure
Liquid solution has been dispersed with stirring 8h in 60 DEG C of environment；The molten middle DMF of mixing of the DMF and acetone and the volume ratio of acetone are 1：
1。
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre, matter are formd
Measure a concentration of 11%；The precursor solution of shell structure has been dispersed with stirring 7.5h in 65 DEG C of environment.
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio
It is 5:Between 8, apply voltage between 12kV, receive distance between 11cm, reception device is the reception device with aluminium foil；
Composite Nano fibre is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Felt is tieed up, after pre-oxidizing 1.5h at 265 DEG C, be carbonized under argon gas atmosphere protection between 1000 DEG C 4h.
First charge-discharge is 1197/1451mAh/g=82.5%.High rate performance is good, 0.1C（0.122A/g）, 1C, 12C item
Capacitance is respectively under part：1307,1141,709mAh/g, after 80 times of increase in current its still have 50.7% it is original
Capacity.
Embodiment 4：
A method of lithium cell negative pole shell-core structure nanofiber is prepared, includes following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The precursor solution of nuclear structure, the mass concentration that the mass concentration of silicon nano is 4.5%, PMMA is 10%；Before nuclear structure
It drives liquid solution and has been dispersed with stirring 7.5h in 68 DEG C of environment；The volume ratio of the mixing molten middle DMF and acetone of the DMF and acetone
It is 1：1.
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre, matter are formd
Measure a concentration of 8%；The precursor solution of shell structure has been dispersed with stirring 6.5h in 80 DEG C of environment.
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio
It is 1:Between 2, apply voltage between 13kV, receive distance between 12cm, reception device is the reception device with aluminium foil；
Composite Nano fibre is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Felt is tieed up, after pre-oxidizing 1.6h at 275 DEG C, be carbonized under argon gas atmosphere protection between 850 DEG C 6h.
First charge-discharge is 1186/1394mAh/g=85.1%.High rate performance is good, 0.1C（0.122A/g）, 1C, 12C item
Capacitance is respectively under part：1325,1132,717mAh/g, after 80 times of increase in current its still have 51.1% it is original
Capacity.
Embodiment 5：
A method of lithium cell negative pole shell-core structure nanofiber is prepared, includes following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The precursor solution of nuclear structure, the mass concentration that the mass concentration of silicon nano is 5.5%, PMMA is 11%；Before nuclear structure
It drives liquid solution and has been dispersed with stirring 6.5h in 70 DEG C of environment；The volume ratio of the mixing molten middle DMF and acetone of the DMF and acetone
It is 1：1.
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre, matter are formd
Measure a concentration of 10%；The precursor solution of shell structure has been dispersed with stirring 8h in 68 DEG C of environment.
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio
It is 3:Between 4, apply voltage between 14kV, receive distance between 13cm, reception device is the reception device with aluminium foil；
Composite Nano fibre is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Felt is tieed up, after pre-oxidizing 1.8h at 280 DEG C, be carbonized under argon gas atmosphere protection between 950 DEG C 3.5h.
First charge-discharge is 1169/1388mAh/g=84.2%.High rate performance is good, 0.1C（0.122A/g）, 1C, 12C item
Capacitance is respectively under part：1321,1121,705mAh/g, after 80 times of increase in current its still have 50.8% it is original
Capacity.
Embodiment 6：
A method of lithium cell negative pole shell-core structure nanofiber is prepared, includes following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The precursor solution of nuclear structure, the mass concentration that the mass concentration of silicon nano is 5%, PMMA is 8%；The presoma of nuclear structure
Solution has been dispersed with stirring 6.8h in 80 DEG C of environment；The molten middle DMF of mixing of the DMF and acetone and the volume ratio of acetone are 1：
1。
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre, matter are formd
Measure a concentration of 8.5%；The precursor solution of shell structure has been dispersed with stirring 6.2h in 58 DEG C of environment.
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio
It is 5:Between 8, apply voltage between 15kV, receive distance between 14cm, reception device is the reception device with aluminium foil；
Composite Nano fibre is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Felt is tieed up, after pre-oxidizing 1.3h at 268 DEG C, be carbonized under argon gas atmosphere protection between 980 DEG C 4.5h.
First charge-discharge is 1207/1445mAh/g=83.5%.High rate performance is good, 0.1C（0.122A/g）, 1C, 12C item
Capacitance is respectively under part：1315,1124,704mAh/g, after 80 times of increase in current its still have 50.6% it is original
Capacity.
The design focal point of the present invention is：By first configure nuclear structure precursor solution and shell structure presoma it is molten
Liquid, then by coaxial electrostatic spinning technology it is simple and practicable prepare with good chemical property and can apply to lithium
The Si-C composite material of ion battery cathode material meets the needs used.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore it is every according to the technical essence of the invention to any subtle modifications, equivalent variations and modifications made by above example, still
Belong in the range of technical solution of the present invention.
Claims (2)
1. a kind of method preparing lithium cell negative pole shell-core structure nanofiber, it is characterised in that：Include following steps：
（1）Silicon nano and PMMA are dissolved in DMF and acetone mixing it is molten in form finally obtained composite fibre
The mass concentration of the precursor solution of nuclear structure, silicon nano is 4%-6%, and the mass concentration of PMMA is 8%-12%；Nuclear structure
Precursor solution 6-8h has been dispersed with stirring in 50-80 DEG C of environment；
（2）PAN is dissolved in DMF, the precursor solution of the shell structure in finally obtained composite fibre is formd, quality is dense
Degree is 8%-12%；The precursor solution of shell structure has been dispersed with stirring 6-8h in 50-80 DEG C of environment；
（3）Coaxial electrostatic spinning parameter is as follows：Coaxial syringe needle ectonexine thickness proportion is 1:1, ectonexine liquid outlet quantity ratio is 1:
2-3:Between 4, apply voltage between 10-15kV, receive distance between 9-14cm, reception device is the reception with aluminium foil
Device；Compound receive is prepared according to above-mentioned parameter using the precursor solution of above-mentioned nuclear structure and the precursor solution of shell structure
Rice fibrofelt, after pre-oxidizing 1-2h at 260-280 DEG C, be carbonized under argon gas atmosphere protection between 800-1000 DEG C 3-6h.
2. a kind of method preparing lithium cell negative pole shell-core structure nanofiber according to claim 1, feature exist
In：The molten middle DMF of mixing of the DMF and acetone and the volume ratio of acetone are 1：1.
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| CN110112405A (en) * | 2019-05-29 | 2019-08-09 | 哈尔滨理工大学 | A kind of core-shell structure silicon/carbon fiber flexible combination electrode material and the preparation method and application thereof |
| WO2020125442A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Aluminum carbon composite material and preparation method therefor, negative electrode, secondary battery, and electrical appliance |
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| CN111477838B (en) * | 2020-04-08 | 2021-05-18 | 北京科技大学 | Integrated stretchable lithium ion battery and preparation method thereof |
| WO2022000589A1 (en) * | 2020-06-29 | 2022-01-06 | 瑞声声学科技(深圳)有限公司 | Method for preparing silicon-based composite negative electrode material |
| CN112242513A (en) * | 2020-10-19 | 2021-01-19 | 天津工业大学 | Tube-wire structure silicon-carbon negative electrode material and preparation method thereof |
| CN113422009A (en) * | 2021-06-01 | 2021-09-21 | 广东工业大学 | Lithium ion battery cathode material and preparation method and application thereof |
| CN113422009B (en) * | 2021-06-01 | 2022-03-18 | 广东工业大学 | Lithium ion battery cathode material and preparation method and application thereof |
| CN114843461A (en) * | 2022-04-18 | 2022-08-02 | 晖阳(贵州)新能源材料有限公司 | Preparation method of low-expansion silicon-based composite material |
| CN116516522A (en) * | 2023-04-03 | 2023-08-01 | 苏州大学 | Lithium ion self-supporting silicon-carbon composite nanofiber negative electrode material and preparation method and application thereof |
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