CN108807888A - A kind of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode and preparation method thereof - Google Patents
A kind of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of three-dimensional porous copper silicon-carbon composite integrated polarizing electrodes and preparation method thereof, the simple ball grinding method of copper silicon forms cupro silicon, presoma is prepared in conjunction with the phase separation method of organic film, the three-dimensional porous copper silicon fiml with certain toughness and mechanical strength is prepared by the solid sintering technology of powder metallurgy, graphene and carbon nanotube are grown using chemical vapour deposition technique, by controlling temperature, gas is passed through the flow of time and acetylene to control the growth of graphene and carbon nanotube, and copper silicon-carbon composite integrated polarizing electrode is finally made.Three-dimensional porous structure can provide sufficient space for the volume expansion of silicon in cyclic process, and graphene and carbon nanotube have larger specific surface area, stable SEI films can be formed, it can prevent the dusting of electrode material and be crushed, finally so that it keeps stable electrochemistry cycle, there is extensive practical application meaning.
Description
Technical field
The invention belongs to the research and development of three-dimensional porous electrode material and applied technical field more particularly to a kind of three-dimensional porous copper
Silicon-carbon composite integrated polarizing electrode further relates to a kind of method preparing above-mentioned electrode.
Background technology
Current stage, since lithium ion battery has more advantage relative to other energy storage devices, such as high quality specific volume
Amount and volume and capacity ratio, therefore lithium ion battery is widely used in various portable electronic devices.For being commercialized with current
The graphite of lithium ion battery is traditional negative material, there was only about 10% volume expansion in charge and discharge process, but it is theoretical
Specific capacity is relatively low, only 372mAh g-1, since people gradually increase the demand of energy storage technology, urgent need will be ground
Send out the electrode material with height ratio capacity.
There is many novel anode material compared with high-energy source memory capacity to have caused researchers' greatly research interest,
Such as silicon (3579mAh g-1), tin (944mAh g-1) etc..Relative to other novel anode materials, silicon show larger advantage by
Have many advantages, such as that high theoretical specific capacity, low voltage platform, nontoxic, inexpensive and content are high in it.However, charging-putting
Big volume expansion (328%) can occur for silicon in electric process, cause the broken and dusting of active material and breaking for electrode structure
It is bad, the fast decay of capacity is eventually led to, therefore serious volume expansion limits its practical application.Current stage, researchers
A series of scheme for proposing solution silicon volume expansions and electrode dusting, as the Nanjing sources Xi Li development in science and technology Co., Ltd is (open
Number it is：201610883943) by the progress surface modification of silicium cathode material, binder being made to be attached to the surface of silicon particle, from
And the integrality of electrode in cyclic process is maintained, improve the electrochemical cycle stability of silicium cathode material.The auspicious power of Suzhou lattice
Power Technology Co., Ltd.'s (Publication No.：201611174374.0) mixed using polyvinylidene fluoride, polytetrafluoroethylene (PTFE) and propylene
The organic solvent type binder for closing object composition replaces traditional Kynoar, and conductive using nano-tube chondritic work
Agent, graphite and silica are as negative material, to help to improve the overall conductivity and cycle charge discharge electrical property of battery,
And the volume expansion of silicon materials is inhibited to a certain extent.
To overcome the above problem of the existing technology, we have proposed a kind of three-dimensional porous copper silicon-carbon composite integrated electricity
Pole with and preparation method thereof.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode.
To achieve the above object, the present invention provides the following technical solutions：A kind of three-dimensional porous copper silicon-carbon composite integrated electricity
The preparation method of pole, includes the following steps：(1) preparation of cupro silicon：By after drying copper powder and silica flour according to volume ratio 2:
It is poured into ball grinder after 1-15: 1 measurement, is then that 10: the 1 ball milling pearls weighed after drying pour into ball grinder according to ratio of grinding media to material,
It pours into alcohol and did not had ball milling pearl, then obtain cupro silicon after ball milling 20-80h on ball mill；(2) before three-dimensional porous copper silicon fiml
Drive the preparation of body：Cupro silicon powder prepared by step (1) is dried, the cupro silicon powder after drying and bonding agent poly- third
Alkene nitrile, which pours into mortar, to be ground uniformly, and Solvents N-methyl -2-Pyrrolidone is then added and continues grinding until being formed uniform and viscous
The casting solution of the suitable knifing of degree；The casting solution of preparation is poured on dry glass plate, after scraping plate membrane with knifing stick, is placed
It allows it to carry out solvent-point exchange of solvent in ready deionized water and obtains three-dimensional porous copper silicon fiml presoma；(3) three-dimensional more
The solid-phase sintering of hole copper silicon fiml：A, Porous Cu silicon fiml presoma sky is burnt, and in air, is heated up using the heating rate of 2 DEG C/min
1-5h is kept the temperature to 500 DEG C and in maximum temperature, binder polyacrylonitrile is removed by pyrolytic in the process, obtains being aoxidized
Porous Cu silicon fiml；B, the Porous Cu silicon fiml aoxidized is restored, in a hydrogen atmosphere, with the heating rate of 10 DEG C/min
It is warming up to 800 DEG C and keeps the temperature 1-5h in maximum temperature, obtain three-dimensional porous copper silicon fiml；4) three-dimensional porous copper silicon-carbon composite integrated
The preparation of electrode：Three-dimensional porous copper silicon fiml prepared by step (3) is placed in crucible, with 10 under 200sccm argon atmospheres
DEG C/heating rate of min rises to 600 DEG C, and keeps the temperature 10-50min in maximum temperature, it is passed through 6sccm acetylene and 100sccm hydrogen
Gas closes acetylene and hydrogen after 3-20min, carries out the growth of graphene and carbon nanotube to it using rapid temperature rise and drop stove, obtain
To three-dimensional porous copper silicon-carbon composite integrated polarizing electrode.
Preferably, the drying mode of copper powder and silica flour is that copper powder and silica flour, which are respectively placed in vacuum, to be done in the step (1)
In dry case, in 50-70 DEG C of dry 5-24h to remove the trace water contained by it.
Preferably, the drying mode of cupro silicon powder is that cupro silicon powder is placed in vacuum drying chamber in the step (2)
Middle 50-70 DEG C dry 5-24h is to remove the trace water contained by it.
Preferably, in the step (2), cupro silicon powder, bonding agent polyacrylonitrile, Solvents N-methyl -2-Pyrrolidone
Weight ratio be 1: 0.01-0.1: 01-0.5.
Preferably, the thickness of knifing stick is 250 μm in the step (2).
It is a further object of the present invention to provide a kind of three-dimensional porous copper silicon-carbon composite integrateds prepared according to the above method
Electrode.
Compared with prior art, the beneficial effects of the invention are as follows：1, the thickness of prepared copper silicon fiml can pass through knifing stick
Control, so as to control the content of active material silicon on unit area, meanwhile, three-dimensional porous structure can be the volume of silicon
Expansion provides cushion space；2, have higher intensity big and preferable tough by the copper silicon fiml prepared by high temperature solid-phase sintering
Property, the requirement of electrode can be met；It 3, can be on it in conjunction with the autocatalytic cleavage of three-dimensional continuous poriferous structure using acetylene as carbon source
Growth graphene and carbon nanotube, carbon nanotube have larger specific surface area, can form stable SEI films, can prevent electricity
The dusting of pole material and broken, improves the stability during charge and discharge cycles, and do not add any catalyst, therefore will not draw
Enter impurity.
Description of the drawings
Fig. 1 is the surface scan electron microscope of the three-dimensional porous copper silicon fiml prepared according to 1 step of the embodiment of the present invention (3)；
Fig. 2 is the surface scan electron microscope of the copper silicon-carbon integrated electrode prepared according to the embodiment of the present invention 1；
Fig. 3 is the surface scan electron microscope of the copper silicon-carbon integrated electrode prepared according to the embodiment of the present invention 2；
Fig. 4 is the surface scan electron microscope of the copper silicon-carbon integrated electrode prepared according to the embodiment of the present invention 3.
Specific implementation mode
The preferred embodiment of the present invention is described below in conjunction with attached drawing, to the technical solution in the preferred embodiment of the present invention into
Row clearly and completely describes.
Embodiment 1：
The preparation method for the copper silicon-carbon integrated electrode that this example specifically provides, includes the following steps：
1) preparation of cupro silicon：Dry copper powder, silica flour, 60 DEG C of dry 12h in vacuum drying chamber in advance.Copper silicon is pressed
It is that 3: 1 to weigh the siliceous amount of copper be respectively to pour into ball grinder after 23g, 2g according to volume ratio, is then to weigh at 10: 1 according to material ratio
250g ball milling pearls equally pour into ball grinder, and pouring into suitable alcohol makes it flood ball milling pearl, then the ball milling 50h on ball mill
After can be obtained cupro silicon.
2) preparation of three-dimensional porous copper silicon fiml presoma：Cupro silicon prepared by step 1) is placed in vacuum drying chamber
After 60 DEG C of dry 12h, weighs 1g cupro silicons powder and is uniformly mixed in mortar with the binder polyacrylonitrile (PAN) of 49.18mg,
Solvents N-methyl -2-Pyrrolidone (NMP) that 0.5g is added later continues grinding until forming uniform and viscosity suitable for knifing
Casting solution.Prepared casting solution is poured in right amount on glass plate dry in advance, the knifing stick for being 250 μm with thickness scrapes flat
Plate film is subsequently placed in ready deionized water and its progress solvent-nonsolvent is allowed to exchange to obtain Porous Cu silicon fiml presoma.
3) solid-phase sintering of three-dimensional porous copper silicon fiml：Using suitable sintering parameter to above-mentioned steps 2) prepared by it is porous
Copper silicon fiml presoma carries out solid-phase sintering.Sintering process is carried out in two steps, and is the empty burning process of Porous Cu silicon fiml presoma first,
In air, 500 DEG C are warming up to the heating rate of 2 DEG C/min, and cooled down with stove after maximum temperature keeps the temperature 2h, herein mistake
Cheng Zhong, binder PAN are removed by pyrolytic, obtain pure zirconia copper silicon fiml；Followed by the Porous Cu silicon fiml to being aoxidized also
Former process is warming up to 800 DEG C and after maximum temperature keeps the temperature 1h with stove with the heating rate of 10 DEG C/min in a hydrogen atmosphere
Cooling.Porous Cu silicon fiml after reduction has certain mechanical strength and flexibility and is three-dimensional porous structure.Such as Fig. 3 institutes
It is shown as the surface scan electron microscope of three-dimensional porous copper silicon fiml manufactured in the present embodiment.
4) preparation of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode：By above-mentioned steps 3) prepared by three-dimensional porous copper silicon
Film is placed in crucible, after rising to 600 DEG C using 10 DEG C/min heating rates under argon atmosphere, and is kept the temperature in maximum temperature
30min is passed through 6sccm acetylene and 100sccm hydrogen, removes burner hearth after 5min, it is more to obtain three-dimensional when temperature reaches 600 DEG C
Hole copper silicon-carbon composite integrated polarizing electrode.The use of prepared copper silicon/carbon composite integrated polarizing electrode is later that negative material assembles electricity
Pond carries out electrochemical property test.
It is illustrated in figure 2 the scanning electron microscope (SEM) photograph of copper silicon-carbon integrated electrode manufactured in the present embodiment, by controlling acetylene
Throughput and soaking time can control the growth of carbon nanotube, it can be seen from the figure that having a small amount of carbon nanotube on its surface
It generates, but the length of carbon nanotube generated is shorter.
Embodiment 2：
Difference from example 1 is that above-mentioned steps 4) in, prepared three-dimensional porous copper silicon fiml is placed in crucible
In, after rising to 600 DEG C using 10 DEG C/min heating rates under argon atmosphere, and 30min is kept the temperature in maximum temperature, when temperature reaches
When to 600 DEG C, it is passed through 6sccm acetylene and 100sccm hydrogen, burner hearth is removed after 10min, obtains three-dimensional porous copper silicon-carbon compound one
Body polarizing electrode.Compared with Example 1, the throughput for controlling acetylene is constant while increasing soaking time when being passed through gas to control
The growth of carbon nanotube processed, the scanning electron microscope (SEM) photograph of copper silicon-carbon integrated electrode as shown in Figure 3, it can be seen from the figure that at it
Surface has more carbon nanotube to generate, and length is relatively uniform, and is grown in pencil.
Embodiment 3：
Difference from example 1 is that above-mentioned steps 4) in, prepared three-dimensional porous copper silicon fiml is placed in crucible
In, after rising to 600 DEG C using 10 DEG C/min heating rates under argon atmosphere, and 30min is kept the temperature in maximum temperature, when temperature reaches
When to 600 DEG C, it is passed through 6sccm acetylene and 100sccm hydrogen, burner hearth is removed after 15min, obtains three-dimensional porous copper silicon-carbon compound one
Body polarizing electrode.Compared to embodiment 1,2, continues to keep the throughput of acetylene constant, when continuing growing heat preservation when being passed through gas
Between control the growth of carbon nanotube, the scanning electron microscope (SEM) photograph of copper silicon-carbon integrated electrode as shown in Figure 4 can from figure
Go out, there are a large amount of carbon nanotubes to generate on its surface, and the carbon nanotube generated wraps up copper silicon in three-dimensional continuous cage structure
Film.
Embodiment 4：
Difference from example 1 is that above-mentioned steps 1) in, according to volume ratio it is that 15: 1 to weigh copper siliceous by copper silicon
It is poured into ball grinder after amount respectively 30g, 0.5g, then weighing 305g ball milling pearls according to material ratio for 10: 1 equally pours into ball milling
In tank, pouring into suitable alcohol makes it flood ball milling pearl, then can be obtained cupro silicon after ball milling 50h on ball mill.
The present invention using it is a kind of it is simple and practicable by the way of prepare three-dimensional porous copper silicon integrated electrode, and using acetylene as carbon
Source can grow graphene and carbon nanotube on it in conjunction with the autocatalytic cleavage of three-dimensional continuous poriferous structure.The simple ball milling of copper silicon
Method forms cupro silicon, prepares presoma in conjunction with phase separation (NIPS) method of organic film, passes through powder metallurgy
Solid sintering technology prepares the three-dimensional porous copper silicon fiml with certain toughness and mechanical strength, utilizes chemical vapor deposition (CVD)
Method grows graphene and carbon nanotube, and by controlling temperature, gas is passed through the flow of time and acetylene to control graphene and carbon
Copper silicon/carbon composite integrated polarizing electrode is finally made in the growth of nanotube.Three-dimensional porous structure can be the body of silicon in cyclic process
Product expansion provides sufficient space, and graphene and carbon nanotube have larger specific surface area, can form stable SEI films,
The dusting of electrode material and broken can be prevented, finally so that it keeps stable electrochemistry cycle, has and widely actually answers
Use meaning.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of preparation method of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode, it is characterised in that：Include the following steps,
(1) preparation of cupro silicon：By after drying copper powder and silica flour according to volume ratio 2: 1-15: 1 measure after pour into ball grinder
In, it is then that 10: the 1 ball milling pearls weighed after drying pour into ball grinder according to ratio of grinding media to material, pours into alcohol and do not had ball milling pearl, then
On ball mill cupro silicon is obtained after ball milling 20-80h；
(2) preparation of three-dimensional porous copper silicon fiml presoma：Cupro silicon powder prepared by step (1) is dried, after dry
Cupro silicon powder and bonding agent polyacrylonitrile pour into mortar and grind uniform, Solvents N-methyl -2-Pyrrolidone is then added
Continue grinding until forming uniform and viscosity suitable for the casting solution of knifing；The casting solution of preparation is poured on dry glass plate,
After scraping plate membrane with knifing stick, it is positioned in ready deionized water and its progress solvent-point exchange of solvent is allowed to obtain three-dimensional
Porous Cu silicon fiml presoma；
(3) solid-phase sintering of three-dimensional porous copper silicon fiml：A, Porous Cu silicon fiml presoma sky is burnt, in air, using 2 DEG C/min's
Heating rate is warming up to 500 DEG C and keeps the temperature 1-5h in maximum temperature, and binder polyacrylonitrile is gone by pyrolytic in the process
It removes, obtains the Porous Cu silicon fiml aoxidized；B, the Porous Cu silicon fiml aoxidized is restored, in a hydrogen atmosphere, with 10 DEG C/
The heating rate of min is warming up to 800 DEG C and keeps the temperature 1-5h in maximum temperature, obtains three-dimensional porous copper silicon fiml；
4) preparation of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode：Three-dimensional porous copper silicon fiml prepared by step (3) is placed in
In crucible, 600 DEG C are risen to the heating rate of 10 DEG C/min under 200sccm argon atmospheres, and 10- is kept the temperature in maximum temperature
50min is passed through 6sccm acetylene and 100sccm hydrogen, acetylene and hydrogen is closed after 3-20min, using rapid temperature rise and drop stove to it
The growth for carrying out graphene and carbon nanotube, obtains three-dimensional porous copper silicon-carbon composite integrated polarizing electrode.
2. the preparation method of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode according to claim 1, it is characterised in that：Institute
It is copper powder and silica flour to be respectively placed in vacuum drying chamber, at 50-70 DEG C to state the drying mode of copper powder and silica flour in step (1)
Dry 5-24h is to remove the trace water contained by it.
3. the preparation method of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode according to claim 1, it is characterised in that：Institute
The drying mode for stating cupro silicon powder in step (2) is that cupro silicon powder is placed in 50-70 DEG C of dry 5- in vacuum drying chamber
For 24 hours to remove the trace water contained by it.
4. the preparation method of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode according to claim 1, it is characterised in that：Institute
State in step (2), cupro silicon powder, bonding agent polyacrylonitrile, Solvents N-methyl -2-Pyrrolidone weight ratio be 1: 0.01-
0.1∶01-0.5。
5. the preparation method of three-dimensional porous copper silicon-carbon composite integrated polarizing electrode according to claim 1, it is characterised in that：Institute
The thickness for stating knifing stick in step (2) is 250 μm.
6. according to three-dimensional porous copper silicon-carbon composite integrated polarizing electrode made from claim 1-5 any one of them preparation methods.
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| CN109599534A (en) * | 2018-11-29 | 2019-04-09 | 西交利物浦大学 | Nanometer flower-shaped silicon copper electrode material based on graphene and the preparation method and application thereof |
| CN109599534B (en) * | 2018-11-29 | 2021-04-27 | 西交利物浦大学 | Graphene-based nano flower-shaped silicon-copper alloy electrode material and preparation method and application thereof |
| CN109888173A (en) * | 2019-02-26 | 2019-06-14 | 天津工业大学 | The preparation method of three-dimensional continuous poriferous copper/graphite electrode |
| CN109888173B (en) * | 2019-02-26 | 2021-09-17 | 天津工业大学 | Preparation method of three-dimensional continuous porous copper/graphite electrode |
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| WO2021008244A1 (en) * | 2019-07-17 | 2021-01-21 | 肇庆市华师大光电产业研究院 | Lithium ion battery negative electrode material with high specific capacity and preparation method therefor |
| CN113564524A (en) * | 2021-07-13 | 2021-10-29 | 南京邮电大学 | Method for preparing carbon-coated three-dimensional porous copper current collector |
| CN117117154A (en) * | 2023-10-19 | 2023-11-24 | 河南鑫泉能源科技有限公司 | Lithium ion battery silicon anode material and preparation method and application thereof |
| CN117117154B (en) * | 2023-10-19 | 2024-01-30 | 河南鑫泉能源科技有限公司 | Lithium ion battery silicon anode material and preparation method and application thereof |
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