CN107394150A - A kind of mesoporous silicon copper composition electrode material and its preparation method and application - Google Patents
A kind of mesoporous silicon copper composition electrode material and its preparation method and application Download PDFInfo
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- CN107394150A CN107394150A CN201710573129.5A CN201710573129A CN107394150A CN 107394150 A CN107394150 A CN 107394150A CN 201710573129 A CN201710573129 A CN 201710573129A CN 107394150 A CN107394150 A CN 107394150A
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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
- H01M4/366—Composites as layered products
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/38—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
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of mesoporous silicon copper composition electrode material and its preparation method and application.Described mesoporous copper silicon combination electrode material has 10 100nm pore passage structure, than the 300m of surface 602/ g, the mass fraction of copper account for 15 75%.The preparation method includes：Magnesium thermit is carried out to the mixture of magnesium powder and mesoporous silicon oxide mesoporous silicon is made；Mesoporous silicon copper composition is prepared using dipping hydrogen reduction method.Present invention also offers application of the described mesoporous silicon copper electrode material in negative electrode of lithium ion battery is prepared.The mesoporous copper silicon combination electrode material of the present invention, have the advantages that reversible capacity height, good cycling stability, good rate capability are high, be produced on a large scale.
Description
Technical field
The present invention relates to a kind of high power capacity, long-life, mesoporous silicon-copper composition electrode material of low cost and its preparation side
Method, belong to the technical field of battery material manufacture.
Background technology
The superior function of lithium ion battery makes it have in portable electric appts, electric automobile, Aero-Space etc.
Wide application prospect.
Commercial negative material still based on the carbon material of carbon element of graphite class, only have by its theoretical maximum specific capacity at present
372mAh/g, constrain the further raising of lithium battery capacity.Silicon is considered as most promising electrode material, its theoretical capacity
Up to 4200mAh/g (Li4.4Si alloys), about the 10 of carbon negative material theoretical specific capacity times are used as lithium ion battery
Negative pole the capacity of battery can be substantially improved.In addition, the lithiumation platform voltage of silicon electrode is higher than the platform voltage of graphite electrode, energy
The formation of dendrite is effectively avoided, lifts the security of lithium ion battery.But conventional research shows that silicon based electrode is in charge and discharge
In electric cyclic process, i.e., Lithium-ion embeding, abjection electrode during, can cause silicon electrode volume great variety (>
300%), cause the avalanche of silicon material structure and the peeling of electrode, efflorescence, the decline of electrical conductivity, and then cause battery capacity sharp
Subtract.
In recent years, start to receive significant attention by the method for the synthesizing porous silicon of magnesiothermic reduction mesoporous silicon oxide, use
The pore passage structure of porous silicon prepared by this method, cushion space can be provided for Volume Changes of the silicon in embedding lithium/de- lithium process,
Part internal stress is offset, there is preferable cyclical stability.But the electric conductivity of simple porous silicon is poor, high-rate discharge capacity
Difference, and repeatedly inducing capacity fading is still more serious after circulation.Thus, inert metal and silicon is compound combined modified, turn into further
Lift silicon based electrode cyclical stability, the new way of high rate performance.
The content of the invention
Technical problem：To lift the electric conductivity of silicon electrode, further delaying electrode efflorescence, the generation of cracking, present invention system
For a kind of mesoporous silicon-copper composition electrode material, using metallic copper electronic conductivity is high, ductility is good, inertia does not store up lithium etc.
Advantage, it is its reversible capacity height, good cycling stability, forthright again using dipping-hydrogen reduction method in mesoporous silicon surface modification copper particle
Energy is good, is produced on a large scale.It is a further object to provide the preparation method of the mesoporous silicon-copper composition and answer
With.
Technical scheme：A kind of mesoporous silicon-copper composition electrode material of the present invention has 10-100nm pore passage structure, than
Surface area is 60-300m2/ g, the mass fraction of copper is 15-75%.
The preparation method of mesoporous silicon-copper composition electrode material of the present invention is to utilize CuCl2Solution is carried out to mesoporous silicon
After dipping, mesoporous silicon-copper composition electrode material is prepared using the method for hydrogen reduction.
The CuCl2When solution impregnates, CuCl2Maceration extract solubility is 0.5-5mol/L；Dip time is 0.5-5h.
During the method hydrogen reduction using hydrogen reduction, the volume flow of hydrogen is 5-50sccm, the volume flow of argon gas
For 5-50sccm, hydrogen reduction temperature is more than 200 DEG C, and heating rate is 0.5-10 DEG C/min.
Mesoporous silicon-copper composition electrode material of the present invention is applied in negative electrode of lithium ion battery.
Beneficial effect：Mesoporous silicon provided by the invention-copper composition electrode material energy density is high, and reversible capacity is high, follows
Ring stability is good, high-rate discharge capacity is good.
Conventional research shows：Silicon materials have higher theoretical electrochemistry capacity, the discharge capacity first of commodity silica flour
Up to more than 3000mAh/g, but due to during embedding and removing, along with huge Volume Changes, causing material powder
Change, lost with collector after making electrical contact with so that capacity drastically declines.And the present invention utilizes mesoporous silicon alternate internal UNICOM, uniform
Pore passage structure, Volume Changes of the buffering silicon materials in process of intercalation, offsets part internal stress；Meanwhile repaiied in mesoporous silicon face
Copper particle is adornd, provides effective support for contraction of the silicon materials during de- lithium, two aspects suppress the efflorescence of silicon materials, lift silicon
The cyclical stability of base electrode.On the other hand, the electric conductivity of copper particle is preferable, and more conductive paths, and copper are provided for electronics
Particle can hinder the aggregation of silicon nanoparticle, the electric conductivity of comprehensive lifting silicon materials, and then reduce electronics transfger impedance, lifting silicon
The high-rate discharge capacity of base electrode.In the present invention circulation volume conservation rate of prepared mesoporous silicon-copper composition electrode compared with
Commodity silica flour and simple mesoporous silicon are significantly increased, and capacity declines smaller, platform effect unobvious during heavy-current discharge,
It is small that multiplying power discharging terminates rear capacitance loss rate.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of mesoporous silicon-copper composition (100g/L) prepared by dipping-hydrogen reduction method；
Fig. 2 is the high rate performance contrast of mesoporous silicon-copper composition prepared by dipping-hydrogen reduction method and simple mesoporous silicon；
Fig. 3 is the electrochemical cycle stability of mesoporous silicon-copper composition prepared by dipping-hydrogen reduction method and simple mesoporous silicon
Contrast；
Fig. 4 is the XRD of different proportion mesoporous silicon-copper composition prepared by dipping-hydrogen reduction method.
Embodiment
Mesoporous silicon of the present invention-copper composition electrode material, described mesoporous silicon-copper composition electrode material have
10-100nm pore passage structure, specific surface area 60-300m2/ g, the mass fraction of copper is 15-75%.
Present invention also offers the preparation method of described mesoporous silicon-copper composition electrode material, including：To magnesium powder with being situated between
The mixture of hole silica carries out magnesiothermic reduction reaction；Mesoporous silicon is carried out to impregnate-hydrogen reduction, it is compound that mesoporous silicon-copper is made
Thing.
The temperature of magnesium thermit is 400-700 DEG C, can be 400-600 DEG C, 600-700 DEG C etc., soaking time 0-
20h, heating rate are 0.5-10 DEG C/min.Soaking time is 0h, and reaction temperature is 400-600 DEG C of accessory substance Mg2Si contents compared with
Height, mass percent 10% or so, as temperature raises, accessory substance Mg2Si contents gradually reduce, when reaction temperature is 650 DEG C,
Mg2Si contents are 4.2% or so, when being increased to 700 DEG C, Mg2Si contents are less than 1%.Pair can be reduced by improving soaking time
Product Mg2Si contents.
The mass ratio of the magnesium powder and mesoporous silicon oxide is 0.8-1.2：1.Under the conditions of pyroreaction, the Mg of part can be with
The form loss of Mg steam, thus Mg is typically excessive during dispensing, when excess is more than 50%, Mg can form a large amount of accessory substances with Si
Mg2Si, Si yield reduce.Therefore after preferably, the mass ratio for determining the magnesium powder and mesoporous silicon oxide is 0.88-1：1.
The magnesium powder is 80-600 mesh, is further 300-350 mesh.But it is not limited to this.
Described mesoporous silicon oxide is SBA-15, but not limited to this, can also use other kinds of meso-porous titanium dioxide
Silicon.
Magnesium thermit terminate it is latter as need to be post-processed reaction product, the post processing is uses reaction product respectively
Hydrochloric acid (washes away reaction product MgO and Mg2Si) and hydrofluoric acid clean (remove react remaining mesoporous silicon oxide), cross and be filtered dry
It is dry.
The process for preparation of the maceration extract is, by ethanol:Deionized water by volume 1:1~5 prepares mother liquor, adds
CuCl2·2H2O powder, the CuCl that concentration is 50-500g/L is made into after dissolving2Solution, can be 50g/L, 100g/L etc..Dipping
Time is 0.5-5h, and dipping process preferably stirs.After dipping terminates, mesoporous silicon needs filtration drying.
The During Hydrogen Reducing is, dipping and dried powder are put into tube calciner, whole process be passed through hydrogen and
Argon gas mixed gas, its volume flow are respectively 5-50sccm and 5-50sccm.200 are warming up to 0.5-10 DEG C/min speed
More than DEG C, it can be 250 DEG C, 300 DEG C etc., soaking time 0.5-5h, then naturally cool to room temperature.
Present invention also offers described mesoporous silicon-copper composition electrode material answering in negative electrode of lithium ion battery is prepared
With.
The present invention is further explained with reference to embodiment.
The particle diameter for the magnesium powder that following examples use is 325 mesh, mesoporous silicon oxide SBA-15.
The first step, by the magnesium powder and meso-porous titanium dioxide Si powder in mass ratio 1 that granularity is 325 mesh:1 is ground, and takes
0.5g mixed-powders.Mix powder is loaded in quartz boat, is put into tube furnace, under an argon atmosphere, with 1 degree/min
Speed is warming up to 700 DEG C, is incubated 5 hours, furnace cooling.The sample in tube furnace is taken out, respectively with 1M HCl solutions and 10%
HF solution cleans, and resulting materials are mesoporous silicon material (see Fig. 2, Fig. 3), and BET test specific surface areas are 249m2/g。
Mesoporous silicon made from magnesium reduction process remains the vermiform pattern of raw material mesoporous silicon oxide substantially, has larger
Specific surface area, aperture integrated distribution is larger in 10-20nm, specific surface area.
Second step, by ethanol:The volume ratio of deionized water is 1:3 prepare mixed solution, add CuCl2·2H2O solids,
It is made into the CuCl of various concentrations2Solution (100g/L, 200g/L, 400g/L).Appropriate mesoporous silicon is poured into solution, ultrasonic vibration
30min.Vacuum drying chamber is put into after suction filtration, with 105 DEG C of dry 10h, that is, obtains CuCl2The mesoporous silicon compound of dipping.
Gained compound is put into tube calciner and carries out hydrogen reduction, is warming up to 350 DEG C with 5 DEG C/min, and be incubated one
Hour.In During Hydrogen Reducing, whole process is passed through 20sccm H2With 10sccm Ar mixed gas, cool to room temperature with the furnace, produce
To mesoporous silicon-copper composition (see Fig. 1).
Obtained mesoporous silicon-copper composition powder, conductive black super P and binding agent sodium alginate are taken out by quality
Than 3:1:1 mixing, add appropriate amount of deionized water and be tuned into uniform slurry, coating (about 5 μm of thickness) is on copper foil of affluxion body.It will apply
The copper foil for being covered with sample is put into vacuum drying chamber, is dried 10 hours in vacuum environment.Dried sample is taken out, rushes electrode
Piece, a diameter of 13mm of electrode slice.
The charge-discharge performance of sample is to test to obtain on Land (blue electricity) charging/discharging apparatus.Electro-chemical test is 2032
Carried out in type button cell system, electrolyte is 1M LiPF6It is dissolved in addition 2%VC (vinylene carbonate) EC/DEC (carbon
Vinyl acetate/diethyl carbonate, volume ratio 1:1) solution, it is metal lithium sheet to electrode.Above-mentioned button cell is connected to
In Land equipment, at room temperature, constant current charge-discharge test is carried out.Stopping potential is first discharged to 200mA/g current density
0.01V(vs.Li/Li+), after standing 2min, then stopping potential 1.0V (vs.Li/ are charged to 200mA/g current density
Li+).Obtained circulation volume (see Fig. 2).
Mesoporous silicon-copper sample (impregnation concentration 100,200,400g/L) prepared by the present invention, after 60 circulations
Specific discharge capacity is respectively 220.9mAh/g, 367.5mAh/g, 714.5mAh/g, discharge capacity attenuation rate is respectively 85.9%,
78.0%th, 51.0%；It is obviously improved compared to simple mesoporous silicon (88.7%).
The charge-discharge performance of sample is to test to obtain on Land (blue electricity) charging/discharging apparatus.Electro-chemical test is 2032
Carried out in type button cell system, electrolyte is 1M LiPF6It is dissolved in addition 2%VC (vinylene carbonate) EC/DEC (carbon
Vinyl acetate/diethyl carbonate, volume ratio 1:1) solution, it is metal lithium sheet to electrode.Above-mentioned button cell is connected to
In Land equipment, at room temperature, rate charge-discharge test is carried out.Detailed process is first to be discharged to 200mA/g current density
Stopping potential 0.01V (vs.Li/Li+), after standing 2min, then stopping potential 1.0V charged to 200mA/g current density
(vs.Li/Li+), circulate ten times.Afterwards current density be changed into 500 according to this, 1000,2000,4000mA/g, finally return
200mA/g, every grade of current density circulate ten times.Obtain high rate performance (see Fig. 3).
When current density is more than 500mA/g, the specific discharge capacity of mesoporous silicon-copper sample is higher than simple mesoporous silicon；Wherein,
When current density is more than 500mA/g and is less than 2000mA/g, the better performances of 100g/L samples；And when current density rises to
During more than 2000mA/g, the specific capacity of 400g/L samples becomes highest.After terminating rate charge-discharge, simple mesoporous silicon is bad rapidly
Change, and inducing capacity fading is serious；And the stability of mesoporous silicon-copper sample is obviously improved.
The electrochemical impedance spectroscopy of sample is tested by the CHI604E type Electrochemical Comprehensive Testers of Shanghai Chen Hua instrument company
Arrive, test frequency is from 100kHz to 1Hz；Cyclic voltammetry curve (CV) is tested, and take-off potential 1.5V, termination current potential is 0.01V,
Sweep speed is 0.5mV/S.
For the charge-transfer resistance of quantitative comparison different materials, impedance curve is fitted using equivalent circuit method, obtained
The electron transmission impedance R arrivedctIt is listed in table 1.With CuCl2The raising of impregnation concentration, the electron transmission impedance of resulting sample
Reduce, illustrate that the copper particle for being attached to porous silicon surface provides for electronics from collector (copper sheet) to porous silicon surface and more ooze
Logical circulation road.The reduction of electron transmission impedance, be advantageous to the lifting of material high-rate discharge capacity.
The electron transmission impedance of the different mesoporous silicon-copper compositions of table 1
To various concentrations CuCl2Maceration extract prepares mesoporous silicon-copper sample and carries out XRD (X-ray diffraction) tests, test result
See Fig. 4.
Claims (5)
- A kind of 1. mesoporous silicon-copper composition electrode material, it is characterised in that described mesoporous silicon-copper composition electrode material tool There are 10-100nm pore passage structure, specific surface area 60-300m2/ g, the mass fraction of copper is 15-75%.
- A kind of 2. preparation method of mesoporous silicon-copper composition electrode material as claimed in claim 1, it is characterised in that：The party Method utilizes CuCl2After solution impregnates to mesoporous silicon, mesoporous silicon-copper composition electrode material is prepared using the method for hydrogen reduction Material.
- 3. the preparation method of mesoporous silicon according to claim 2-copper composition electrode material, it is characterised in that described CuCl2When solution impregnates, CuCl2Maceration extract solubility is 0.5-5mol/L；Dip time is 0.5-5h.
- 4. the preparation method of mesoporous silicon according to claim 2-copper composition electrode material, it is characterised in that described to adopt During with the method hydrogen reduction of hydrogen reduction, the volume flow of hydrogen is 5-50sccm, and the volume flow of argon gas is 5-50sccm, and hydrogen is also Former temperature is more than 200 DEG C, and heating rate is 0.5-10 DEG C/min.
- A kind of 5. application of mesoporous silicon-copper composition electrode material as claimed in claim 1, it is characterised in that the electrode material Material is applied in negative electrode of lithium ion battery.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108232149A (en) * | 2017-12-29 | 2018-06-29 | 华东理工大学 | Copper-silicon composite cathode material, preparation method and the lithium battery containing it |
| CN108335800A (en) * | 2017-12-29 | 2018-07-27 | 天津工业大学 | Copper silicon integrated electrode and preparation method thereof |
| CN109103443A (en) * | 2018-08-08 | 2018-12-28 | 欣旺达电子股份有限公司 | Silicon based anode material and preparation method thereof |
| CN109585834A (en) * | 2018-12-10 | 2019-04-05 | 包头市石墨烯材料研究院有限责任公司 | A kind of mesoporous silicon-tin composite electrode material and its preparation method and application |
| JP2020102337A (en) * | 2018-12-21 | 2020-07-02 | 三洋電機株式会社 | Manufacturing method of mixture layer material, manufacturing method of secondary battery, and secondary battery |
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| CN108232149A (en) * | 2017-12-29 | 2018-06-29 | 华东理工大学 | Copper-silicon composite cathode material, preparation method and the lithium battery containing it |
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