CN106898726A - A kind of noncrystalline membrane nano-silicon electrode material is prepared and applied in lithium ion battery - Google Patents
A kind of noncrystalline membrane nano-silicon electrode material is prepared and applied in lithium ion battery Download PDFInfo
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- CN106898726A CN106898726A CN201710167676.3A CN201710167676A CN106898726A CN 106898726 A CN106898726 A CN 106898726A CN 201710167676 A CN201710167676 A CN 201710167676A CN 106898726 A CN106898726 A CN 106898726A
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0438—Processes of manufacture in general by electrochemical processing
- H01M4/045—Electrochemical coating; Electrochemical impregnation
- H01M4/0452—Electrochemical coating; Electrochemical impregnation from solutions
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
A kind of noncrystalline membrane nano-silicon electrode material is prepared and applied in lithium ion battery, belongs to lithium battery material preparing technical field.Conductive agent is dried first, to remove moisture therein, is dissolved in organic solvent after drying, silicon compound is subsequently adding, using three-electrode system, constant potential electro-deposition is carried out at normal temperatures, copper surface is cleaned after electro-deposition with organic solvent, unformed film nano silicon is obtained.The electrode material that the active material obtained with the method is prepared is assembled into lithium ion battery, can reach the capacity of more than 1000mAh/g, and with good cyclical stability and high rate performance, processing step is simple to operation, has a good application prospect.
Description
Technical field：
The invention provides a kind of noncrystalline membrane nano-silicon electrode material technology of preparing, belong to lithium battery material and prepare skill
Art field.
Background technology：
Silicon why can as one of high power capacity of new generation, the candidate material of high power lithium ion cell because its
With the up to theoretical specific capacity of 4200mAh/g and relatively low charge and discharge potential.However, embedding lithium alloyage and de- lithium alloyage mistake
Along with huge volumetric expansion (300%) in journey, it will cause silicon electrode material breaks, efflorescence, ultimately result in battery capacity
Fall sharply.
Further to improve the cyclical stability of silicium cathode material, scientific circles have proposed various nanostructured silicon electrodes,
Such as thin-film material, nanowires/nanotubes, nanoparticle and mesoporous material.There is high energy consumption, security in these preparation methods
The problems such as difference, purity are difficult to control to, especially cyclical stability is poor for the chemical property of most importantly prepared material.
Amorphous substance has very due to the unformed state of structure for suppressing the volumetric expansion after silicon lithium alloyage
Obvious effect, the volumetric expansion of amorphous silicon is relatively small, and film and nano particle further alleviate product in expansion process
Tired stress, the combination of three effectively inhibits the volumetric expansion of silicon.
Important innovations of the invention are to obtain unformed film nano silicon electrode by electro-deposition in organic solvent, without
Addition bonding agent and conductive agent, directly as the negative material of lithium ion battery.
The content of the invention：
Unformed film nano silicon is obtained it is an object of the invention to provide a kind of Direct Electrolysis silicon compound at normal temperatures
Used as the method for lithium ion battery negative material, its Core-technology is to prepare lithium ion battery by the method for electro-deposition
Negative material.The method has electrolysis temperature low, and without high pressure, process is simple is easy to operate, advantages of environment protection.
The technical scheme is that：
Conductive agent is dried (such as dry 24h under 80 DEG C of vacuum environments) first, to remove moisture therein, is dried
After be dissolved in organic solvent, be subsequently adding silicon compound, using three-electrode system, constant potential electro-deposition is carried out at normal temperatures,
Copper surface is cleaned after electro-deposition with organic solvent, unformed film nano silicon is obtained.Be then transferred into glove box, as lithium from
The negative material of sub- battery is assembled into button cell.
The method that the present invention prepares unformed film nano silicon, the described silicon compound for being dissolved in organic solvent is selected from
SiCl4、SiBr4、SiI4、SiHCl3, its concentration in organic solvent is 0.3M~1M.
The method that the present invention prepares unformed film nano silicon, the described conductive agent for being dissolved in organic solvent is selected from tetramethyl
Ammonium chloride (TMAC), etamon chloride (TEAC), 4-propyl ammonium chloride (TPAC), tetrabutylammonium chloride (TBACl), it is having
Concentration in machine solvent is 0.1M~0.5M.
The method that the present invention prepares unformed film nano silicon, described organic solvent is selected from ethylene carbonate (EC), carbon
Acid propylene ester (PC), tetrahydrofuran (THF), acetonitrile (CH3CN)。
The method that the present invention prepares unformed film nano silicon, in methods described during constant potential electro-deposition, with Pt as reference
Electrode, voltage is -1.6V~-2.7V.
The method that the present invention prepares unformed film nano silicon, electrodeposition time is 1h-10h.The present invention prepares unformed
The method of film nano silicon, cleans the surface of three electrodes with watery hydrochloric acid before deposition, being put into afterwards in acetone carries out ultrasound, electro-deposition
Afterwards with being cleaned with organic solution solution first, then the impurity for removing remained on surface is cleaned with acetone soln.
The unformed film nano silicon of electro-deposition as lithium ion battery negative material application.
Electrode material prepared by methods described has the relatively stable, high rate performance of circulation as lithium ion secondary battery negative pole
Good the features such as, can be applied to portable electric appts.
Advantages of the present invention：
1) film nano silicon crystal grain is tiny, uniform particle sizes, about 50nm or so；
2) lithium storage content is big
In 0.01v-1.5v charge and discharge process, its charging and discharging capacity may remain in electrode material of the present invention
1000mAh/g or so.
3) good cycling stability
Electrode material of the present invention circulates 200 times without obvious capacity under the charge-discharge mechanism of 0.01-1.5V
Decay, discharge voltage plateau embodies good cyclical stability without being decreased obviously.
4) low energy consumption is prepared
Electrode material of the present invention has low temperature preparation feature as lithium ion battery negative, and energy consumption cost is low, tool
There is good market competition advantage.
Brief description of the drawings
Fig. 1 is the linear scan figure of unformed film nano silicon electrode electrolyte prepared by the present invention；
Fig. 2 is unformed film nano silicon electrode figure prepared by the present invention；
Fig. 3 is the energy spectrum diagram of unformed film nano silicon electrode prepared by the present invention；
Fig. 4 is the XRD of unformed film nano silicon electrode prepared by the present invention；
Fig. 5 is the charging and discharging curve figure (embodiment 2) of unformed film nano silicon electrode prepared by the present invention；
Fig. 6 is the capacity attenuation figure (embodiment 2) of unformed film nano silicon electrode prepared by the present invention；
Fig. 7 is the high rate performance figure (embodiment 2) of unformed film nano silicon electrode prepared by the present invention；
Fig. 8 is the impedance spectra (embodiment 2) of unformed film nano silicon electrode prepared by the present invention；
Fig. 9 is the capacity attenuation figure (embodiment 4) of unformed film nano silicon electrode prepared by the present invention；
Figure 10 is the capacity attenuation figure (embodiment 5) of unformed film nano silicon electrode prepared by the present invention；
Figure 11 is unformed film nano silicon electrode figure (embodiment 6) prepared by the present invention；
Figure 12 is the capacity attenuation figure (embodiment 6) of unformed film nano silicon electrode prepared by the present invention.
Specific embodiment
The present invention is further illustrated below by specific embodiment, it should be understood, however, that these embodiments are only
It is used for specifically describing in more detail, and is not to be construed to the present invention.
Following examples to experimental technique used in present invention experiment to carrying out general description.Although to realize this
The many materials and operating method that goal of the invention is used are it is known in the art that still the present invention still makees as detailed as possible herein
Thin description.It will be apparent to those skilled in the art that within a context, if not specified, material therefor of the present invention and operating method
It is well known in the art.
Embodiment 1
By Copper substrate in concentration is for the watery hydrochloric acid of 1mol/L supersound washing 10min, then with distilled water flushing to Copper substrate
Surface in neutrality, then by Copper substrate in isometric acetone and alcohol mixed solution supersound washing 10min, vacuum drying,
Copper substrate after being cleaned.
Conductive agent tetrabutylammonium chloride is dried into 24h in 80 DEG C of vacuum drying chamber, to remove moisture therein.
Tetrabutylammonium chloride (TBACl) is dissolved in propene carbonate organic solvent, the concentration of tetrabutylammonium chloride is
0.1M, again by SiCl after uniform stirring4It is added in above-mentioned solution, SiCl4Concentration is 0.3M, and working electrode is metal copper foil, auxiliary
Help electrode for platinum plate electrode, reference electrode is platinum filament.Constant potential electro-deposition, operating voltage is -1.6V, and temperature is 25 DEG C, is passed through
The product silicon in copper foil surface is obtained after 2h electro-deposition, after Copper Foil is taken out from electrolyte, carbonic allyl ester solution is first passed through
Washing, then washed with acetone, to remove the impurity on surface, it is then transferred into argon gas atmosphere glove box.
Embodiment 2
Other are such as embodiment 1.
Tetrabutylammonium chloride (TBACl) is dissolved in propene carbonate organic solution, the concentration of tetrabutylammonium chloride is
0.1M, again by SiCl after uniform stirring4It is added in above-mentioned solution, SiCl4Concentration is 0.5M, and working electrode is metal copper foil, auxiliary
Help electrode for platinum plate electrode, reference electrode is platinum filament.Constant pressure electro-deposition, operating voltage is -1.6V, and temperature is 25 DEG C, by 2h
The product silicon in copper foil surface is obtained after electro-deposition, after Copper Foil is taken out from electrolyte, carbonic allyl ester solution is first passed through and is washed
Wash, then washed with acetone soln, to remove the impurity on surface, be then transferred into argon gas atmosphere glove box.
Embodiment 3
Other are such as embodiment 1.
Tetrabutylammonium chloride (TBACl) is dissolved in propene carbonate organic solution, the concentration of tetrabutylammonium chloride is
0.1M, again by SiCl after uniform stirring4It is added in above-mentioned solution, SiCl4Concentration is 0.7M, and working electrode is metal copper foil, auxiliary
Help electrode for platinum plate electrode, reference electrode is platinum filament.Constant pressure electro-deposition, operating voltage is -1.6V, and temperature is 25 DEG C, by 2h
The product silicon in copper foil surface is obtained after electro-deposition, after Copper Foil is taken out from electrolyte, carbonic allyl ester solution is first passed through and is washed
Wash, then washed with acetone soln, to remove the impurity on surface, be then transferred into argon gas atmosphere glove box.
Embodiment 4
Other are such as embodiment 1.
Tetrabutylammonium chloride (TBACl) is dissolved in propene carbonate organic solution, the concentration of tetrabutylammonium chloride is
0.1M, again by SiCl after uniform stirring4It is added in above-mentioned solution, SiCl4Concentration is 0.5M, and working electrode is metal copper foil, auxiliary
Help electrode for platinum plate electrode, reference electrode is platinum filament.Constant pressure electro-deposition, operating voltage is -1.6V, and temperature is 25 DEG C, by 3h
The product silicon in copper foil surface is obtained after electro-deposition, after Copper Foil is taken out from electrolyte, carbonic allyl ester solution is first passed through and is washed
Wash, then washed with acetone soln, to remove the impurity on surface, be then transferred into argon gas atmosphere glove box.
Embodiment 5
Other are such as embodiment 1.
Tetrabutylammonium chloride (TBACl) is dissolved in propene carbonate organic solution, the concentration of tetrabutylammonium chloride is
0.1M, again by SiCl after uniform stirring4It is added in above-mentioned solution, SiCl4Concentration is 0.5M, and working electrode is metal copper foil, auxiliary
Help electrode for platinum plate electrode, reference electrode is platinum filament.Constant pressure electro-deposition, operating voltage is -1.6V, and temperature is 25 DEG C, by 4h
The product silicon in copper foil surface is obtained after electro-deposition, after Copper Foil is taken out from electrolyte, carbonic allyl ester solution is first passed through and is washed
Wash, then washed with acetone soln, to remove the impurity on surface, be then transferred into argon gas atmosphere glove box.
Embodiment 6
Other are such as embodiment 1.
Tetrabutylammonium chloride (TBACl) is dissolved in propene carbonate organic solution, the concentration of tetrabutylammonium chloride is
0.1M, again by SiCl after uniform stirring4It is added in above-mentioned solution, SiCl4Concentration is 0.5M, and working electrode is metal foam copper,
Auxiliary electrode is platinum plate electrode, and reference electrode is platinum filament.Constant pressure electro-deposition, operating voltage is -1.6V, and temperature is 25 DEG C, is passed through
The product silicon in copper foil surface is obtained after 2h electro-deposition, after Copper Foil is taken out from electrolyte, carbonic allyl ester solution is first passed through
Washing, then washed with acetone soln, to remove the impurity on surface, it is then transferred into argon gas atmosphere glove box.
Embodiment 9
Other are such as embodiment 1.
Tetrabutylammonium chloride (TBACl) is dissolved in propene carbonate, the concentration of tetrabutylammonium chloride is 0.1M, uniformly
Again by SiCl after stirring4It is added in above-mentioned solution, SiCl4Concentration is 0.5M, and working electrode is metal porous copper, auxiliary electrode
It is platinum plate electrode, reference electrode is platinum filament.Constant pressure electro-deposition, operating voltage is -1.6V, and temperature is 25 DEG C, by 2h electro-deposition
The product silicon in copper foil surface is obtained afterwards, after Copper Foil is taken out from electrolyte, first passes through carbonic allyl ester solution washing, then use
Acetone soln is washed, and to remove the impurity on surface, is then transferred into argon gas atmosphere glove box.
Embodiment 10
The present embodiment is used to illustrate the preparation of electrode slice and battery.
Above-mentioned post-depositional unformed film nano silicon electrode is prepared into lithium ion battery, is concretely comprised the following steps：To prepare
Good electrode active material is cut into the pole piece of a diameter of 10mm after drying, weighing records standby.Being assemblied in for simulated battery is full of
Carried out in the glove box of Ar atmosphere, with the LiPF6/EC+DEC (EC of 1M:DEC=1：1) solution is used as electrolyte, cathode pole piece lithium
Piece is comparison electrode, is assembled into button cell.Then it is tested in blue electricity CT2001A type charging-discharge tester systems, is surveyed
Examination voltage is 0.01-1.5V, and current density is 300mA/g.The first circle discharge capacity of the visible film nano silicon electrodes of Fig. 5 is
4800mAh/g, first circle charging capacity is 1300mAh/g.The cyclical stability of the visible film nano silicon electrodes of Fig. 6, electrode material
Charging and discharging capacity after the circle of circulation 200 is maintained at 1000mAh/g.(a) is the forthright again of film nano silicon electrode in Fig. 7
Can, current density from 300mA/g, 500mA/g, 1000mA/g, 2000mA/g, its capacity be 1200mAh/g, 1100mAh/g,
900mAh/g, 600mAh/g, when current density returns to 300mAh/g, its capacity restoration to 1200mAh/g.Fig. 8 is film
The impedance spectra of nanometer silicon electrode, it is seen that with the growth of the circulation number of turns, the summation of SEI film resistances and load transfer resistance subtracts always
It is small.
Claims (8)
1. a kind of preparation method of unformed film nano silicon thin film, it is characterised in that comprise the following steps：First by conductive agent
It is dried, to remove moisture therein, is dissolved in organic solvent after drying, silicon compound is subsequently adding, using three electrodes
System, carries out constant potential electro-deposition at normal temperatures, cleans copper surface after electro-deposition with organic solvent, obtains unformed film nano
Silicon.
2. according to the method for claim 1, it is characterised in that the silicon compound for being dissolved in organic solvent is SiCl4, SiBr4、SiI4
Or SiHCl3In one or more.
3. according to the method for claim 1, it is characterised in that conductive agent is quaternary ammonium salt tetramethyl ammonium chloride (TMAC), tetraethyl
One or more in ammonium chloride (TEAC), 4-propyl ammonium chloride (TPAC) or tetrabutylammonium chloride (TBAC).
4. in accordance with the method for claim 1, it is characterised in that organic solvent is aprotic solvent propene carbonate
(PC), ethylene carbonate (EC), tetrahydrofuran (THF) or acetonitrile (CH3CN one or more in).
5. according to the method for claim 1, it is characterised in that working electrode is metallic copper in described electrodepositing silicon system, auxiliary
Help electrode for platinized platinum, reference electrode is platinum filament.
6. according to the method for claim 1, it is characterised in that concentration of the silicon compound in organic solvent electrolyte is
0.3M~1M, the conductive agent concentration is 0.1M~0.5M, and the current potential during constant potential electro-deposition is -1.6~-2.7V, institute
The sedimentation time stated is 1h~10h.
7. according to the method for claim 1, it is characterised in that electro-deposition product is cleaned with organic solution solution first, then with third
The cleaning of ketone solution removes the impurity of remained on surface.
8. the application of the unformed film nano silicon thin film for being prepared according to claim 1-7 any one methods, as lithium from
The negative material of sub- battery is assembled into button cell.
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| CN201710167676.3A CN106898726A (en) | 2017-03-20 | 2017-03-20 | A kind of noncrystalline membrane nano-silicon electrode material is prepared and applied in lithium ion battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107394176A (en) * | 2017-07-31 | 2017-11-24 | 中国地质大学（北京） | Si-C composite material, preparation method and application and lithium ion battery negative material |
| CN111370650A (en) * | 2020-03-16 | 2020-07-03 | 湘潭大学 | Amorphous silicon-graphite composite material and preparation method and application thereof |
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| CN101667638A (en) * | 2009-09-04 | 2010-03-10 | 上海交通大学 | Preparation method of lithium silicon alloy membrane electrode used for lithium ion battery |
| US20130078532A1 (en) * | 2011-09-27 | 2013-03-28 | Zonghai Chen | Non-aqueous electrolytes for lithium ion batteries |
| CN104064732A (en) * | 2014-07-07 | 2014-09-24 | 盐城市新能源化学储能与动力电源研究中心 | Method for preparing cathode of lithium ion battery with lithium-silicon film through pulse electrodeposition |
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2017
- 2017-03-20 CN CN201710167676.3A patent/CN106898726A/en active Pending
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| CN101667638A (en) * | 2009-09-04 | 2010-03-10 | 上海交通大学 | Preparation method of lithium silicon alloy membrane electrode used for lithium ion battery |
| US20130078532A1 (en) * | 2011-09-27 | 2013-03-28 | Zonghai Chen | Non-aqueous electrolytes for lithium ion batteries |
| CN104064732A (en) * | 2014-07-07 | 2014-09-24 | 盐城市新能源化学储能与动力电源研究中心 | Method for preparing cathode of lithium ion battery with lithium-silicon film through pulse electrodeposition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107394176A (en) * | 2017-07-31 | 2017-11-24 | 中国地质大学（北京） | Si-C composite material, preparation method and application and lithium ion battery negative material |
| CN111370650A (en) * | 2020-03-16 | 2020-07-03 | 湘潭大学 | Amorphous silicon-graphite composite material and preparation method and application thereof |
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Application publication date: 20170627 |