CN109817962A - A kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method of phenolic resin modification - Google Patents
A kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method of phenolic resin modification Download PDFInfo
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Abstract
The present invention provides the Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method of a kind of modification of phenolic resin, the material is modified to nano silicon particles pyrogenically prepared by using phenolic resin, phenolic resin crosslinking is carried out on silicon nanoparticle surface, phenolic resin after making crosslinking coats silicon nanoparticle, then pyrolysis obtains the nanometer silicon composite material of porous carbon cladding, i.e. the lithium ion battery silicon based anode material of phenolic resin modification in inert atmosphere.The electric conductivity of the porous carbon-coated nanometer silicon composite material and the volume change of charge and discharge process have compared to nano silicon particles to be obviously improved, and capacity holding capacity is high, electrochemical performance；And the present invention uses the phenolic resin of green low cost as covering material in preparation process, and preparation method is simple, and raw material is easy to get, mild condition, can produce in batches, has fine preparation of industrialization prospect.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, specially a kind of lithium-ion electric of phenolic resin modification
Pond silicon based anode material and preparation method.
Background technique
Lithium ion battery is widely applied on the portable electronic devices such as mobile phone, laptop, is tentatively made
With on electric car, it is contemplated that can large-scale use in future.Main target is in the exploitation of next-generation lithium ion battery
Extend cycle life, improves energy density and charging and discharging capacity.Negative electrode material becomes the pass for determining that can this target be realized
Key.
Graphite is as widely used negative electrode material in current lithium ion battery, theoretical specific capacity 372mAh g-1, cannot
It adapts at present to the widespread demand of large capacity, high power electrochmical power source.Therefore find can be kept under low potential high capacity with
High-power material is very important work to substitute graphite.The theoretical lithium storage content of silicon (Si) is up to 4200mAh g-1, it is
11 times of graphite theoretical capacity.The voltage platform of silicon is slightly above graphite, and the phenomenon that causing surface to analyse lithium, safety are difficult in charging
Performance is better than graphite cathode material.It is nontoxic in addition, silicon is the highest element of abundance in the earth's crust, it is from a wealth of sources, deposit is abundant, valence
Lattice are cheap, therefore silicon is the most promising candidate of electrode material of next-generation lithium ion battery.
During the electrochemical lithium storage of silicon, average each silicon atom combines 4.4 lithium atoms to obtain Li22Si5Alloy phase,
The volume change of material reaches 300% or more simultaneously.The mechanicals efforts that so huge bulk effect generates can make electrode active
It is gradually disengaged between property substance and collector, after charge and discharge, silicon active phase itself can also rupture, dusting, structural breakdown,
Occur to cause the serious destruction of electrode material structure, in addition the electric conductivity of silicon is very from crystalline state to amorphous irreversible transformation
It is low, cause irreversible capacity to generate, electrode cycle performance is caused to decline rapidly.In addition, silicon is semiconductor material, intrinsic conductivity
It is low, only 6.7 × 10-4S·cm-1, electric conductivity needs to improve.
Therefore, the enormousness effect and lower conductivity generated in charge and discharge process seriously hinders silicon as lithium ion
The commercial applications of cell negative electrode material.
Summary of the invention
The purpose of the invention is in view of the deficiencies of the prior art, provide a kind of lithium ion battery of phenolic resin modification
Silicon based anode material and preparation method thereof is obtained by using phenolic resin pyrolysis modified to nano silicon particles, i.e., in nanometer
Silicon particle surface carries out the crosslinking of phenolic resin, to make phenolic resin coat nano silicon particles, then in inert atmosphere
Pyrolysis obtains the silicon nanocomposite of porous carbon cladding.The preparation method is simple, and mild condition, raw material is easy to get；What is obtained is more
The carbon-coating of the carbon-coated silicon nanocomposite in hole is conducive to store more Li there are more defects and more activated centres
The transmission of+ion and electronics conduction, while the buffering of soft charcoal layer avoids active material that dusting occurs in charge and discharge process, so that should
Composite material capacity holding capacity is higher, has excellent chemical property.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification, by using phenolic resin pair
Nano silicon particles are modified pyrogenically prepared, comprising the following steps:
Nano silicon particles are added in the aqueous solution of phenolic resin and are uniformly mixed, 2,5- dimercapto -1,3,4- is then added
The ethanol solution of thiadiazoles, and surfactant is added under agitation, then initiator is added dropwise, after stirring 24~72h
Solvent is evaporated, obtained solid product is heated to 20~120 DEG C in oxygen-free environment and is tentatively crosslinked, finally in indifferent gas
In body atmosphere in 700~1000 DEG C pyrolysis obtain porous carbon cladding silicon nanocomposite, i.e., phenolic resin modification lithium from
Sub- battery silicon based anode material；
Wherein, phenolic resin, nano silicon particles, 2,5- dimercapto-1,3,4-thiadiazole, surfactant and initiator
Mass ratio is 0.3:0.1:1.5:0.5~0.52:6.85.
Preferably, the partial size of nano silicon particles is 70~150nm, and the mass concentration of the aqueous solution of phenolic resin is 6g/L,
0.5~4h of ultrasound at 20~40 DEG C is uniformly mixed nano silicon particles with the aqueous solution of the phenolic resin.
Preferably, the mass concentration of the ethanol solution of 2,5- dimercapto-1,3,4-thiadiazole is 30g/L.
Preferably, surfactant is cetyl trimethylammonium bromide or sodium cetanesulfonate, and stirring rate is
500~800r/min.
Preferably, initiator is ammonium persulfate solution, and the mass concentration of ammonium persulfate solution is 137g/L, and ammonium persulfate is molten
The rate of addition of liquid is 1~10mL/min.
Preferably, evaporation solvent uses revolving method, and revolving temperature is 30~90 DEG C, and the revolving time is 0.1~2h.
Preferably, the soaking time that solid product is tentatively crosslinked is 0.5~72h, and preliminary crosslinking passes through vacuum oven reality
Existing oxygen-free environment.
Preferably, pyrolytic process are as follows: be warming up to 700~1000 DEG C according to the heating rate of 3 DEG C/min, keep the temperature 0.5~7h；
Inert gas is argon gas.
The lithium ion battery silicon substrate cathode material for the phenolic resin modification that the present invention also protects above-mentioned preparation method to be prepared
Material.
Compared with prior art, beneficial effects of the present invention are as follows:
1, the present invention is modified nano silicon particles by phenolic resin, i.e., carries out phenolic resin in nanometer silicon face
Crosslinking, the phenolic resin cladding silicon nanoparticle after making crosslinking, then pyrolysis obtains receiving for porous carbon cladding in inert atmosphere
Rice silicon composite, the present invention select the phenolic resin of green low cost as covering material, and raw material is easy to get, preparation method letter
Single, mild condition can be produced in batches, have fine preparation of industrialization prospect；
2, the present invention is conducive to electrolyte permeability by the cladding to nano-silicon progress porous carbon, to increase reaction position
Point, while carbon can make the structure of nanocomposite more stable, i.e. the buffering of soft charcoal layer avoids active material in charge and discharge
Dusting occurs in the process, and carbon-coating also generates more defects and more activated centres, is conducive to store more Li+From
Son transmission and electronics conduction；
3, the present invention effectively increases the electric conductivity of composite material by the cladding to nano-silicon progress porous carbon, and
Under the action of outer layer porous carbon, it is reduced in the volume change of charge and discharge process, and obtained composite material has excellent electricity
Chemical property.
Detailed description of the invention
Fig. 1 be in the present invention phenolic resin coated Si material as lithium ion battery negative material the shape in charge and discharge process
At stable SEI layer schematic diagram；
Fig. 2 is the preparation process schematic diagram of porous carbon-coated silicon nanocomposite in the present invention；
Fig. 3 is the scanning electron microscope of porous carbon-coated silicon nanocomposite prepared by the embodiment of the present invention 1 and comparative example 1
Figure；In figure: (a), (b), (c) be embodiment 1 sample Si@IIIC nanocomposite scanning electron microscope (SEM) photograph；It (d) is comparative example
The scanning electron microscope (SEM) photograph of porous carbon materials C@III in 1.
Fig. 4 is the transmission electron microscope picture of porous carbon-coated silicon nanocomposite prepared by the embodiment of the present invention 1；In figure:
It (a) is the transmission electron microscope picture of phenolic resin coated Si in embodiment 1；(b), (c) is the transmission electricity of novolac resin layer in embodiment 1
Mirror figure；(d), (e), (f) are the transmission electron microscope pictures of sample Si@IIIC nanocomposite in embodiment 1；It (g) is Selected area electron
Diffraction pattern；(h), (i) is the high-resolution-ration transmission electric-lens figure of sample Si@IIIC nanocomposite in embodiment 1；(j),(k),
(l) be the sample Si@IIIC nanocomposite of embodiment 1, Si, C element image map；
Fig. 5 is the XRD diagram of Si@IIIC nanocomposite prepared by the embodiment of the present invention 1；
Fig. 6 is the Raman figure of Si@IIIC nanocomposite prepared by the embodiment of the present invention 1
Fig. 7 is the N of Si@IIIC nanocomposite prepared by the embodiment of the present invention 12Adsorption desorption curve graph；
Fig. 8 is the chemical property figure of sample prepared by the embodiment of the present invention 1, embodiment 2, comparative example 1 and comparative example 2,
In figure: being (a) sample of embodiment 1 (Si@IIIC) and embodiment 2 (Si@IC) in 0.1Ag-1Current density under circulation it is steady
Qualitative test result；It (b) is the sample of comparative example 1 (C@III) and comparative example 2 (C@I) in 0.1Ag-1Current density under follow
Ring stability test result；(c) be embodiment 1 sample Si@IIIC cyclic voltammetry curve figure；(d) be embodiment 1 sample
The electrochemical impedance test result figure of Si@IIIC.
Specific embodiment
Below by specific embodiments and the drawings, the present invention will be described in detail.The scope of the present invention is not limited to this
Specific embodiment.
Embodiment 1
A kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification, comprising the following steps:
0.3g phenolic resin is added in the water of 50ml, stir to being completely dissolved, then be added 0.1g partial size be 70~
The nano silicon particles of 130nm, and ultrasound 4h is uniformly mixed it at 40 DEG C.Then by 1.5g 2,5- dimercapto -1,3,4- thiophene
Diazole, which is dissolved in 50ml ethyl alcohol, obtains the ethanol solution of 2,5- dimercapto-1,3,4-thiadiazole, and by itself and phenolic resin and silicon
The mixed solution of nano particle mixes, and 0.5g cetyl trimethyl bromination is then added under the stirring condition of 500r/min
Ammonium, and continue stirring to avoid reunion.Then 6.85g ammonium persulfate is dissolved in 50mL water and obtains ammonium persulfate solution, and according to
Ammonium persulfate solution is added drop-wise in above-mentioned solution by the drop rate of 2mL/min dropwise.After stirring for 24 hours, rotated at 50 DEG C
Product is collected after 0.5h, obtained solid is heated in a vacuum drying oven 120 DEG C, heating for 24 hours, is crosslinked it tentatively.Then,
It is warming up to 900 DEG C according to the heating rate of 3 DEG C/min in argon atmosphere again, 5h is kept the temperature, makes its pyrolysis, obtain porous carbon
The Silicon Based Anode Materials for Lithium-Ion Batteries of the silicon nanocomposite of cladding, i.e. phenolic resin modification, is denoted as Si@IIIC.
Embodiment 2
It is identical as the method and steps of embodiment 1, the difference is that the pyrolysis temperature of preliminary cross-linking products is 700 DEG C, obtain
Phenolic resin modification Silicon Based Anode Materials for Lithium-Ion Batteries, be denoted as Si@IC.
Embodiment 3
It is identical as the method and steps of embodiment 1, the difference is that the pyrolysis temperature of preliminary cross-linking products is 800 DEG C.
Embodiment 4
It is identical as the method and steps of embodiment 1, the difference is that the pyrolysis temperature of preliminary cross-linking products is 1000 DEG C.
Embodiment 5
It is identical as the method and steps of embodiment 1, the difference is that 0.52g cetyl trimethylammonium bromide is added.
Embodiment 6
It is identical as the method and steps of embodiment 2, the difference is that 0.52g cetyl trimethylammonium bromide is added.
Embodiment 7
It is identical as the method and steps of embodiment 1, the difference is that the surfactant being added is sodium cetanesulfonate.
Comparative example 1
Phenolic resin is directly carried out to crosslinking pyrolysis according to the method for embodiment 1, obtains porous carbon materials, is denoted as C@III.
Comparative example 2
It is identical as the process of comparative example 1, the difference is that the pyrolysis temperature of comparative example 2 is 700 DEG C, it is denoted as C@I.
The sample that we prepare embodiment 1, embodiment 2 and comparative example 1, comparative example 2 carries out physical property characterization, including scanning
Electron microscope, transmission electron microscope, X-ray diffraction, Raman spectrum and the test of nitrogen adsorption desorption；We are by embodiment simultaneously
1 sample Si IIIC has carried out the assembling of battery and can be carried out test to its electrochemistry.
First by sample made from embodiment 1 and mass fraction be 10% polyvinylidene fluoride, mass fraction 10%
Carbon black according to 8:1:1 mass ratio mix, and be added N-Methyl pyrrolidone mixing be completely dispersed its said mixture, make
At slurry and be pasted on copper foil, in 80 DEG C of dry 3h, then in 80 DEG C of vacuum drying 12h, then be dissolved in ethylene carbonate/
LiPF in dimethyl carbonate6For electrolyte, CR2025 type battery is assembled in applying argon gas glove box.
Fig. 1 is that the sample of embodiment in the present invention forms stabilization as lithium ion battery negative material in charge and discharge process
SEI layer schematic diagram；Fig. 2 is the preparation process schematic diagram of embodiment sample in the present invention；Fig. 3, Fig. 4, Fig. 5, Fig. 6 and Fig. 7 points
It Wei not the SEM figure of the sample for preparing of Examples 1 to 2 and comparative example 1~2, TEM figure, XRD diagram, Raman figure and nitrogen adsorption desorption song
Line.
Fig. 3 (a), (b), (c) be embodiment 1 sample Si@IIIC nanocomposite scanning electron microscope (SEM) photograph；It (d) is pair
The scanning electron microscope (SEM) photograph of porous carbon materials C@III in ratio 1；From figure 3, it can be seen that the silicon nanometer modified by phenolic resin
The surface of grain becomes coarse, illustrates that carbon is successfully coated on nano silicon particles surface；It is obtained after illustrating phenolic resin crosslinking pyrolysis simultaneously
To porous structure.
(a) is the transmission electron microscope picture of phenolic resin coated Si in embodiment 1 in Fig. 4；(b), (c) is phenolic aldehyde in embodiment 1
The transmission electron microscope picture of resin layer；(d), (e), (f) are the transmission electron microscope pictures of sample Si@IIIC nanocomposite in embodiment 1；
It (g) is selective electron diffraction figure；(h), (i) is the high-resolution-ration transmission electric-lens of sample Si@IIIC nanocomposite in embodiment 1
Figure；(j), (k), (l) are the element image map of the sample Si@IIIC nanocomposite of embodiment 1, Si, C；It can from Fig. 4
Out, the surface coated carbon layers having thicknesses of nano silicon particles are 7nm or so, can by Elemental redistribution map (j), (k), (l) in Fig. 4
To find out, carbon-coating is uniformly wrapped in the surface of nano silicon particles, is consistent with the result of Fig. 3.
Fig. 5 and Fig. 6 is the XRD diagram and Raman figure of sample Si@IIIC prepared by embodiment 1 respectively, from fig. 5, it can be seen that
The peak and card JCPDS No.27-1402 generated in the sample of embodiment 1 exactly matches, it was demonstrated that contains inside the sample of embodiment 1
There is Si；Then further component analysis is carried out using sample of the Raman to embodiment 1, from fig. 6, it can be seen that having on spectrogram bright
The aobvious peak G and the peak D illustrates that there are carbon in the sample, and is agraphitic carbon.
Fig. 7 is the nitrogen adsorption desorption curve graph of the sample Si@IIIC of embodiment 1, from figure 7 it can be seen that embodiment 1 obtains
Sample Si@IIIC be porous structure.
Therefore, it by morphology characterization and structural characterization, obtains, the sample Si IIIC of embodiment 1 is porous carbon-coated silicon
Nanocomposite.
Fig. 8 is the chemical property figure of sample prepared by embodiment 1, embodiment 2, comparative example 1 and comparative example 2, wherein (a)
Figure be under different calcination temperatures porous carbon-coated silicon nanocomposite in 0.1Ag-1Current density under cyclical stability
Test result, (a) are sample the following under the current density of 0.1Ag-1 of embodiment 1 (Si@IIIC) and embodiment 2 (Si@IC)
Ring stability test result；It (b) is the sample of comparative example 1 (C@III) and comparative example 2 (C@I) in 0.1Ag-1Current density under
Cyclical stability test result, that is, under different pyrolysis temperature porous carbon materials cyclical stability test result；(c) it is
The cyclic voltammetry curve figure of the sample Si@IIIC of embodiment 1；(d) be embodiment 1 sample Si@IIIC electrochemical impedance survey
Test result figure；From Fig. 8 (a) it can be seen that the composite material after 900 DEG C of processing has preferable specific discharge capacity and follows
Ring stability；From Fig. 8 (b) as can be seen that the porous carbon materials C@III prepared under the conditions of 900 DEG C also has preferable electric discharge ratio
Capacity, but performance is obviously poor compared with the sample Si@IIIC of embodiment 1, illustrates that porous carbon is made jointly with silicon nanoparticle
With, make embodiment 1 sample have good chemical property；From Fig. 8 (c) as can be seen that corresponding peak is Si in figure, show
The performance of the material is Si；After Fig. 8 (d) shows that the sample Si@IIIC of embodiment 1 surveys circulation by 20, the impedance of battery
Increase.So being found out by electrochemical property test, porous carbon-coated silicon nanocomposite prepared by the present invention passes through more
Hole carbon coating nano silicon particles increase material conductivity and reduce it in the volume change of charge and discharge process, effectively enhance
The chemical property of material.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification, which is characterized in that by using
Phenolic resin is modified to nano silicon particles pyrogenically prepared, comprising the following steps:
Nano silicon particles are added in the aqueous solution of phenolic resin and are uniformly mixed, 2,5- dimercapto -1,3,4- thiophene two is then added
The ethanol solution of azoles, and surfactant is added under agitation, then initiator is added dropwise, it is evaporated after stirring 24~72h
Obtained solid product is heated in oxygen-free environment 20~120 DEG C and is tentatively crosslinked, finally in inert gas atmosphere by solvent
The silicon nanocomposite of porous carbon cladding, the i.e. lithium-ion electric of phenolic resin modification are obtained in 700~1000 DEG C of pyrolysis in enclosing
Pond silicon based anode material；
The quality of the phenolic resin, nano silicon particles, 2,5- dimercapto -1,3,4- thiadiazoles, surfactant and initiator
Than for 0.3:0.1:1.5:0.5~0.52:6.85.
2. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification according to claim 1,
It is characterized in that, the partial size of the nano silicon particles is 70~150nm, the mass concentration of the aqueous solution of phenolic resin is 6g/L,
0.5~4h of ultrasound at 20~40 DEG C is uniformly mixed the nano silicon particles with the aqueous solution of the phenolic resin.
3. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification according to claim 1,
It is characterized in that, the mass concentration of the ethanol solution of 2, the 5- dimercapto-1,3,4-thiadiazole is 30g/L.
4. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification according to claim 1,
It is characterized in that, the surfactant is cetyl trimethylammonium bromide or sodium cetanesulfonate, the stirring rate
For 500~800r/min.
5. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification according to claim 1,
It is characterized in that, the initiator is ammonium persulfate solution, the mass concentration of the ammonium persulfate solution is 137g/L, the mistake
The rate of addition of ammonium sulfate is 1~10mL/min.
6. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification according to claim 1,
It is characterized in that, the evaporation solvent uses revolving method, revolving temperature is 30~90 DEG C, and the revolving time is 0.1~2h.
7. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification according to claim 1,
It is characterized in that, the soaking time that the solid product is tentatively crosslinked is 0.5~72h.
8. a kind of preparation method of the Silicon Based Anode Materials for Lithium-Ion Batteries of phenolic resin modification according to claim 1,
It is characterized in that, the process of the pyrolysis are as follows: 700~1000 DEG C are warming up to according to the heating rate of 3 DEG C/min, heat preservation 0.5~
7h；The inert gas is argon gas.
9. the lithium ion battery for the phenolic resin modification that described in any item preparation methods are prepared according to claim 1~8
Silicon based anode material.
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Application publication date: 20190528 |