CN109755506A - A kind of Si-C composite material and preparation method thereof - Google Patents
A kind of Si-C composite material and preparation method thereof Download PDFInfo
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- CN109755506A CN109755506A CN201811545910.2A CN201811545910A CN109755506A CN 109755506 A CN109755506 A CN 109755506A CN 201811545910 A CN201811545910 A CN 201811545910A CN 109755506 A CN109755506 A CN 109755506A
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Abstract
The present invention is suitable for the invention belongs to technical field of lithium batteries, more particularly to a kind of Si-C composite material and preparation method thereof, the described method includes: being added the cetyl trimethylammonium bromide of 4-8 parts by weight into hydrochloric acid alcohol-water mixture, it is uniformly mixed under condition of ice bath；The ammonium sulfate for continuously adding 6-15 parts by weight is stirred to react 20-60 minutes under condition of ice bath；The silicon particle that the partial size of 0.2-0.8 parts by weight is 30-150nm is added in the solution containing white precipitate, the aniline monomer of 2-4.5 parts by weight is continuously added, is reacted 15-25 hours under condition of ice bath；Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, calcined under the conditions of 550-800 DEG C 1-5 hours to get.The Si-C composite material individual particle of preparation of the embodiment of the present invention is high-visible, and particle diameter distribution is uniform, and no obvious agglomeration occurs, and discharge capacity is high.
Description
Technical field
The invention belongs to technical field of lithium batteries, and in particular to a kind of Si-C composite material and preparation method thereof.
Background technique
A kind of secondary cell of the lithium ion battery as a new generation has energy density height, service life cycle length, puts certainly
The advantages that electric rate is low and memory-less effect, therefore, in the past few years by extensively should in electric car, energy storage device,
Consumer electronics product, the fields such as electric tool.
Traditional commercial lithium battery mainly uses negative electrode material of the graphite as battery at present, but its theoretical specific capacity only has
372mAh g-1, it is unable to satisfy the application requirement of current high-energy density storage equipment.
In many negative electrode materials of lithium ion battery, silicon (Si) is considered most potential with high storage capacity
One of negative electrode material, and think the negative electrode material of new generation for being possible to substitution graphite.Silicon has very high specific capacity, and (it is theoretical
Specific capacity value reaches 4200mAh g-1) and extremely low embedding de- lithium voltage platform.However, silicon exists as the negative electrode material of lithium ion battery
In charge and discharge process, it is usually associated with huge volume change (300%), so that it is broken to occur that silicon materials easily on electrode slice
Phenomena such as broken, dusting, electrode coating falls off, capacity rapid decay is ultimately caused, seriously hinders it in lithium ion battery
Practical application；Simultaneously as silicon is semiconductor material, electric conductivity is poor, causes the high rate performance of silicon materials poor.
The prior art can overcome the volume expansion of silicon materials using carbon coating silicon to a certain extent, however traditional benefit
With the preparation methods such as ball-milling method, hot bath method, spray drying process, sintering process prepare carbon coating silicon materials there are covered effects not
It is good, and then lead to the problem for causing discharge capacity low there are particle agglomeration phenomenon.
Summary of the invention
The embodiment of the present invention provides a kind of preparation method of Si-C composite material, prepares silicon-carbon composite wood by this method
Material, to solve the above problems.
A kind of preparation method of Si-C composite material provided in an embodiment of the present invention, includes the following steps:
The cetyl trimethylammonium bromide of 4-8 parts by weight is added to the salt acid alcohol water that concentration is 0.5-2mol/L and is mixed
It in liquid, is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1 in the hydrochloric acid alcohol-water mixture:
2-3, the concentration of cetyl trimethylammonium bromide is 0.03-0.1g/ml in the mixed liquor；
The ammonium sulfate of 6-15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20-60 minutes, it is raw
At the solution containing white precipitate；
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30-150nm is added in the solution containing white precipitate,
The aniline monomer of 2-4.5 parts by weight is continuously added, is reacted 15-25 hours under condition of ice bath, bottle green product is generated；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5-2mol/L than the alcohol-water mixture alternating for 1:2-2
Eccentric cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45-80 DEG C, and the time is 30-120 points
Clock；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, in 550-800 DEG C of condition
Lower calcining 1-5 hours to get.
The embodiment of the present invention also provides a kind of Si-C composite material, and the Si-C composite material is made by the following method:
The cetyl trimethylammonium bromide of 4-8 parts by weight is added to the salt acid alcohol water that concentration is 0.5-2mol/L and is mixed
It in liquid, is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1 in the hydrochloric acid alcohol-water mixture:
2-3, the concentration of cetyl trimethylammonium bromide is 0.03-0.1g/ml in the mixed liquor；
The ammonium sulfate of 6-15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20-60 minutes, it is raw
At the solution containing white precipitate；
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30-150nm is added in the solution containing white precipitate,
The aniline monomer of 2-4.5 parts by weight is continuously added, is reacted 15-25 hours under condition of ice bath, bottle green product is generated；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5-2mol/L than the alcohol-water mixture alternating for 1:2-2
Eccentric cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45-80 DEG C, and the time is 30-120 points
Clock；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, in 550-800 DEG C of condition
Lower calcining 1-5 hours to get.
The Si-C composite material individual particle of the preparation method of Si-C composite material provided in an embodiment of the present invention, preparation is clear
Clear as it can be seen that particle diameter distribution is uniform, no obvious agglomeration occurs, and discharge capacity height, reaches as high as 1130mAh/g or more.
Detailed description of the invention
Fig. 1 (a) is the electron microscope of the Si-C composite material for the method preparation that this bright embodiment 1 provides；
Fig. 1 (b) is the electron microscope of the Si-C composite material for the method preparation that comparative example 1 of the present invention provides；
Fig. 2 (a) is the electron microscope of the Si-C composite material for the method preparation that the embodiment of the present invention 2 provides；
Fig. 2 (b) is the electron microscope of the Si-C composite material for the method preparation that the embodiment of the present invention 3 provides；
Fig. 2 (c) is the electron microscope of the Si-C composite material for the method preparation that comparative example 2 of the present invention provides；
Fig. 3 is that the sintering temperature-of the Si-C composite material for the method preparation that 4-9 of the embodiment of the present invention is provided is discharged appearance for the first time
Magnitude relation schematic diagram.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The embodiment of the present invention provides a kind of preparation method of Si-C composite material, includes the following steps:
The cetyl trimethylammonium bromide of 4-8 parts by weight is added to the salt acid alcohol water that concentration is 0.5-2mol/L and is mixed
It in liquid, is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1 in the hydrochloric acid alcohol-water mixture:
2-3, the concentration of cetyl trimethylammonium bromide is 0.03-0.1g/ml in the mixed liquor；6- is added in the mixed liquor
The ammonium sulfate of 15 parts by weight is stirred to react 20-60 minutes under condition of ice bath, generates the solution containing white precipitate；By 0.2-
The silicon particle that the partial size of 0.8 parts by weight is 30-150nm is added in the solution containing white precipitate, continuously adds 2-4.5 weight
The aniline monomer of part is measured, is reacted 15-25 hours under condition of ice bath, bottle green product is generated；By the bottle green product 0.5-
The hydrochloric acid solution and alcohol water of 2mol/L is than the alcohol-water mixture alternating centrifugal cleaning for 1:2-2, in cleaning solution is colourless and is
Property, the wash products of acquisition；The wash products are subjected to predrying in a vacuum drying oven, temperature is 45-80 DEG C, and the time is
30-120 minutes；Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, at 550-800 DEG C
Under the conditions of calcine 1-5 hours to get.
In embodiments of the present invention, the purity of cetyl trimethylammonium bromide is between 95-99%, the purity of ammonium sulfate
Between 98~99.8%, the purity of aniline monomer is between 95-99%, the commercially available acquisition of above-mentioned raw material,
Details are not described herein.
The Si-C composite material individual particle of the preparation method of Si-C composite material provided in an embodiment of the present invention, preparation is clear
Clear as it can be seen that particle diameter distribution is uniform, no obvious agglomeration occurs, and discharge capacity height, reaches as high as 1130mAh/g or more.
It is carried out below in conjunction with process and effect of the specific embodiment to the preparation method of Si-C composite material of the invention detailed
It describes in detail bright.
Embodiment 1:
The cetyl trimethylammonium bromide of 6 parts by weight is added in the hydrochloric acid alcohol-water mixture for being 1mol/L to concentration,
It is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:1, institute in the hydrochloric acid alcohol-water mixture
The concentration for stating cetyl trimethylammonium bromide in mixed liquor is 0.5g/ml；
The ammonium sulfate of 10 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 40 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.5 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 3 parts by weight reacts 20 hours under condition of ice bath, generates bottle green product；
By the bottle green product hydrochloric acid solution of 1mol/L and alcohol water than for the alcohol-water mixture alternating centrifugal of 1:1 it is clear
It washes, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 60 DEG C, and the time is 80 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 750 DEG C
Burn 4 hours to get.
Embodiment 2:
The cetyl trimethylammonium bromide of 4 parts by weight is added to the hydrochloric acid alcohol-water mixture for being 0.5mol/L to concentration
In, it being uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 3:1 in the hydrochloric acid alcohol-water mixture,
The concentration of cetyl trimethylammonium bromide is 0.03g/ml in the mixed liquor；
The ammonium sulfate of 6 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 60 minutes, generation contains
The solution of white precipitate；
The silicon particle that the partial size of 0.2 parts by weight is 30nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 4.5 parts by weight reacts 15 hours under condition of ice bath, generates bottle green product；
By the bottle green product hydrochloric acid solution of 2mol/L and alcohol water than for the alcohol-water mixture alternating centrifugal of 2:1 it is clear
It washes, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 80 DEG C, and the time is 30 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 700 DEG C
Burn 3 hours to get.
Embodiment 3:
The cetyl trimethylammonium bromide of 4 parts by weight is added to the hydrochloric acid alcohol-water mixture for being 0.5mol/L to concentration
In, it being uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 3:1 in the hydrochloric acid alcohol-water mixture,
The concentration of cetyl trimethylammonium bromide is 0.03g/ml in the mixed liquor；
The ammonium sulfate of 6 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 60 minutes, generation contains
The solution of white precipitate；
The silicon particle that the partial size of 0.2 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 4.5 parts by weight reacts 15 hours under condition of ice bath, generates bottle green product；
By the bottle green product hydrochloric acid solution of 2mol/L and alcohol water than for the alcohol-water mixture alternating centrifugal of 2:1 it is clear
It washes, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 80 DEG C, and the time is 30 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 700 DEG C
Burn 3 hours to get.
Embodiment 4:
The cetyl trimethylammonium bromide of 8 parts by weight is added in the hydrochloric acid alcohol-water mixture for being 2mol/L to concentration,
It is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2, institute in the hydrochloric acid alcohol-water mixture
The concentration for stating cetyl trimethylammonium bromide in mixed liquor is 0.1g/ml；
The ammonium sulfate of 15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.8 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 2 parts by weight reacts 25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5mol/L than the alcohol-water mixture alternating centrifugal for 1:2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45 DEG C, and the time is 120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 550 DEG C
Burn 5 hours to get.
Embodiment 5:
The cetyl trimethylammonium bromide of 8 parts by weight is added in the hydrochloric acid alcohol-water mixture for being 2mol/L to concentration,
It is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2, institute in the hydrochloric acid alcohol-water mixture
The concentration for stating cetyl trimethylammonium bromide in mixed liquor is 0.1g/ml；
The ammonium sulfate of 15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.8 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 2 parts by weight reacts 25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5mol/L than the alcohol-water mixture alternating centrifugal for 1:2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45 DEG C, and the time is 120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 600 DEG C
Burn 4 hours to get.
Embodiment 6:
The cetyl trimethylammonium bromide of 8 parts by weight is added in the hydrochloric acid alcohol-water mixture for being 2mol/L to concentration,
It is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2, institute in the hydrochloric acid alcohol-water mixture
The concentration for stating cetyl trimethylammonium bromide in mixed liquor is 0.1g/ml；
The ammonium sulfate of 15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.8 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 2 parts by weight reacts 25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5mol/L than the alcohol-water mixture alternating centrifugal for 1:2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45 DEG C, and the time is 120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 650 DEG C
Burn 3 hours to get.
Embodiment 7:
The cetyl trimethylammonium bromide of 8 parts by weight is added in the hydrochloric acid alcohol-water mixture for being 2mol/L to concentration,
It is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2, institute in the hydrochloric acid alcohol-water mixture
The concentration for stating cetyl trimethylammonium bromide in mixed liquor is 0.1g/ml；
The ammonium sulfate of 15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.8 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 2 parts by weight reacts 25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5mol/L than the alcohol-water mixture alternating centrifugal for 1:2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45 DEG C, and the time is 120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 700 DEG C
Burn 2 hours to get.
Embodiment 8:
The cetyl trimethylammonium bromide of 8 parts by weight is added in the hydrochloric acid alcohol-water mixture for being 2mol/L to concentration,
It is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2, institute in the hydrochloric acid alcohol-water mixture
The concentration for stating cetyl trimethylammonium bromide in mixed liquor is 0.1g/ml；
The ammonium sulfate of 15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.8 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 2 parts by weight reacts 25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5mol/L than the alcohol-water mixture alternating centrifugal for 1:2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45 DEG C, and the time is 120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 750 DEG C
Burn 1.5 hours to get.
Embodiment 9:
The cetyl trimethylammonium bromide of 8 parts by weight is added in the hydrochloric acid alcohol-water mixture for being 2mol/L to concentration,
It is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2, institute in the hydrochloric acid alcohol-water mixture
The concentration for stating cetyl trimethylammonium bromide in mixed liquor is 0.1g/ml；
The ammonium sulfate of 15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.8 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 2 parts by weight reacts 25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5mol/L than the alcohol-water mixture alternating centrifugal for 1:2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45 DEG C, and the time is 120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 800 DEG C
Burn 1 hour to get.
Comparative example 1:
The ammonium sulfate of 10 parts by weight is added in the hydrochloric acid alcohol-water mixture of the 1mol/L of 1 dosage of embodiment, in ice bath item
It is stirred to react under part 40 minutes, generates the solution containing white precipitate；
The silicon particle that the partial size of 0.5 parts by weight is 100nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 3 parts by weight reacts 20 hours under condition of ice bath, generates bottle green product；
By the bottle green product hydrochloric acid solution of 1mol/L and alcohol water than for the alcohol-water mixture alternating centrifugal of 1:1 it is clear
It washes, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 60 DEG C, and the time is 80 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 750 DEG C
Burn 4 hours to get.
Comparative example 2:
Embodiment 2:
The cetyl trimethylammonium bromide of 4 parts by weight is added to the hydrochloric acid alcohol-water mixture for being 0.5mol/L to concentration
In, it being uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 3:1 in the hydrochloric acid alcohol-water mixture,
The concentration of cetyl trimethylammonium bromide is 0.03g/ml in the mixed liquor；
The ammonium sulfate of 6 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 60 minutes, generation contains
The solution of white precipitate；
The silicon particle that the partial size of 0.2 parts by weight is 200nm is added in the solution containing white precipitate, is continuously added
The aniline monomer of 4.5 parts by weight reacts 15 hours under condition of ice bath, generates bottle green product；
By the bottle green product hydrochloric acid solution of 2mol/L and alcohol water than for the alcohol-water mixture alternating centrifugal of 2:1 it is clear
It washes, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 80 DEG C, and the time is 30 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 700 DEG C
Burn 3 hours to get.
The Si-C composite material prepared for above-described embodiment 1 and comparative example 1 carries out electron-microscope scanning analysis, obtains such as Fig. 1
(a) electron microscope with 1 (b), wherein 1 (a) is the electron microscope of 1 product of embodiment, and 1 (b) is the electron microscope of comparative example 1, can be seen
Out, Fig. 1 (a) individual particle is high-visible, and particle diameter distribution is uniform, and no obvious agglomeration occurs, and Fig. 1 (b) is produced because of reunion
The integrated stress that raw macroaggregate is subject to is the comprehensive superposition of individual particle stress.In conjunction with the embodiments 1 and comparative example 1
Preparation process can reduce the surface of silicon nanoparticle it is found that joined stability cationicsurfactants in embodiment 1
Tension plays the role of discrete particles, inhibits particle agglomeration；And comparative example 1 is the product after the cladding of surfactant-free, because
Reunite and the integrated stress that is subject to of macroaggregate that generates is the comprehensive superposition of individual particle stress, is easy to make aggregate
It is destroyed at structure, to reduce the overall stability of electrode.
Electron-microscope scanning analysis is carried out for above-described embodiment 2-3 and comparative example 2 Si-C composite material prepared, is obtained as schemed
2 (a) and 2 (b) and 2 (c) electron microscope, wherein Fig. 2 (a) is the electron microscope of 2 product of embodiment, and Fig. 2 (b) is 3 product of embodiment
Electron microscope, Fig. 2 (c) is the electron microscope of 2 product of comparative example.2-3, comparative example 2 and above-mentioned electron microscope can be seen in conjunction with the embodiments
Out, the cladding situation of the silicon of different-grain diameter, with the increase of silicon grain diameter, carbon coating layer thickness is gradually decreased, the silicon of small particle, shape
It is visibly homogeneous at the dispersion of silicon-carbon composite cathode material, particle diameter distribution is relatively narrow, and silicon particle surface layer is obviously coated with one layer of carbon
Film, the thickness of surface coating layer gradually decreases when partial size increases, and agglomeration occurs in particle, illustrates the cladding of carbon-coating, to silicon
Dispersion, the reunion of grain are inhibited, and in comparative example 2, when silicon grain diameter reaches 200nm, it is existing that apparent reunion occurs in particle
As.
For the Si-C composite material of embodiment 4-9 preparation, it is assembled into half-cell respectively, electrochemistry is carried out by blue electricity
The test of energy tests their cycle performance test result, five embodiments for each material with reference to Fig. 3 under the multiplying power of 0.1C
Discharge capacity for the first time reach 1000mAh/g or more, wherein sintering temperature be 700 DEG C when, discharge capacity reaches for the first time
1130mAh/g or more, discharge capacity are high.
The Si-C composite material individual particle of the preparation method of Si-C composite material provided in an embodiment of the present invention, preparation is clear
Clear as it can be seen that particle diameter distribution is uniform, no obvious agglomeration occurs, and discharge capacity height, reaches as high as 1130mAh/g or more.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of preparation method of Si-C composite material, which comprises the steps of:
The cetyl trimethylammonium bromide of 4-8 parts by weight is added to the hydrochloric acid alcohol-water mixture for being 0.5-2mol/L to concentration
In, it is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2- in the hydrochloric acid alcohol-water mixture
3, the concentration of cetyl trimethylammonium bromide is 0.03-0.1g/ml in the mixed liquor；
The ammonium sulfate of 6-15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20-60 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30-150nm is added in the solution containing white precipitate, is continued
The aniline monomer of 2-4.5 parts by weight is added, is reacted 15-25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5-2mol/L than the alcohol-water mixture alternating centrifugal for 1:2-2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45-80 DEG C, and the time is 30-120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 550-800 DEG C
Burn 1-5 hours to get.
2. the preparation method of Si-C composite material as described in claim 1, which is characterized in that described in atmosphere of inert gases
Under, the step of the wash products after predrying are placed in tube furnace, are calcined 1-5 hours under the conditions of 550-800 DEG C, tool
Body are as follows:
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 650-800 DEG C
It burns 1-5 hours.
3. the preparation method of Si-C composite material as described in claim 1, which is characterized in that described in atmosphere of inert gases
Under, the step of the wash products after predrying are placed in tube furnace, are calcined 1-5 hours under the conditions of 550-800 DEG C, tool
Body are as follows:
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, calcine 1- under the conditions of 700 DEG C
5 hours.
4. the preparation method of Si-C composite material as described in claim 1, which is characterized in that described by 0.2-0.8 parts by weight
Partial size be that the step in the solution containing white precipitate is added in the silicon particle of 30-150nm, specifically:
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30-100nm is added in the solution containing white precipitate.
5. the preparation method of Si-C composite material as described in claim 1, which is characterized in that described by 0.2-0.8 parts by weight
Partial size be that the step in the solution containing white precipitate is added in the silicon particle of 30-150nm, specifically:
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30 is added in the solution containing white precipitate.
6. a kind of Si-C composite material, which is characterized in that the Si-C composite material is made by the following method:
The cetyl trimethylammonium bromide of 4-8 parts by weight is added to the hydrochloric acid alcohol-water mixture for being 0.5-2mol/L to concentration
In, it is uniformly mixed under condition of ice bath and forms mixed liquor, wherein the volume ratio of alcohol water is 1:2- in the hydrochloric acid alcohol-water mixture
3, the concentration of cetyl trimethylammonium bromide is 0.03-0.1g/ml in the mixed liquor；
The ammonium sulfate of 6-15 parts by weight is added in the mixed liquor, is stirred to react under condition of ice bath 20-60 minutes, generation contains
There is the solution of white precipitate；
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30-150nm is added in the solution containing white precipitate, is continued
The aniline monomer of 2-4.5 parts by weight is added, is reacted 15-25 hours under condition of ice bath, generates bottle green product；
By the bottle green product with the hydrochloric acid solution and alcohol water of 0.5-2mol/L than the alcohol-water mixture alternating centrifugal for 1:2-2
Cleaning, until cleaning solution is colourless and is neutrality, the wash products of acquisition；
The wash products are subjected to predrying in a vacuum drying oven, temperature is 45-80 DEG C, and the time is 30-120 minutes；
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 550-800 DEG C
Burn 1-5 hours to get.
7. Si-C composite material as claimed in claim 6, which is characterized in that it is described under atmosphere of inert gases, it will be by pre-
The step of wash products after drying are placed in tube furnace, are calcined 1-5 hours under the conditions of 550-800 DEG C, specifically:
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, are forged under the conditions of 650-800 DEG C
It burns 1-5 hours.
8. Si-C composite material as claimed in claim 6, which is characterized in that it is described under atmosphere of inert gases, it will be by pre-
The step of wash products after drying are placed in tube furnace, are calcined 1-5 hours under the conditions of 550-800 DEG C, specifically:
Under atmosphere of inert gases, the wash products after predrying are placed in tube furnace, calcine 1- under the conditions of 700 DEG C
5 hours.
9. Si-C composite material as claimed in claim 6, which is characterized in that the partial size by 0.2-0.8 parts by weight is 30-
The step in the solution containing white precipitate is added in the silicon particle of 150nm, specifically:
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30-100nm is added in the solution containing white precipitate.
10. Si-C composite material as claimed in claim 6, which is characterized in that the partial size by 0.2-0.8 parts by weight is
The step in the solution containing white precipitate is added in the silicon particle of 30-150nm, specifically:
The silicon particle that the partial size of 0.2-0.8 parts by weight is 30nm is added in the solution containing white precipitate.
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