CN109686957A - A kind of preparation method of artificial graphite, SiO base silicon-carbon composite cathode material - Google Patents
A kind of preparation method of artificial graphite, SiO base silicon-carbon composite cathode material Download PDFInfo
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- CN109686957A CN109686957A CN201811649772.2A CN201811649772A CN109686957A CN 109686957 A CN109686957 A CN 109686957A CN 201811649772 A CN201811649772 A CN 201811649772A CN 109686957 A CN109686957 A CN 109686957A
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- H—ELECTRICITY
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- 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
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- 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
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- 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
- H01M4/625—Carbon or graphite
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides the preparation method of a kind of artificial graphite, SiO base silicon-carbon composite cathode material, is related to technical field of lithium ion battery negative, includes the following steps: 1) spherical SiO precursor preparation；2) preparation of artificial graphite, SiO ball；3) three big processes are prepared with four kinds of artificial graphite, pitch, SiO, special additive material preparation silicon substrate balls inside VC mixing machine.The present invention can effectively solve volume expansion of the lithium ion battery in charge and discharge process by the use of artificial graphite, SiO base silicon-carbon composite cathode material, improve the energy density of negative electrode material；Artificial plumbago negative pole material and SiO pass through pitch combined this structure well, it can be further improved the structural stability of this negative electrode material, entire invented technology process is simple, and artificial graphite, SiO base silicon-carbon composite cathode material have shown good physical property and electrochemistry in lithium ion battery negative material and battery performance test.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative more particularly to a kind of artificial graphite, SiO base silicon-carbon are multiple
Close the preparation method of negative electrode material.
Background technique
In lithium ion battery, graphite cathode material is the critical material in five big raw material, graphite cathode material because
Itself stability is strong, good cycle, with compatibility of electrolyte is high and the advantages such as cheap and becomes battery producer and exists
Primary selection when selection negative electrode material, but the country of attention and promotion due to to(for) new energy industry, it is clear that graphite cathode
The gram volume of material script 372, which has not had advantage, its high rate performance, can not meet new energy row in new energy industry
Requirement of the industry power battery to negative electrode material, therefore urgent a negative electrode material of exploitation can have good cyclicity simultaneously
The negative electrode material of energy and higher capacity is quite significant to meet the needs of new energy industry is for high-energy-density density.
The high-capacity cathode material having currently on the market mainly promising graphene additive negative electrode material, silicon-carbon cathode material
Material, the negative material of tin, aluminium ion battery etc., wherein still silicon-carbon cathode is slightly mature relatively and for technology, but volume expansion
It always is the technical barrier that silicon-carbon cathode faces, so that silicon-carbon cathode is difficult to exercise one's ability in industrial application.It is domestic not yet
Weary many projects with regard to silicon-carbon cathode there are the shortcomings that research and develop new structure, main direction of studying is come around carbon coating
Solve the expansion of silicon materials in the circulating cycle.
A kind of new direction is provided in the patent of Patent No. CN105118974 A, content is a kind of silicon-based anode
Material and preparation method thereof incorporates silicon materials in carbon nano-fiber due to being introduced into electrospinning device, to efficiently solve
The broken problem of the volume expansion of silicon carbon material and silicon carbide particles, while the later period for effectively reducing SEI film lives again phenomenon, benefit
The mechanical strength of negative electrode material is effectively increased with nanofibrous structures, can electrospinning device low efficiency, consistency difference asks
Topic is so that the silicon based anode material that this mode of nanofiber produces is difficult to realize industrial volume production.This patent targetedly proposes
Preparation process is simple, and volume production converts easy production technology and artificial graphite, SiO base silicon-carbon composite cathode material have Gao Rong
Amount, high magnification, the negative electrode material of high conductivity.
Summary of the invention
The purpose of the present invention is to provide the preparation methods of a kind of artificial graphite, SiO base silicon-carbon composite cathode material, with solution
Certainly above-mentioned technical problem.
The present invention using following technical scheme in order to solve the above technical problems, realized:
A kind of preparation method of artificial graphite, SiO base silicon-carbon composite cathode material, characterized by the following steps:
(1) crystal silicon powder or polysilicon block are taken and quartz pushrod is the raw material for preparing SiO, is placed in crucible, with quartz pushrod and crucible
Interior polycrystalline silicon melt keeps the continuous rotating contact of opposite direction, so that quartz pushrod is sufficiently reacted with polycrystalline silicon melt, in molten
Reaction generates SiO steam under state；
(2) mixed gas of SiO steam and argon gas is passed through water-cooled deposition device, carries out cooling deposition；
(3) SiO powder is formed after the water cooled precipitation equipment of the mixed gas of SiO steam and argon gas is cooling, is deposited to sediment box four
It is separated on all outer walls, it is spare to collect SiO powder；
(4) ready graphite, pitch are sucked into VC mixing machine by vacuum lead, mixed slowly 5 minutes, guarantee two kinds of material
Shut down after effectively mixing；
(5) SiO obtained in step (3) and special additive are sucked in VC mixing machine by vacuum lead and is stirred, SiO,
This two kinds of materials of special additive point two investment VC mixing machines, when graphite and SiO basically form uniform particle, then
Discharging；Divide two investments so that the SiO and special additive entered later can be uniform under the drive that central blade rotates
It is adhered to the artificial graphite surface layer uniformly wrapped up by pitch；
(6) artificial graphite being stirred, SiO base silicon-carbon composite cathode material presoma change cladding furnace high temperature are coated.
Preferably, the artificial graphite, pitch, SiO, special additive mass ratio be artificial graphite: pitch:
SiO: special additive=300 ~ 350Kg:15 ~ 25Kg:30 ~ 50Kg:1 ~ 5Kg.
Preferably, the special additive is carbon nanotube, and monodimension nanometer material is light-weight, and hexagonal structure has connected
Beauty has many abnormal mechanics, electricity and chemical property.
Preferably, the artificial graphite is glad from artificial graphite KAG-1S processed, and the SiO particle size range is 5 ~ 25um.
Preferably, the artificial graphite structure is spherical layer structure, and there are a fixed gaps between layers.
Preferably, the VC mixing machine mixing time in the step (5) is 30min.
Preferably, the temperature of the cladding furnace in the step (6) is 680 DEG C.Purpose is will be artificial during stirring
The pitch that adhesive is served as between graphite and SiO carries out carbon, carries out in VC mixing machine after asphalt carbonization is complete cold
But, this method can allow internal artificial graphite, SiO base silicon-carbon composite cathode material structure to be formed, to realize this technique pair
The microstructure establishment of artificial graphite, SiO base silicon-carbon composite cathode material.
The beneficial effects of the present invention are:
The present invention can effectively solve lithium ion battery by the use of artificial graphite, SiO base silicon-carbon composite cathode material and fill
Volume expansion in discharge process, while improving the energy density of negative electrode material, and possess good cycle performance, forthright again
Energy；Artificial plumbago negative pole material and SiO pass through pitch combined this structure well, can use asphalt carbonization
Process improves the amalgamation of the two, further increases the structural stability of this negative electrode material, entire invented technology process is simple, people
Make graphite, SiO base silicon-carbon composite cathode material has been shown well in lithium ion battery negative material and battery performance test
Physical property and chemical property, the gram volume of material effectively improve, full battery test in show preferably to follow
Ring performance and its higher energy density.
Detailed description of the invention
The SEM figure of artificial graphite, SiO base silicon-carbon composite cathode material that Fig. 1 produces for the present invention；
Fig. 2 is the microstructure schematic diagram of graphite of the invention；
Fig. 3 is that graphite pitch of the invention coats microcosmic sectional view；
Fig. 4 is the microcosmic sectional view of pitch-coating of the invention；
Fig. 5 is that SiO base of the invention coats microcosmic sectional view；
Appended drawing reference: 1- artificial graphite；2- pitch；3-SiO.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained, and however, the following embodiments are merely preferred embodiments of the present invention, and not all.
Based on the implementation example in the implementation mode, those skilled in the art's obtained other realities without making creative work
Example is applied, protection scope of the present invention is belonged to.Experimental method in following embodiments is unless otherwise specified conventional method,
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
(1) crystal silicon powder or polysilicon block are taken and quartz pushrod is the raw material for preparing SiO3, is placed in crucible, makes quartz pushrod and crucible
Interior polycrystalline silicon melt keeps the continuous rotating contact of opposite direction, so that quartz pushrod is sufficiently reacted with polycrystalline silicon melt, in molten
Reaction generates SiO steam under state；
(2) mixed gas of SiO steam and argon gas is passed through water-cooled deposition device, carries out cooling deposition；
(3) SiO3 powder is formed after the water cooled precipitation equipment of the mixed gas of SiO steam and argon gas is cooling, is deposited to sediment box four
It is separated on all outer walls, it is spare to collect SiO3 powder；
(4) artificial graphite 1 takes 315Kg, pitch 2 to take 28Kg, sucks VC mixing machine by vacuum lead, mixes slowly 5 minutes,
Guarantee that two kinds of material shut down after effectively mixing；As in Figure 2-4；
(5) take SiO3 obtained in step (3) that 50Kg and special additive 2Kg is taken to suck in VC mixing machine by vacuum lead
Quickly stirring, two investment VC mixing machines of this two kinds of materials of SiO3, special additive point, when artificial graphite 1 and SiO3 fundamental form
At uniform particle, then discharge；As shown in Fig. 5 and Fig. 1.
(6) artificial graphite 1 being stirred, SiO base silicon-carbon composite cathode material presoma change cladding furnace high temperature are carried out
Cladding.
Embodiment 2
(1) crystal silicon powder or polysilicon block are taken and quartz pushrod is the raw material for preparing SiO3, is placed in crucible, makes quartz pushrod and crucible
Interior polycrystalline silicon melt keeps the continuous rotating contact of opposite direction, so that quartz pushrod is sufficiently reacted with polycrystalline silicon melt, in molten
Reaction generates SiO steam under state；
(2) mixed gas of SiO steam and argon gas is passed through water-cooled deposition device, carries out cooling deposition；
(3) SiO3 powder is formed after the water cooled precipitation equipment of the mixed gas of SiO steam and argon gas is cooling, is deposited to sediment box four
It is separated on all outer walls, it is spare to collect SiO3 powder；
(4) it takes that artificial graphite 1 is 320Kg, pitch 2 is 25Kg, VC mixing machine is sucked by vacuum lead, mixes slowly 5 points
Clock guarantees that two kinds of material shut down after effectively mixing；As in Figure 2-4；
(5) taking SiO3 obtained in step (3) is that 48Kg and special additive 2Kg is sucked in VC mixing machine by vacuum lead
Quickly stirring, two investment VC mixing machines of this two kinds of materials of SiO3, special additive point, when artificial graphite 1 and SiO3 fundamental form
At uniform particle, then discharge；As shown in Fig. 5 and Fig. 1；
(6) artificial graphite 1 being stirred, SiO base silicon-carbon composite cathode material presoma change cladding furnace high temperature are coated.
Embodiment 3
(1) crystal silicon powder or polysilicon block are taken and quartz pushrod is the raw material for preparing SiO3, is placed in crucible, makes quartz pushrod and crucible
Interior polycrystalline silicon melt keeps the continuous rotating contact of opposite direction, so that quartz pushrod is sufficiently reacted with polycrystalline silicon melt, in molten
Reaction generates SiO steam under state；
(2) mixed gas of SiO steam and argon gas is passed through water-cooled deposition device, carries out cooling deposition；
(3) SiO3 powder is formed after the water cooled precipitation equipment of the mixed gas of SiO steam and argon gas is cooling, is deposited to sediment box four
It is separated on all outer walls, it is spare to collect SiO3 powder；
(4) it takes that artificial graphite 1 is 330Kg, pitch 2 is 20Kg, VC mixing machine is sucked by vacuum lead, mixes slowly 5 points
Clock guarantees that two kinds of material shut down after effectively mixing；As in Figure 2-4；
(5) taking SiO3 obtained in step (3) is that 43Kg and special additive 2Kg is sucked in VC mixing machine by vacuum lead
Quickly stirring, two investment VC mixing machines of this two kinds of materials of SiO3, special additive point, when artificial graphite 1 and SiO3 fundamental form
At uniform particle, then discharge；As shown in Fig. 5 and Fig. 1；
(6) artificial graphite 1 being stirred, SiO base silicon-carbon composite cathode material presoma change cladding furnace high temperature are coated.
Product test
(1) electrical testing is detained
The sum of artificial graphite, SiO base silicon-carbon composite cathode material is made referring to domestic certain lithium-ion electric for Examples 1 to 3
Pond silicon-carbon cathode material is fabricated to button cell respectively and carries out data comparison, respectively that glad source artificial graphite, SiO base silicon-carbon is compound
Cathode material SiO500-1, SiO500-2, SiO500-3 and CSi-1；Button cell the preparation method comprises the following steps:
Cathode slurrying: respectively with glad source artificial graphite, SiO base silicon-carbon composite cathode material SiO500-1, SiO500-2,
Conductive agent SP, CMC and SBR and H20 are added in SiO500-3 and CSi-1, are stirred homogenate, configured slurry is through Shenzhen section
Brilliant MSK-AFA-III lab coater is coated, and is made by drying and the crystalline substance twin rollers MSK-2150 tabletting of Shenzhen section
Cathode pole piece.Binder used is section's crystalline substance conventional binders CMC, and conductive agent SP, specific ratio is 94g:2g:4g:200ml；Electricity
The electrolyte that liquid is configured with Xin Zhou nation according to artificial graphite, SiO base silicon-carbon composite cathode material is solved, to 0.25 thick lithium of electrode
Piece, diaphragm use polyethylene (PE), polypropylene (PP) or ceramic composite membrane, button cell in the glove box that argon gas is protected into
Row, carries out electrochemical property test on Blue.G 5v/10mA type cell tester, charging/discharging voltage range be 0.005V extremely
2.0V, charge-discharge velocity 0.05C.
1 Examples 1 to 3 of table and comparative example buckle electrical test results
| Button cell | SiO500-1 | SiO500-2 | SiO500-3 | CSi-1 |
| Negative electrode material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Discharge capacity (mAh/g) for the first time | 502.4 | 510.1 | 504.7 | 482.9 |
| First charge discharge efficiency (%) | 89.1 | 90.8 | 89.3 | 88.7 |
It is obtained by the analysis of 1 data of table, the glad source artificial graphite of Examples 1 to 3, SiO base silicon-carbon composite cathode material are being fabricated to button
Parameter after battery is better than the parameter of silicon carbon material in comparative example, and glad source artificial graphite, SiO base silicon-carbon are compound in example 2
The discharge capacity for the first time and first charge discharge efficiency of negative electrode material are more better than electrical parameter performance in comparative example.The experimental results showed that this hair
The negative electrode material electrical parameter superior performance of the glad source artificial graphite, SiO base silicon-carbon composite cathode material that are proposed in bright patent.It is artificial
The gram volume and first effect of graphite, SiO base silicon-carbon composite cathode material in method 2 are all well and good, so we determined that technique is
Formula in second example.
(2) soft-package battery is tested
Artificial graphite, SiO base silicon-carbon composite cathode material and domestic certain silicon-carbon cathode material are made with Examples 1 to 3 respectively
As negative electrode material, with ternary lithium (NCA) for positive electrode, using Xin Zhou nation according to artificial graphite, SiO base silicon-carbon composite cathode
The electrolyte of material configuration, XY-NAMI-PE composite membrane are diaphragm, assemble 80mAh soft-package battery XY-1, XY-2, XY-3, XX-1,
And the chemical property of its soft-package battery is tested under identical conditions.
Soft-package battery electrochemical property test is as shown in table 2.
The glad source difference negative electrode material of table 2 recycles comparison sheet with comparison negative electrode material
It is obtained from the analysis of table 2, the Soft Roll made of glad source artificial graphite, SiO base silicon-carbon composite cathode material Examples 1 to 3
Capacity and capacity retention ratio of the battery after 500 circulations are above the silicon-carbon cathode material in comparative example, in glad source artificial stone
The rate of decay of capacity and the overall attenuation rate of capacity are all superior in ink, the cyclic process in 500 weeks of SiO base silicon-carbon composite cathode material
With the soft-package battery of the silicon-carbon cathode material production in comparative example.The experimental results showed that using artificial graphite of the invention, SiO
Soft-package battery made from base silicon-carbon composite cathode material has good cycle performance and capacity to keep again.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
For personnel it should be appreciated that the present invention is not limited to the above embodiments, described in the above embodiment and specification is only the present invention
Preference, be not intended to limit the invention, without departing from the spirit and scope of the present invention, the present invention also has various
Changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by institute
Attached claims and its equivalent thereof.
Claims (7)
1. the preparation method of a kind of artificial graphite, SiO base silicon-carbon composite cathode material, characterized by the following steps:
(1) crystal silicon powder or polysilicon block are taken and quartz pushrod is the raw material for preparing SiO, is placed in crucible, with quartz pushrod and crucible
Interior polycrystalline silicon melt keeps the continuous rotating contact of opposite direction, so that quartz pushrod is sufficiently reacted with polycrystalline silicon melt, in molten
Reaction generates SiO steam under state；
(2) mixed gas of SiO steam and argon gas is passed through water-cooled deposition device, carries out cooling deposition；
(3) SiO powder is formed after the water cooled precipitation equipment of the mixed gas of SiO steam and argon gas is cooling, is deposited to sediment box four
It is separated on all outer walls, it is spare to collect SiO powder；
(4) ready artificial graphite, pitch are sucked into VC mixing machine by vacuum lead, mixes slowly 5 minutes, guarantees two
Kind material is shut down after being thoroughly mixed；
(5) SiO obtained in step (3) and special additive are sucked in VC mixing machine by vacuum lead and are quickly stirred,
Both materials of SiO, special additive put into VC mixing machine in two times, when graphite and SiO basically form particle of uniform size,
Then it discharges；
(6) artificial graphite being stirred, SiO base silicon-carbon composite cathode material presoma change cladding furnace high temperature are coated.
2. the preparation method of a kind of artificial graphite according to claim 1, SiO base silicon-carbon composite cathode material, feature
Be: the artificial graphite, pitch, SiO, special additive mass ratio be artificial graphite: pitch: SiO: special additive
=300 ~ 350Kg:15 ~ 25Kg:30 ~ 50Kg:1 ~ 5Kg.
3. the preparation method of a kind of artificial graphite according to claim 1, SiO base silicon-carbon composite cathode material, feature
Be: the special additive is carbon nanotube, is monodimension nanometer material, light-weight, and hexagonal structure connection is perfect, has and is permitted
The normal mechanics of polyisocyanate, electricity and chemical property.
4. the preparation method of a kind of artificial graphite according to claim 1, SiO base silicon-carbon composite cathode material, feature
Be: the artificial graphite is glad from artificial graphite KAG-1S processed, and the SiO particle size range is 5 ~ 25um.
5. the preparation method of a kind of artificial graphite according to claim 1, SiO base silicon-carbon composite cathode material, feature
Be: the artificial graphite structure is spherical layer structure, and there are gaps between layers.
6. the preparation method of a kind of artificial graphite according to claim 1, SiO base silicon-carbon composite cathode material, feature
Be: the VC mixing machine mixing time in the step (5) is 30min.
7. the preparation method of a kind of artificial graphite according to claim 1, SiO base silicon-carbon composite cathode material, feature
Be: the internal temperature of the cladding furnace in the step (6) is 680 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114361416A (en) * | 2021-12-29 | 2022-04-15 | 宁波杉杉新材料科技有限公司 | Silicon-based composite material, lithium ion battery and preparation method and application thereof |
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| CN102403491A (en) * | 2011-11-30 | 2012-04-04 | 奇瑞汽车股份有限公司 | Silicon carbon composite anode material of lithium-ion battery, method for preparing silicon carbon composite anode material, and lithium-ion battery |
| CN102769139A (en) * | 2012-08-10 | 2012-11-07 | 深圳市斯诺实业发展有限公司永丰县分公司 | Preparation method of high power capacity lithium ion battery cathode material |
| CN105576209A (en) * | 2016-02-04 | 2016-05-11 | 中南大学 | High-capacity silicon-based anode material for lithium ion battery and preparation method thereof, and lithium ion battery |
| CN107640774A (en) * | 2017-10-27 | 2018-01-30 | 北方民族大学 | A kind of method for preparing SiO powder |
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| CN102403491A (en) * | 2011-11-30 | 2012-04-04 | 奇瑞汽车股份有限公司 | Silicon carbon composite anode material of lithium-ion battery, method for preparing silicon carbon composite anode material, and lithium-ion battery |
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| CN107640774A (en) * | 2017-10-27 | 2018-01-30 | 北方民族大学 | A kind of method for preparing SiO powder |
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| CN114361416A (en) * | 2021-12-29 | 2022-04-15 | 宁波杉杉新材料科技有限公司 | Silicon-based composite material, lithium ion battery and preparation method and application thereof |
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