CN108539173A - A kind of preparation method of graphene coated silicon composite - Google Patents
A kind of preparation method of graphene coated silicon composite Download PDFInfo
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- CN108539173A CN108539173A CN201810360818.2A CN201810360818A CN108539173A CN 108539173 A CN108539173 A CN 108539173A CN 201810360818 A CN201810360818 A CN 201810360818A CN 108539173 A CN108539173 A CN 108539173A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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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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- 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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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a kind of preparation methods of graphene coated silicon composite, include the following steps：Metal magnesium powder, silica flour are uniformly mixed with magnesia powder to obtain mixed powder；Under the conditions of the carbon dioxide gas pressure of 0.5~10MPa, the pyroreaction of mixed powder is induced, black powder is obtained；The black powder it is washed and dry graphene coated silicon composite.The present invention causes magnesium powder and carbon dioxide reaction using magnesium powder and carbon dioxide as reaction system, using helical tungsten filament heating power, and reaction generates magnesia and graphene；Wherein magnesia powder can effectively prevent the graphene generated from reuniting during the reaction as diluent.The reaction of the present invention can be adjusted the silicon carbon ratio of product, prepare graphene coated silicon composite by the ratio of adjusting magnesium powder and silica flour.Reaction short preparation period, technical process is simple, production cost is low.
Description
Technical field
The present invention relates to cell negative electrode material technical fields.More particularly, to a kind of graphene coated silicon composite
Preparation method.
Background technology
Secondary lithium battery because with energy density is big, charge discharge life is long, self-discharge rate is low, it is pollution-free, safety can
By the advantages that, it is considered to be the tool of ideal energy storage and conversion.Currently, lithium ion battery be widely used in it is portable
The fields such as formula electronic equipment, electric vehicle/hybrid vehicle and energy-storage system.In the key of manufacture secondary lithium battery
In material, negative material is current commercialized negative material an important factor for determining lithium ion battery working performance and price
Mainly graphite-like carbon negative pole material, actual capacity have been approached theoretical value (372mAh/g), it is difficult to meet growing
High-energy density demand.Therefore, seek high power capacity, long-life, safe and reliable novel anode material replace the graphite-like carbon negative
Pole is the active demand of lithium ion battery development.
In various novel alloy lithium storage materials, silicon capacity highest can form Li with lithium12Si7、Li13Si4、Li7Si3、
Li15Si4And Li22Si5Equal alloys, theoretical lithium storage content are up to 3600mAh/g, about the 10 of graphite capacity times；Silicon-based anode material
Material also has many advantages, such as that and intercalation potential low with electrolyte reactivity is low (being less than 0.5V).The embedding lithium voltage platform of silicon is slightly above
Graphite, the phenomenon that in charging being difficult to that surface lithium is caused to deposit, security performance is better than graphite-based negative material.In addition, silicon is ground
One of highest element of abundance, derives from a wealth of sources in shell, cheap, and without toxicity, the commercialization of silicium cathode material is answered
With with great advantage.But capacity rapid decay caused by bulk effect of silicon electrode during removal lithium embedded, it is it
The huge obstruction of practicalization.During electrochemical lithium storage, each silicon atom obtains after averagely combining 4.4 lithium ions
Li22Si5Alloy phase causes the volume change of material to can reach 300% or more.Since the machinery that huge bulk effect generates is answered
Power can promote the generation and propagation of electrode surface micro-crack, and active material is made gradually to rupture, fall off from collector, to lose
With the electrical contact of collector, electrode cycle performance is caused to decline rapidly.In addition, since silicon itself is semi-conducting material, intrinsic electricity
Conductance is relatively low, and only 6.7 × 10-4S/cm, therefore conductive agent need to be added to improve the electric conductivity of electrode.
Silicon is close with the chemical property of carbon, and the two can combine closely, if silicon materials and carbon material is multiple by all means
It closes, makes in nano silicon particles even dispersion and carbon material matrix, structure and a large amount of lithium ions in conjunction with possessed by carbon material itself
Channel can, increase the embedded location of lithium ion, then can both have complementary advantages, obtain theoretical capacity it is high, good cycle new one
For graphene coated silicon composite.
Accordingly, it is desirable to provide a kind of preparation method of graphene coated silicon composite, at least solves one of above-mentioned ask
Topic.
Invention content
It is an object of the present invention to provide a kind of preparation methods of graphene coated silicon composite.
In order to achieve the above objectives, the present invention uses following technical proposals：
A kind of preparation method of graphene coated silicon composite, includes the following steps：
Metal magnesium powder, silica flour are uniformly mixed with magnesia powder to obtain mixed powder；
Under the conditions of the carbon dioxide gas pressure of 0.5~10MPa, the pyroreaction of mixed powder is induced, black is obtained
Powder；
The black powder it is washed and dry graphene coated silicon composite.The method of the present invention can be in very great Cheng
Reduce or buffer the bulk effect of silicon on degree, improve the electric conductivity of material, and this method short preparation period, technical process it is simple,
Production cost is low；In addition, confirmed through lot of experiments of the present invention, under the pressure condition of the present invention, material obtained by the reaction
Best performance, hypotony metal magnesium powder can not react completely, and requirement of the hypertonia to equipment can also increase therewith；With pressure
The increase of power, ignition temperature also increase as, and graphene crystallinity increases.Further, in the certain specific embodiment parties of the present invention
In formula, the pressure condition is, for example, 0.5~1MPa, 1~10MPa etc..
Preferably, the mixed powder is placed in air pressure auxiliary combustion synthesis device and carries out pyroreaction.
Preferably, the pyroreaction of mixed powder is induced using helical tungsten filament heating power.
Preferably, the helical tungsten filament is powered to apply to the helical tungsten filamentDirect current.
Preferably, the washing process is to be washed under the conditions of magnetic agitation to black powder using dilute acid soln,
To remove the magnesia powder in black powder.
Preferably, a concentration of 0.1~2M of the dilute acid soln；Wherein, dilute acid soln concentration is too low, then can cause to use
Amount of solution is excessive；Dilute acid soln excessive concentration, then the heat that dilute acid soln and the reaction of MgO powder generate is excessive, can be to the stone of production
Black alkene structure causes secondary defect；In the given dilute acid soln concentration range of the present invention, obtained graphene coated silicon is compound
Material property is optimal.
Preferably, the dilute acid soln is dilute hydrochloric acid, dilute sulfuric acid or dust technology.
Preferably, the drying is freeze-drying, and the freeze-drying is conventional technical means, and condition is preferably drying
- 85 DEG C of temperature, drying time are 5 days.
Preferably, it counts in parts by weight, in the mixed powder, the metal magnesium powder is 10~20 parts, and the silica flour is
10~50 parts, the magnesia powder is 30~80 parts；The present invention can regulate and control production by regulating and controlling the ratio of metal magnesium powder and silica flour
Object carbon silicon ratio adjusts the performance for generating graphene by adjusting the content of magnesia powder；Wherein metal magnesium powder content is too low, nothing
Method is lighted；Content of magnesia is too low, and reaction product is block；In the given formulation weight fraction range of the present invention, obtain
Graphene coated silicon composite best performance.
Preferably, the average grain diameter of the metal magnesium powder is 1~100 μm；Wherein, magnesium powder grain size is excessive, magnesium powder and dioxy
Change the graphene coated of carbon reaction generation on magnesium powder surface, prevents the further progress of reaction, metal magnesium powder can be caused incomplete
Reaction；Magnesium powder grain size is too small, and corresponding cost is consequently increased；In the given metal magnesium powder average particle size range of the present invention,
Obtained graphene coated silicon composite best performance.
Preferably, the average grain diameter of the silica flour is 0.15~1 μm, wherein is used for the silicon-carbon cathode material of lithium ion battery
Material preferentially uses nano silica fume.
Preferably, the average grain diameter of the magnesia powder is 0.05~1 μm, wherein the grain size of magnesia can influence to generate
The specific surface area and crystal property of graphene, magnesia powder grain size is smaller, and the graphene specific surface area of generation is bigger, crystal property
It is poorer；In the average particle size range of the given magnesia powder of the present invention, obtained graphene coated silicon composite performance is most
It is excellent.
The preparation method of the graphene coated silicon composite specifically comprises the following steps：
Metal magnesium powder, silica flour are uniformly mixed with magnesia powder to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to spiral tungsten in the mixed powder
Silk；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas until the air pressure
The pressure of auxiliary combustion synthesis device is 0.5~10MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature initiation reaction, obtains
Black powder；
The black powder obtained after reaction and enough dilute acid solns are mixed, through in magnetic agitation to black powder
Magnesia reacts completely, through filtering and being freeze-dried and obtaining graphene coated silicon composite.
In addition, unless otherwise specified, it is raw materials used in the present invention can be by commercially available commercially available, recorded in the present invention
Any range includes that any number between any numerical value and end value or end value between end value and end value is constituted
Arbitrary subrange.
Beneficial effects of the present invention are as follows：
The present invention causes magnesium powder and titanium dioxide using magnesium powder and carbon dioxide as reaction system, using helical tungsten filament heating power
Carbon reacts, and reaction generates magnesia and graphene；Wherein magnesia powder can be prevented effectively during the reaction as diluent
The graphene of generation is reunited.The reaction of the present invention can adjust the silicon carbon ratio of product by the ratio of adjusting magnesium powder and silica flour, make
Standby graphene coated silicon composite.Reaction short preparation period, technical process is simple, production cost is low.
Description of the drawings
Specific embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the graphene coated silicon composite XRD spectrum of the embodiment of the present invention 1.
Fig. 2 shows the graphene coated silicon composite Raman collection of illustrative plates of the embodiment of the present invention 2.
Fig. 3 shows the graphene coated silicon composite SEM-EDS collection of illustrative plates of the embodiment of the present invention 3.
Specific implementation mode
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.It will be appreciated by those skilled in the art that specifically described content is illustrative and be not restrictive below, it should not be with this
It limits the scope of the invention.
In the present invention, preparation method is then conventional method unless otherwise specified.Raw material used is equal unless otherwise instructed
It can be obtained from disclosed commercial sources.
Embodiment 1
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (20 μm), silica flour (200nm) is mixed with magnesia powder (50nm) according to 10: 10: 80 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 1MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilute hydrochloric acid solution of 1M, magnetic agitation washs and at -85 DEG C
Under the conditions of be freeze-dried 5 days after obtain graphene coated silicon composite.
XRD tests (as shown in Figure 1) are carried out to obtained graphene coated silicon composite, test result shows：Production
If owner is existed by graphene, silicon and silicon carbide composition, no other impurities.
Embodiment 2
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (1 μm), silica flour (150nm) is mixed with magnesia powder (200nm) according to 20: 10: 80 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 0.5MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and two
Carbon dioxide reaction obtains black powder；
The black powder obtained after reaction is placed in the dilute hydrochloric acid solution of 0.1M, magnetic agitation washs and -85
Graphene coated silicon composite is obtained after being freeze-dried 5 days under the conditions of DEG C.
Raman tests (as shown in Figure 2) are carried out to obtained graphene coated silicon composite, test result shows：
The Raman spectrum of product have typical sp2The relevant peaks G (1575cm-1), it is chaotic caused by the peaks D (1336cm-1), the peaks 2D
(2671cm-1) and the peaks D+G (2910cm-1), it is determined that there are a large amount of edges and plane ripples for limited stacking order, further
The generation of graphene is determined.
Embodiment 3
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (100 μm), silica flour (1000nm) and magnesia powder (1000nm) according to 10: 50: 80 mass ratio
It is uniformly mixed to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 10MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilute hydrochloric acid solution of 2M, magnetic agitation washs and at -85 DEG C
Under the conditions of be freeze-dried 5 days after obtain graphene coated silicon composite.
SEM-EDS tests (as shown in Figure 3), test result table are carried out to obtained graphene coated silicon composite
It is bright：Product grain realizes cladding of the carbon on silicon particle.
Embodiment 4
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (20 μm), silica flour (200nm) is mixed with magnesia powder (50nm) according to 20: 50: 80 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 1MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilute nitric acid solution of 1M, magnetic agitation washs and at -85 DEG C
Under the conditions of be freeze-dried 5 days after obtain graphene coated silicon composite.
Embodiment 5
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (20 μm), silica flour (200nm) is mixed with magnesia powder (50nm) according to 10: 50: 30 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 1MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilution heat of sulfuric acid of 1M, magnetic agitation washs and at -85 DEG C
Under the conditions of be freeze-dried 5 days after obtain graphene coated silicon composite.
Embodiment 6
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (20 μm), silica flour (200nm) is mixed with magnesia powder (50nm) according to 20: 50: 30 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 1MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilute nitric acid solution of 0.1M, magnetic agitation washs and -85
Graphene coated silicon composite is obtained after being freeze-dried 5 days under the conditions of DEG C.
Embodiment 7
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (20 μm), silica flour (200nm) is mixed with magnesia powder (50nm) according to 10: 10: 30 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 1MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilute nitric acid solution of 2M, magnetic agitation washs and at -85 DEG C
Under the conditions of be freeze-dried 5 days after obtain graphene coated silicon composite.
Embodiment 8
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (20 μm), silica flour (200nm) is mixed with magnesia powder (50nm) according to 20: 10: 30 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 1MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilution heat of sulfuric acid of 0.1M, magnetic agitation washs and -85
Graphene coated silicon composite is obtained after being freeze-dried 5 days under the conditions of DEG C.
Embodiment 9
The preparation of graphene coated silicon composite, includes the following steps：
By metal magnesium powder (20 μm), silica flour (200nm) is mixed with magnesia powder (50nm) according to 10: 10: 80 mass ratio
It is uniform to obtain mixed powder；
The mixed powder is placed in air pressure auxiliary combustion synthesis device, and is embedded to helical tungsten filament in mixed powder；
The pressure of air pressure auxiliary combustion synthesis device is down to 5 × 10-2Pa is passed through carbon dioxide gas, until the air pressure
The pressure of auxiliary combustion synthesis device is 1MPa；
The helical tungsten filament is appliedDirect current, the helical tungsten filament generates high temperature and causes metal magnesium powder and dioxy
Change carbon reaction, obtains black powder；
The black powder obtained after reaction is placed in the dilution heat of sulfuric acid of 2M, magnetic agitation washs and at -85 DEG C
Under the conditions of be freeze-dried 5 days after obtain graphene coated silicon composite.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene coated silicon composite, which is characterized in that include the following steps：
Metal magnesium powder, silica flour are uniformly mixed with magnesia powder to obtain mixed powder；
Under the conditions of the carbon dioxide gas pressure of 0.5~10MPa, the pyroreaction of mixed powder is induced, black powder is obtained；
The black powder it is washed and dry graphene coated silicon composite.
2. preparation method according to claim 1, which is characterized in that the mixed powder is placed in the synthesis of air pressure auxiliary combustion
Pyroreaction is carried out in equipment.
3. preparation method according to claim 1, which is characterized in that induce mixed powder using helical tungsten filament heating power
Pyroreaction.
4. preparation method according to claim 1, which is characterized in that the washing process is using dilute acid soln, in magnetic
Black powder is washed under power stirring condition.
5. preparation method according to claim 4, which is characterized in that a concentration of 0.1~2M of dilute acid soln.
6. preparation method according to claim 5, which is characterized in that the dilute acid soln be dilute hydrochloric acid, dilute sulfuric acid or
Dust technology.
7. preparation method according to claim 1, which is characterized in that it counts in parts by weight, it is described in the mixed powder
Metal magnesium powder is 10~20 parts, and the silica flour is 10~50 parts, and the magnesia powder is 30~80 parts.
8. preparation method according to claim 1, which is characterized in that the average grain diameter of the metal magnesium powder is 1~100 μ
m。
9. preparation method according to claim 1, which is characterized in that the average grain diameter of the silica flour is 0.15~1 μm.
10. preparation method according to claim 1, which is characterized in that the average grain diameter of the magnesia powder is 0.05~1
μm。
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| CN110518224A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of preparation method of lithium ion battery carbon silicon anode material |
| CN113725409A (en) * | 2021-07-29 | 2021-11-30 | 合肥国轩高科动力能源有限公司 | Silicon-based negative electrode material and preparation method thereof |
| CN114229854A (en) * | 2021-12-17 | 2022-03-25 | 新疆晶硕新材料有限公司 | Preparation method of silicon-oxygen-carbon composite material, negative plate and battery |
| CN114424364A (en) * | 2019-11-01 | 2022-04-29 | 株式会社Lg新能源 | Negative electrode active material, method for preparing same, and negative electrode and secondary battery comprising same |
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