CN109167046A - Silicon carbide particles for cathode of lithium battery - Google Patents
Silicon carbide particles for cathode of lithium battery Download PDFInfo
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- CN109167046A CN109167046A CN201811064374.4A CN201811064374A CN109167046A CN 109167046 A CN109167046 A CN 109167046A CN 201811064374 A CN201811064374 A CN 201811064374A CN 109167046 A CN109167046 A CN 109167046A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
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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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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses the silicon carbide particles for cathode of lithium battery, belong to silicon materials preparation technical field；Including spherical carbon particle and spherical silicon particle, the partial size ratio of silicon particle and carbon particle is 0.6-1:4-6, and the surface layer of carbon particle is connected with multiple silicon particles；Wherein, spherical silicon particle includes spherical elemental silicon inner core, and spherical elemental silicon core surface wraps up silica outer layer, aoxidizes perforation on outer silicon and multiple holes are distributed with；Silicon particle structure of the invention, be conducive to be thoroughly mixed to form chondritic with graphite, be conducive to alleviate the bulk effect of silicon, the spherical package structure formed with carbon particle keeps the combination of silicon particle and carbon particle more stable, electrode material is in charge and discharge process, the silicon carbide particles of formation are not pulverized easily on a current collector to be peeled off from collector, is not easy to form new solid-phase electrolyte layer, is improved the chemical property of lithium battery.
Description
Technical field
The invention belongs to silicon materials preparation technical fields, and in particular to the silicon carbide particles for cathode of lithium battery.
Background technique
Lithium ion battery is most widely used energy storage battery core in current energy storage technology, and improving battery core energy storage density is
The target that the whole world is pursued, the raising of battery core energy density depend on the progress of its positive and negative electrode material.
People generally use negative electrode material of the carbon based negative electrodes material as lithium ion battery, but carbon based negative electrodes material energy is close
Spend low (theoretical specific capacity 372mAh/g, practical reversible specific capacity are 330mAh/g).Silicon is to be currently known specific capacity (theoretical specific volume
Measure 4200mAh/g) highest lithium ion battery negative material, but due to its huge bulk effect (> 300%), silicon electrode material
Dusting is understood in charge and discharge process and is peeled off from collector, so that active material and active material, active material and collector
Between lose electrical contact, while constantly forming new solid-phase electrolyte layer SEI, eventually lead to the deterioration of chemical property.
The material of crystalline silicon slice about 40% becomes powder by Buddha's warrior attendant wire cutting and is lost, by taking polycrystalline silicon rod as an example, 2018
About 105 yuan of August part per kilogram, upper half annual output about 50GW in 2018, about 200,000 tons of crystal bar is converted into, slice is lost 40%, converts into 10
Ten thousand tons, and the powder diameter is too small (particle diameter distribution 200nm ~ 2.5um), and conventional method can not be handled, and be formed to environmental protection
Biggish pressure.
Summary of the invention
Overcome the deficiencies in the prior art of the present invention, waste material can not recycle benefit after solving photovoltaic industry crystalline silicon diamond wire slice
With the problem of, provide it is a kind of using Buddha's warrior attendant wire cutting waste silicon powder prepare the silicon carbide particles for cathode of lithium battery, can solve because
The phenomenon that silicium cathode structure caused by silicium cathode embedding and removing collapses, dusting.
To achieve the above object, the technical scheme adopted by the invention is as follows: using Buddha's warrior attendant wire cutting waste silicon powder prepare lithium electricity
The method of pond negative electrode material, comprising the following steps:
A) by Buddha's warrior attendant wire cutting waste silicon powder using the hydrochloric acid of 0.1 ~ 0.5mol/L, the sulfuric acid that mass fraction is 30% ~ 50%, 20% ~
The mixed solution of 45% nitric acid impregnates 3 ~ 6h；It rinses later and dry.
B) under inert gas protection, the Buddha's warrior attendant wire cutting waste silicon powder after drying is small in 180 ~ 260 DEG C of high-temperature calcinations 2 ~ 5
When；The hydrofluoric acid dips of 0.03 ~ 0.08mol/L, and 30 ~ 100min of magnetic agitation are reused, the modified silicon powder A in surface is obtained.
C) silicon powder A modified to surface carries out partial size consistency treatment using the method for wet grinding and obtains consistency silicon powder B,
The consistency silicon powder B partial size is 30 ~ 50nm of D95 partial size, and D20 partial size < 10nm.
D) the sorting silicon powder C that partial size is 30 ~ 50nm is sub-elected from the consistency silicon powder B, by the sorting silicon
After powder C carries out carbonization treatment, lithium battery silicon carbon anode material is obtained.
Preferably, impurity remaining in Buddha's warrior attendant wire cutting waste silicon powder is first removed before the step a).
Preferably, the hydrochloric acid, sulfuric acid, nitric acid volume ratio are 1-2.5:0.8-1.5:1.
Preferably, which is characterized in that hydrochloric acid, sulfuric acid, nitric acid mixed solution temperature be 40-80 DEG C.
Preferably, the magnetic agitation of the step b) is superimposed forced vibration, and forms forced convection, and forced vibration includes
Any one of ultrasound, mechanical stirring, reactor shaking, electric and magnetic oscillation.
The partial size consistency treatment be by the modified silicon powder A in the surface according to the every increase 100-200nm of partial size into
Row stepping forms the modified silicon powder in surface of different-grain diameter rank, and mixed liquor H is added in the modified silicon powder in the surface of each rank, is carried out
It includes dispersing agent, surfactant, addition that dry mixed, which obtains consistency the silicon powder B, the mixed liquor H, after grinding
Agent, the additive are diethanol amine or triethanolamine.
Preferably, the surfactant is SDBS, and the dispersing agent is polyethylene glycol 200.
Preferably, 30 ~ 60wt% of dispersing agent, 5 ~ 20wt% of surfactant, 5 ~ 20wt% of additive.
Preferably, the temperature of the mixed liquor H is 60-90 DEG C, pH 7-9.
Preferably, which is characterized in that in the process of lapping, using 0.2 ~ 0.6mm zirconium oxide or corundum it is spherical
Or ellipticity abrasive media, milling apparatus stir 8 ~ 12m/s of axial velocity, milling time 2 ~ 8 hours.
Particle unit in the modified silicon powder A in the surface being prepared by the above method is spherical or laminated structure, described
Spherical or laminated structure there is elemental silicon inner core, the elemental silicon inner core of the chondritic is wrapped with oxidation outer silicon,
The elemental silicon inner core upper and lower surface of the laminated structure has oxidation outer silicon, and perforation distribution is more on the oxidation outer silicon
A hole.
Preferably, multiple holes are evenly distributed on oxidation outer silicon.
The graphite material for meeting cathode of lithium battery is chosen, by grinding, sorting, the partial size of the graphite material is adjusted
Extremely: D95 partial size 200 ~ 300nm, D10 partial size < 200nm obtains graphite D.
The sorting silicon powder C into after carbonization treatment excessively is mixed with graphite D by weight 0.8-1.2:1.
Conductive agent, binder are added in sorting silicon powder C and graphite D mixture, and sufficiently stirs evenly, reaches sorting silicon powder C
It is uniformly mixed with graphite D；Uniform intermixture is applied to copper foil again, through oversintering, is prepared into cathode.
After mixing, since the partial size of graphite D is greater than the partial size of sorting silicon powder C, there is spherical sorting silicon powder C particle
It is wrapped in the outer surface of graphite D particle.When the partial size of the graphite material D: D95 partial size 30 ~ 50nm, D10 partial size <
30nm.At this time since the partial size of the partial size of graphite D and sorting silicon powder C is close, graphite D particle and the sorting silicon with chondritic
The particle of powder C is interlaced to form uniform mixture.
By above method, the silicon carbide particles structure of the present invention for cathode of lithium battery is formd, it is described
Silicon carbide particles structure includes spherical carbon particle and spherical silicon particle, and the silicon particle and the partial size ratio of the carbon particle are
0.6-1:4-6, the surface layer of the carbon particle are connected with multiple silicon particles；Wherein, the spherical silicon particle packet
Include spherical elemental silicon inner core, the spherical elemental silicon core surface wraps up silica outer layer, on the oxidation outer silicon
Multiple holes are distributed in perforation.
Further, the partial size of the silicon particle is 30-50nm, and the partial size of the carbon particle is 200-300nm.
Further, the radius ratio of the elemental silicon inner core and the oxidation outer silicon is 1:1.2-1.5.
Further, multiple holes are uniformly distributed in the oxidation outer silicon.
Further, multiple silicon particles are evenly distributed on the surface of the carbon particle, and by the carbon particle
Package.
Further, the silicon carbide particles include spherical carbon particle and spherical silicon particle, the silicon particle with
The partial size ratio of the carbon particle is 1:1, and the carbon particle is connect with the silicon particle in horizontal and vertical space-alternating.
Further, the carbon particle and the granularity of silicon particle are 30-50nm.
Compared with prior art the invention has the following advantages:
The present invention is using chemical attack combination high-temperature calcination, the method for strong stirring, to the silicon materials in diamond wire cutting waste liquor
Surface is modified processing, forms special silicon particle structure, and inner core is elemental silicon, outer layer covers silica, and is formed and passed through
Multiple holes of oxidation outer silicon are worn, these holes formed are on the one hand by internal layer elemental silicon partial denudation, another aspect surface
This structure package oxide layer its unique axial direction for being conducive to be thoroughly mixed to form chondritic with graphite, and being prepared into
On thickness, be very beneficial for alleviate silicon bulk effect.In addition, lesser specific surface area also effectively reduces silicon materials and electrolysis
Side reaction between liquid.
The spherical package structure and silicon-carbon two kinds of particles formed with carbon particle, which is connected with each other structure, makes silicon particle and carbon
The combination of grain is more stable, and in charge and discharge process, the silicon carbide particles of formation are not pulverized easily on a current collector from collection electrode material
It is peeled off on fluid, carbon particle and the silicon particle combination of inner and outside and package keep two kinds of electrical contacts between particle and collector more stable,
It is not easy to form new solid-phase electrolyte layer, improves the chemical property of lithium battery.
By being recycled, being purified to the silicon materials in crystalline silicon diamond wire cutting waste liquor, surface is modified, consistency treatment
Etc. the obtained this silicon carbide particles of technical process can be used for preparing lithium battery silicon based anode material, meet lithium battery silicon-carbon cathode
Requirement, realize the recycling of diamond wire cutting waste material, and realize huge economic benefit.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the modified silicon particle in surface of chondritic.
Fig. 2 is the sectional view of the modified silicon particle in surface of chondritic.
Fig. 3 is the silicon carbide particles structural schematic diagram in embodiment 1.
Fig. 4 is the silicon carbide particles structural schematic diagram in embodiment 3.
Wherein, 1 is elemental silicon inner core, and 2 be oxidation outer silicon, and 3 be hole, and 4 be carbon particle, and 5 be silicon particle.
Specific embodiment
Below with reference to the examples and drawings technical solution that the present invention will be described in detail, but the scope of protection is not limited by this.
Embodiment 1
The method for preparing lithium cell cathode material using Buddha's warrior attendant wire cutting waste silicon powder, comprising the following steps:
1) by the crystalline silicon Buddha's warrior attendant wire cutting waste silicon powder being collected into remove remaining metal in crystalline silicon Buddha's warrior attendant wire cutting waste silicon powder,
The impurity such as polyethylene glycol, glue, glass.
2) configure mixed solution: using the hydrochloric acid of 0.3mol/L, mass fraction be 40% sulfuric acid, 45% nitric acid is configured to
Mixed solution, wherein hydrochloric acid, sulfuric acid, nitric acid volume ratio are 1:0.8:1；The temperature of mixed solution is 80 DEG C.
3) by Buddha's warrior attendant wire cutting waste silicon powder be placed in mixed solution impregnate 6h and be stirred under vacuum, with remove metallic copper,
Buddha's warrior attendant wire cutting waste silicon powder particle surface is tentatively corroded while iron, nickel plasma, is not less than later using resistivity
10 ~ 15 megaohms of DI water, alcohol mixeding liquid progress 5 ~ 20 times rinsings, and the mode of heating in vacuum is taken to be dried, it heats
120 DEG C of temperature, hold time 6h.
4) under argon gas, helium protective atmosphere, the Buddha's warrior attendant wire cutting waste silicon powder after drying is small in 260 DEG C of high-temperature calcinations 3
When；The hydrofluoric acid dips of 0.05mol/L are reused, and combine magnetic agitation and ultrasonic vibration treatment 100min, surface is obtained and changes
Property silicon powder A.
5) will purifying silicon powder A by partial size carry out stepping, mono- grade of every 100 ~ 200nm, obtain purifying silicon powder A1(300nm ~
400nm), purify silicon powder A2(400nm ~ 600nm), purifying silicon powder A3(600nm ~ 800nm), purifying silicon powder A4(800nm ~
1000nm), purify silicon powder A5(1000nm ~ 1200nm), purifying silicon powder A6(1200nm ~ 1400nm), purifying silicon powder A7(1400nm
~ 1600nm), purifying silicon powder A8(1600nm ~ 1800nm), purifying silicon powder A9(1800nm ~ 2000nm).
6) configuration includes the mixed liquor H of dispersing agent, 20% surfactant, 15% additive that mass percent is 30%；Point
Powder uses polyethylene glycol 400, and surfactant SDBS, additive is diethanol amine；The temperature of mixed liquor H is 60 DEG C, pH
Value is 8.
7) will purifying silicon powder A1-A9 mixed respectively with mixed liquor H, respectively obtain AH1, AH2, AH3, AH4, AH5,
AH6、AH7、AH8、AH9。
8) in such a way that diaphragm is pumped into grinder, will AH9 grind 2h after mix with AH8 after grinding 3h after, then with AH7
After mixed grinding 4h, then with after AH6 mixed grinding 3h, then with after AH5 mixed grinding 4h, then with after AH4 mixed grinding 5h；Again with
After AH3 mixed grinding 5h；Again and after AH2 mixed grinding 4h；AH is obtained with after AH1 mixed grinding 8h again, AH is subjected to solid-liquid point
From obtaining consistency silicon powder B after dry.
9) consistency silicon powder B is sorted, by consistency silicon powder B partial size according to<30nm, 30 ~ 50nm,>50nm third gear
It is sorted and is packed, obtain the sorting silicon powder C1 of partial size<30nm, the sorting silicon powder C2 of 30 ~ 50nm of partial size, partial size>50nm point
Silicon powder C3 is selected, wherein can will sell after sorting silicon powder C1, sorting silicon powder C3 packaging.
10) carbonization treatment is carried out using the method for vapor deposition to sorting silicon powder C2, obtains lithium battery silicon carbon anode material.
By the above method, silicon carbide particles of the present invention have been obtained, as shown in Figure 1-3, for cathode of lithium battery
Silicon carbide particles, including spherical carbon particle 4 and spherical silicon particle 5, the partial size of silicon particle 5 is 30mn, and the partial size of carbon particle 4 is
300nm, the surface layer of carbon particle 4 are connected with several silicon particles 5；Multiple silicon particles 5 wrap up 4 surface of carbon particle.Wherein, spherical
Silicon particle 5 include spherical elemental silicon inner core 1, spherical elemental silicon inner core 1 be coated with oxidation outer silicon 2, aoxidize outer silicon 2
Multiple holes 3 are distributed in upper perforation.The radius ratio of elemental silicon inner core 1 and oxidation outer silicon 2 is 1:1.2.
Embodiment 2
As shown in figure 3, the preparation method of the silicon carbide particles is same as Example 1, for the silicon carbide particles of cathode of lithium battery,
Including spherical carbon particle 4 and spherical silicon particle 5, the partial size of silicon particle 5 is 50mn, and the partial size of carbon particle 4 is 200nm, carbon
The surface layer of particle 4 is connected with several silicon particles 5；Multiple silicon particles 5 wrap up 4 surface of carbon particle.Wherein, spherical silicon particle
5 include spherical elemental silicon inner core 1, and spherical elemental silicon inner core 1 is coated with oxidation outer silicon 2, aoxidizes perforation point on outer silicon 2
It is furnished with multiple holes 3.The radius ratio of elemental silicon inner core 1 and oxidation outer silicon 2 is 1:1.5.
Embodiment 3
As shown in figure 4, the preparation method of the silicon carbide particles is same as Example 1, for the silicon carbide particles of cathode of lithium battery,
Including spherical carbon particle 4 and spherical silicon particle 5, the partial size of silicon particle 5 is 30mn, and the partial size of carbon particle 4 is 30nm, carbon
Grain 4 is connect with silicon particle 5 in horizontal and vertical space-alternating.Wherein, spherical silicon particle 5 includes spherical elemental silicon inner core 1, ball
Shape elemental silicon inner core 1 is coated with oxidation outer silicon 2, aoxidizes perforation on outer silicon 2 and multiple holes 3 are distributed with.In elemental silicon
The radius ratio of core 1 and oxidation outer silicon 2 is 1:1.3.
The above content is combine specific preferred embodiment to the further description done of the present invention, and it cannot be said that
A specific embodiment of the invention is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, is not taking off
Under the premise of from the present invention, several simple deduction or replace can also be made, all shall be regarded as belonging to the present invention by being submitted
Claims determine scope of patent protection.
Claims (7)
1. being used for the silicon carbide particles of cathode of lithium battery, which is characterized in that the silicon particle including spherical carbon particle (4) and spherical shape
(5), the silicon particle (5) and the partial size ratio of the carbon particle (4) are 0.6-1:4-6, and the surface layer of the carbon particle (4) connects
It is connected to multiple silicon particles (5)；Wherein, the spherical silicon particle (5) includes spherical elemental silicon inner core (1), described
Spherical elemental silicon inner core (1) be coated with oxidation outer silicon (2), perforation is distributed with more on the oxidation outer silicon (2)
A hole (3).
2. the silicon carbide particles according to claim 1 for cathode of lithium battery, which is characterized in that the silicon particle (5)
Partial size be 30-50nm, the partial size of the carbon particle (4) is 200-300nm.
3. the silicon carbide particles according to claim 1 for cathode of lithium battery, which is characterized in that the elemental silicon inner core
It (1) is 1:1.2-1.5 with the radius ratio of the oxidation outer silicon (2).
4. the silicon carbide particles according to claim 1 for cathode of lithium battery, which is characterized in that multiple holes
(3) it is uniformly distributed in the oxidation outer silicon (2).
5. the silicon carbide particles according to claim 1 for cathode of lithium battery, which is characterized in that multiple silicon particles
(5) it is evenly distributed on the surface of the carbon particle (4), and the carbon particle (4) is wrapped up.
6. the silicon carbide particles according to claim 1 for cathode of lithium battery, which is characterized in that the silicon carbide particles packet
The silicon particle (5) of spherical carbon particle (4) and spherical shape is included, the silicon particle (5) and the partial size ratio of the carbon particle (4) are 1:
1, the carbon particle (4) is connect with the silicon particle (5) in horizontal and vertical space-alternating.
7. the silicon carbide particles according to claim 6 for cathode of lithium battery, which is characterized in that the carbon particle (4)
Granularity with silicon particle (5) is 30-50nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110885073A (en) * | 2019-12-16 | 2020-03-17 | 河南英能新材料科技有限公司 | Preparation method of carbon nanohorn-silicon composite material |
| CN113991095A (en) * | 2021-12-28 | 2022-01-28 | 安普瑞斯（南京）有限公司 | Negative active material, preparation method thereof, electrode and battery |
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| CN104112850A (en) * | 2014-06-30 | 2014-10-22 | 张力 | Preparation method and application of lithium ion battery negative electrode material based on silicon waste of photovoltaic industry |
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| CN110885073A (en) * | 2019-12-16 | 2020-03-17 | 河南英能新材料科技有限公司 | Preparation method of carbon nanohorn-silicon composite material |
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