CN208722987U - A kind of compound silicon carbide particles for cathode of lithium battery - Google Patents
A kind of compound silicon carbide particles for cathode of lithium battery Download PDFInfo
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- CN208722987U CN208722987U CN201821489678.0U CN201821489678U CN208722987U CN 208722987 U CN208722987 U CN 208722987U CN 201821489678 U CN201821489678 U CN 201821489678U CN 208722987 U CN208722987 U CN 208722987U
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- Y02E60/10—Energy storage using batteries
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Abstract
The utility model discloses a kind of compound silicon carbide particles for cathode of lithium battery, belong to silicon materials preparation technical field；The partial size of silicon particle including spherical carbon particle and sheet, carbon particle is 200-300nm, and the surface layer of carbon particle is connected with the side wall of multiple silicon particles；Silicon particle includes sheet elemental silicon inner core, and sheet elemental silicon inner core upper and lower surface has oxidation outer silicon, aoxidizes perforation on outer silicon and multiple holes are distributed with；The sheet silicon grain structure of the utility model, be conducive to be thoroughly mixed to form branched or network-like structure with graphite, be conducive to alleviate the bulk effect of silicon, the spatial intersecting 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 utility model belongs to silicon materials preparation technical field, and in particular to a kind of compound silicon-carbon for cathode of lithium battery
Particle.
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.
Utility model content
The utility model overcome the deficiencies in the prior art, waste material can not return after solving photovoltaic industry crystalline silicon diamond wire slice
The problem of utilizing is received, a kind of a kind of compound silicon-carbon for cathode of lithium battery prepared using Buddha's warrior attendant wire cutting waste silicon powder is provided
The phenomenon that grain, silicium cathode structure caused by can solving because of silicium cathode embedding and removing collapses, dusting.
To achieve the above object, the technology employed by the present utility model is being prepared using Buddha's warrior attendant wire cutting waste silicon powder
The method of lithium cell cathode 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%,
The mixed solution of 20% ~ 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, the sorting silicon powder C with laminated structure
Particle is incorporated in the surface of graphite D particle with branch-like.
When the partial size of the graphite material D: D95 partial size 30 ~ 50nm, D10 partial size < 30nm.At this time due to graphite D's
The partial size of partial size and sorting silicon powder C are close, when mixing for the sorting silicon powder C with laminated structure with graphite D, are formed to sort
Silicon powder C is network, and graphite D is the structure of network node.
By above method, a kind of compound silicon-carbon for cathode of lithium battery described in the utility model is formd
Grain, the silicon particle including spherical carbon particle and sheet, the partial size of the carbon particle are 200-300nm, the carbon particle
Surface layer be connected with the side wall of multiple silicon particles；The silicon particle includes sheet elemental silicon inner core, the piece
Shape elemental silicon inner core upper and lower surface has oxidation outer silicon, and multiple holes are distributed in perforation on the oxidation outer silicon.
Further, the silicon particle with a thickness of 30 ~ 50nm.
Further, the thickness ratio of the elemental silicon inner core and the oxidation outer silicon is 2-3:1.
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 compound silicon carbide particles include the silicon particle of spherical carbon particle and sheet, the carbon
The partial size of grain is 30-50nm, and the silicon particle of multiple sheets is interconnected on horizontal and vertical space and forms reticular structure,
The silicon particle intersection point interconnected of multiple sheets is tie point, is connected with a carbon particle on the tie point.
Further, the silicon particle with a thickness of 30-50nm.
Compared with prior art the utility model has the following beneficial effects:
The utility model is using chemical attack combination high-temperature calcination, the method for strong stirring, in diamond wire cutting waste liquor
Silicon materials surface be modified processing, form special lamella silicon particle structure, inner core is simple substance silicon wafer layer, upper and lower surface
One layer of silica is covered, and forms multiple holes through oxidation outer silicon, the side of sheet silicon grain exposes elemental silicon inner core,
These holes formed on the one hand from the upper and lower surface of sheet silicon grain by internal layer elemental silicon partial denudation, another aspect surface this
Its uniqueness of the package oxide layer that kind structure is conducive to be thoroughly mixed to form branch-like and network-like structure with graphite, and is prepared into
Laminated structure and axial direction on thickness, be very beneficial for alleviate silicon bulk effect.In addition, lesser specific surface area is also effective
Reduce the side reaction between silicon materials and electrolyte.
The branched package structure and network-like structure formed with carbon particle keeps the combination of silicon particle and carbon particle more steady
Fixed, carbon particle is firmly incorporated on the tie point of silicon particle, and overall structure is not easy to be destroyed, and electrode material is in charge and discharge process
In, the silicon carbide particles of formation are not pulverized easily on a current collector to be peeled off from collector, carbon particle and silicon particle it is network-like with point
Dendritic morphology makes the two kinds of particles combination of inner and outside and package, keeps two kinds of electrical contacts between particle and collector more stable, is not easy shape
The solid-phase electrolyte layer of Cheng Xin；Improve 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 compound silicon carbide particles of technical process can be used for preparing lithium battery silicon based anode material, meet lithium battery silicon-carbon
To the requirement of silicon materials in cathode, the recycling of diamond wire cutting waste material is realized, and realize huge economic benefit.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of sheet silicon grain.
Fig. 2 is the compound silicon carbide particles branch structure schematic diagram in embodiment 1.
Fig. 3 is the compound silicon carbide particles network-like structure 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
The technical solution of the utility model is described in detail below with reference to examples and drawings, but protection scope is not limited by this
System.
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) the crystalline silicon Buddha's warrior attendant wire cutting waste silicon powder being collected into is removed remaining in crystalline silicon Buddha's warrior attendant wire cutting waste silicon powder
The impurity such as metal, 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, compound silicon carbide particles described in the utility model have been obtained, as shown in Figs. 1-2, including spherical shape
Carbon particle 4 and sheet silicon particle 5, the partial size of carbon particle 4 is 200nm, silicon particle 5 with a thickness of 30nm, the table of carbon particle 4
Layer is connected with the side wall of multiple silicon particles 5；Silicon particle 5 includes sheet elemental silicon inner core 1, following table on sheet elemental silicon inner core 1
Mask silica outer layer 2 aoxidizes perforation on outer silicon 2 and multiple holes 3 is distributed with.Multiple holes 3 are uniformly distributed in silica
Outer layer 2.The thickness ratio of elemental silicon inner core 1 and oxidation outer silicon 2 is 2:1.Multiple silicon particles 5 are evenly distributed on the table of carbon particle 4
Face, and carbon particle 4 is wrapped up, make the outer surface of carbon particle 4 with branched form combination silicon particle 5.
Embodiment 2
The preparation method of the compound silicon carbide particles is same as Example 1, as shown in Figs. 1-2, compound silicon carbide particles packet
Include the silicon particle 5 of spherical carbon particle 4 and sheet, the partial size of carbon particle 4 is 300nm, silicon particle 5 with a thickness of 50nm, carbon
The surface layer of grain 4 is connected with the side wall of multiple silicon particles 5；Silicon particle 5 includes sheet elemental silicon inner core 1, sheet elemental silicon inner core 1
Upper and lower surface has oxidation outer silicon 2, aoxidizes perforation on outer silicon 2 and multiple holes 3 are distributed with.Multiple holes 3 are uniformly distributed in
Aoxidize outer silicon 2.The thickness ratio of elemental silicon inner core 1 and oxidation outer silicon 2 is 3:1.Multiple silicon particles 5 are evenly distributed on carbon particle
4 surface, and carbon particle 4 is wrapped up, make the outer surface of carbon particle 4 with branched form combination silicon particle 5.
Embodiment 3
The preparation method of the compound silicon carbide particles is same as Example 1, as shown in figs. 1 and 3, compound silicon carbide particles packet
Include the silicon particle 5 of spherical carbon particle 4 and sheet, the partial size of carbon particle 4 is 40nm, silicon particle 5 with a thickness of 30nm, multiple
The silicon particle 5 of shape is interconnected on horizontal and vertical space and forms reticular structure, the friendship interconnected of silicon particle 5 of multiple sheets
Point is tie point, is connected with a carbon particle 4 on tie point.Being formed with the silicon particle 5 of sheet is network, inside connection carbon particle 4
Space structure.Silicon particle 5 includes sheet elemental silicon inner core 1, and 1 upper and lower surface of sheet elemental silicon inner core has oxidation outer silicon 2,
Multiple holes 3 are distributed in perforation on oxidation outer silicon 2.Multiple holes 3 are uniformly distributed in oxidation outer silicon 2.Elemental silicon inner core 1 with
The thickness ratio for aoxidizing outer silicon 2 is 3:1.
The above content is the further descriptions done in conjunction with specific preferred embodiment to the utility model, cannot
Assert that specific embodiment of the present utility model is only limitted to this, for the utility model person of an ordinary skill in the technical field
For, under the premise of not departing from the utility model, several simple deduction or replace can also be made, all shall be regarded as belonging to
The utility model determines scope of patent protection by the claims submitted.
Claims (7)
1. a kind of compound silicon carbide particles for cathode of lithium battery, which is characterized in that including spherical carbon particle (4) and sheet
Silicon particle (5), the partial size of the carbon particle (4) are 200-300nm, the surface layer of the carbon particle (4) and multiple described
The side wall of silicon particle (5) is connected；The silicon particle (5) includes sheet elemental silicon inner core (1), in the sheet elemental silicon
Core (1) upper and lower surface has oxidation outer silicon (2), and multiple holes (3) are distributed in perforation on the oxidation outer silicon (2).
2. a kind of compound silicon carbide particles for cathode of lithium battery according to claim 1, which is characterized in that the silicon
Particle (5) with a thickness of 30 ~ 50nm.
3. a kind of compound silicon carbide particles for cathode of lithium battery according to claim 1, which is characterized in that the list
The thickness ratio of matter silicon inner core (1) and the oxidation outer silicon (2) is 2-3:1.
4. a kind of compound silicon carbide particles for cathode of lithium battery according to claim 1, which is characterized in that described is more
A hole (3) is uniformly distributed in the oxidation outer silicon (2).
5. a kind of compound silicon carbide particles for cathode of lithium battery according to claim 1, which is characterized in that described is more
A silicon particle (5) is evenly distributed on the surface of the carbon particle (4), and the carbon particle (4) is wrapped up.
6. a kind of compound silicon carbide particles for cathode of lithium battery according to claim 1, which is characterized in that described answers
The silicon particle (5) that silicon carbide particles include spherical carbon particle (4) and sheet is closed, the partial size of the carbon particle (4) is 30-
50nm, the silicon particle (5) of multiple sheets are interconnected on horizontal and vertical space and form reticular structure, and described is multiple
Silicon particle (5) intersection point interconnected of sheet is tie point, is connected with a carbon particle (4) on the tie point.
7. a kind of compound silicon carbide particles for cathode of lithium battery according to claim 6, which is characterized in that the silicon
Particle (5) with a thickness of 30-50nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109148867A (en) * | 2018-09-12 | 2019-01-04 | 山西中电科新能源技术有限公司 | Compound silicon carbide particles for cathode of lithium battery |
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| CN109148867A (en) * | 2018-09-12 | 2019-01-04 | 山西中电科新能源技术有限公司 | Compound silicon carbide particles for cathode of lithium battery |
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