CN110289400A - A kind of dispersing method of nano-silicon - Google Patents
A kind of dispersing method of nano-silicon Download PDFInfo
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- CN110289400A CN110289400A CN201910443514.7A CN201910443514A CN110289400A CN 110289400 A CN110289400 A CN 110289400A CN 201910443514 A CN201910443514 A CN 201910443514A CN 110289400 A CN110289400 A CN 110289400A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- 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
- H01M4/362—Composites
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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
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of dispersing methods of nano-silicon, comprising the following steps: (1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；(2) SILICA FUME is dissolved in polar solvent and stirring is made into the silicon solution of solid content 10%-15%；(3) it takes wet ball grinding technique to carry out ball milling silicon solution, and cetyl trimethylammonium bromide ionic dispersants is added in mechanical milling process, up to nano-silicon powder after ball milling.The present invention in mechanical milling process by being precisely added cetyl trimethylammonium bromide ionic dispersants, effectively improve slurry fluidity, enhance Stability of Slurry, and improve the efficiency of ball milling, so that the nano silica fume pelleting property of preparation is good, grain diameter is uniform, has preferable dispersed structure；The chemical property of the silicon powder of preparation is greatly improved, to can effectively improve the chemical property of silicon electrode material, the specific capacity and coulomb effect of battery is improved, improves the cycle performance of battery.
Description
Technical field
The invention belongs to novel energy resource material technology fields, and in particular to a kind of dispersing method of nano-silicon.
Background technique
In the lithium ion battery negative material system studied at present, metal alloy compositions such as Si, Sn, Al etc. can be with Li
It forms more lithium alloys and there is the theoretical specific capacity more much higher than conventional graphite negative material, meanwhile, the metalloid alloy class material
The removal lithium embedded current potential of material is not likely to produce Li dendrite, security performance compared with conventional graphite negative material height during fast charging and discharging
It is excellent.Wherein, for elemental silicon because it is with highest theoretical specific capacity 4200mAh/g, intercalation potential is 0.2V (vs.Li/Li+),
It has a safety feature, rich reserves, sexual valence is relatively high, has obtained extensive concern and the research of academia and industry, quilt in recent years
It is considered the first choice of next-generation ideal negative electrode material.However silicium cathode material also has certain defect in practical applications, causes
Commercialization process is relatively slow, this is because silicon is a kind of alloy anode, each silicon atom can carry about four lithium atoms, this lithium
Change mechanism due to a large amount of lithium atoms insertion and lead to huge volume change, when being transformed into Li4.4Si from Si, volume expansion is about
Be 420%, the rupture that this big volume expansion/contraction during lithium intercalation/deintercalation causes big stress to will lead to Si and
It crushing, the dusting of active material is peeled off on silicon electrode, cause to lose electrical contact between silicon particle and between particle and collector,
It is even entirely ineffective so as to cause battery capacity sharp-decay.
In order to solve the problems, such as material dusting, researcher proposes to concentrate the distribution of silicon nanosizing prepared sizes, stablize, partial size
Regulatable nano silica-base material can be relieved the Volumetric expansion of silicon, shorten lithium ion diffusion length, and provide good
Electrical contact and electrical conduction, shorten the delivering path of lithium ion, improve the electrochemistry cycle performance of silica-base material, improve following for battery
The ring service life.
To prepare nano-silicon substrate by the way of wet ball grinding, silicon powder particle partial size is deepened constantly not with ball milling
It is disconnected to reduce, silicon powder particle refinement to a certain extent when, specific surface area and specific surface energy gradually increase, intensity and hardness also with
Increase, grain defect reduces, and ball milling difficulty also increases, and particle agglomeration effect also enhances, when these aggregates powder after
Phase processes in use process, since cohesive force is larger, is difficult to open between molecule, is also not easy to be evenly dispersed in organic solvent body
In the processing matrix of system and later period battery pole piece, so that the performance of material is difficult to play desired effect.Therefore, in mechanical milling process
Dispersing agent is added, intergranular interaction can be effectively reduced, reduces subparticle and is adhered to the degree on abrasive media, promote
The flowing of grinding material reduces the energy consumption of ball milling, improves product quality and production efficiency.
Dispersant is various, including the three categories such as cation, anionic, nonionic and mixed type.Dispersing agent is outstanding
It prevents to reunite mutually and having an effect with particle surface in supernatant liquid, the mechanism of action is roughly divided into three kinds: electrostatic repulsion is made
With the effect of, steric hindrance and electrical steric stabilization effect.
Ionic dispersant is electrolysed in water dispersion medium as charged ion or hydrophilic and lipophilic group, is adsorbed in solid
Body particle surface forms an electrically charged protection screen barrier layer, i.e. diffusion electric double layer, and electrostatic repulsion increases, and particle is difficult to happen
Collision is reunited, to play electrostatic stabilization peptizaiton.
Non-ionic polymer such as hyper-dispersant etc., molecular structure include anchoring group and solvent chain two
Point, anchoring group is adsorbed in solid particles surface, and solvent chain is sufficiently extended in medium, forms steric hindrance layer to prevent solid grain
The flocculation of son is reunited, and has the function that steric hindrance.
The molecular weight of high polymer dispersion generally should be difficult to overcome in 103~104 ranges when strand is too short
Densification is played in Van der Waals force, too long easy bridging connection.And polyelectrolyte is electrolysed in water dispersion medium and is adsorbed on particle
Surface, the polymer molecule layer of electrification not only can repel surrounding ions by itself electrically charged electrostatic repulsion effect, but also can
Flick particle mutually using the steric hindrance of solvent chain, to play electrical steric stabilization effect.
All it is the common dispersing agent being added mostly in the mechanical milling process of nano-silicon at present, fails for dispersion solute
Surface nature further screening is made to dispersing agent.
Therefore, it is a kind of suitable to select under the premise of the surface nature for considering decentralized medium comprehensively and locating dicyandiamide solution
Dispersing agent is most important to stable nano-silicon is prepared.
Summary of the invention
The technical problems to be solved by the invention are in view of the above shortcomings of the prior art, to provide a kind of point of nano-silicon
Dissipate method.
The technical scheme adopted by the invention is that: a kind of dispersing method of nano-silicon, comprising the following steps:
(1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；
(2) SILICA FUME is dissolved in polar solvent and stirring is made into the silicon solution of solid content 10%-15%；
(3) it takes wet ball grinding technique to carry out ball milling silicon solution, and cetyl trimethyl is added in mechanical milling process
Ammonium bromide ionic dispersants, up to nano-silicon powder after ball milling.
Preferably, the polar solvent in step (2) uses dehydrated alcohol.
Preferably, the solid content for the silicon solution being made into step (2) is 15%.
Preferably, the ratio of grinding media to material of the wet ball grinding in step (3) is 3:1, media diameters 1mm, rotational speed of ball-mill 1200r/
Min, Ball-milling Time 8h, ball milling temperature are controlled at 26 DEG C -30 DEG C.
Preferably, the additional amount of cetyl trimethylammonium bromide ionic dispersants is silicon solution in the step (3)
The 0.5%-2.5% of total amount.
Preferably, the additional amount of cetyl trimethylammonium bromide ionic dispersants is silicon solution in the step (3)
The 1.5% of total amount.
Nano-silicon powder made from a kind of nano-silicon dispersing method is used for lithium ion battery negative material.
The beneficial effects of the present invention are:
(1) by the way that cetyl trimethylammonium bromide ionic dispersants are added in mechanical milling process, so that the nanometer of preparation
Silicon silicon powder pelleting property is good, and particle is uniform, has preferable dispersed structure；
(2) by accurately controlling additional amount of the cetyl trimethylammonium bromide ionic dispersants in mechanical milling process, from
And the mobility of slurry is effectively improved, the stability of slurry is enhanced, the efficiency of ball milling is effectively increased, reduces silicon powder
The average grain diameter of grain；
(3) by the way that cetyl trimethylammonium bromide ionic dispersants are added, the electricity of the silicon powder of preparation is greatly improved
Chemical property improves the specific capacity and coulomb effect of battery to can effectively improve the chemical property of silicon electrode material, improves
The cycle performance of battery.
Detailed description of the invention
Fig. 1 is the TEM figure of nano-silicon powder prepared by the embodiment of the present invention 1；
Fig. 2 is nano-silicon powder particle after cetyl trimethylammonium bromide ionic dispersants dosage of the present invention and ball milling
The relation schematic diagram of diameter；
Fig. 3 is the TEM figure of the nano-silicon powder of comparative example 1 of the present invention preparation；
Fig. 4 is the TEM figure of the nano-silicon powder of comparative example 2 of the present invention preparation；
Fig. 5 is the TEM figure of the nano-silicon powder of comparative example 3 of the present invention preparation；
Fig. 6 is the TEM figure of the nano-silicon powder of comparative example 4 of the present invention preparation.
Specific embodiment
Invention is further described in detail below in conjunction with the accompanying drawings and the specific embodiments.
Embodiment 1
The dispersing method of nano-silicon provided in this embodiment, comprising the following steps:
(1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；
(2) SILICA FUME is dissolved in dehydrated alcohol, and stirs the silicon solution for being made into solid content 15%；
(3) wet ball grinding technique is taken to carry out ball milling silicon solution, the ratio of grinding media to material of ball milling is 3:1, ball-milling medium diameter
1mm, rotational speed of ball-mill 1200r/min, Ball-milling Time 8h, 28 DEG C of ball milling temperature, and silicon solution total amount is added in mechanical milling process
1.5% cetyl trimethylammonium bromide ionic dispersants, up to nano-silicon powder after ball milling.Measure of nano-silicon powder
Grain partial size is 85nm, and transmission electron microscope picture is as shown in Figure 1.
Embodiment 2
The dispersing method of nano-silicon provided in this embodiment, comprising the following steps:
(1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；
(2) SILICA FUME is dissolved in dehydrated alcohol, and stirs the silicon solution for being made into solid content 15%；
(3) wet ball grinding technique is taken to carry out ball milling silicon solution, the ratio of grinding media to material of ball milling is 3:1, ball-milling medium diameter
1mm, rotational speed of ball-mill 1200r/min, Ball-milling Time 8h, 26 DEG C of ball milling temperature, and silicon solution total amount is added in mechanical milling process
0.5% cetyl trimethylammonium bromide ionic dispersants, up to nano-silicon powder after ball milling.
Embodiment 3
The dispersing method of nano-silicon provided in this embodiment, comprising the following steps:
(1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；
(2) SILICA FUME is dissolved in dehydrated alcohol, and stirs the silicon solution for being made into solid content 15%；
(3) wet ball grinding technique is taken to carry out ball milling silicon solution, the ratio of grinding media to material of ball milling is 3:1, ball-milling medium diameter
1mm, rotational speed of ball-mill 1200r/min, Ball-milling Time 8h, 27 DEG C of ball milling temperature, and silicon solution total amount 1% is added in mechanical milling process
Cetyl trimethylammonium bromide ionic dispersants, up to nano-silicon powder after ball milling.
Embodiment 4
The dispersing method of nano-silicon provided in this embodiment, comprising the following steps:
(1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；
(2) SILICA FUME is dissolved in dehydrated alcohol, and stirs the silicon solution for being made into solid content 15%；
(3) wet ball grinding technique is taken to carry out ball milling silicon solution, the ratio of grinding media to material of ball milling is 3:1, ball-milling medium diameter
1mm, rotational speed of ball-mill 1200r/min, Ball-milling Time 8h, 29 DEG C of ball milling temperature, and silicon solution total amount 2% is added in mechanical milling process
Cetyl trimethylammonium bromide ionic dispersants, up to nano-silicon powder after ball milling.
Embodiment 5
The dispersing method of nano-silicon provided in this embodiment, comprising the following steps:
(1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；
(2) SILICA FUME is dissolved in dehydrated alcohol, and stirs the silicon solution for being made into solid content 15%；
(3) wet ball grinding technique is taken to carry out ball milling silicon solution, the ratio of grinding media to material of ball milling is 3:1, ball-milling medium diameter
1mm, rotational speed of ball-mill 1200r/min, Ball-milling Time 8h, 30 DEG C of ball milling temperature, and silicon solution total amount is added in mechanical milling process
2.5% cetyl trimethylammonium bromide ionic dispersants, up to nano-silicon powder after ball milling.
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, the milling parameters in embodiment 5 are identical, ball therein
Temperature is ground in 28 ± 2 DEG C of the temperature difference range, but the cetyl trimethylammonium bromide ion being added in each embodiment
The additional amount of dispersing agent is different, by obtaining curve graph shown in Fig. 2 to the silicon powder particle grain diameter measurement after the grinding of each embodiment.
As shown in Fig. 2, as the dosage of the cetyl trimethylammonium bromide ionic dispersants of addition increases, nano silica fume grain diameter
Show the trend for first reducing and increasing afterwards.
The effect of cetyl trimethylammonium bromide ionic dispersants is exactly the surface for being adsorbed on particle, is hindered between particle
Mutual absorption, prevent growing up for particle, with the increase of dispersant, coat more and more, dispersing agent is to the quiet of particle
Electricity and steric hindrance effect enhancing, the mobility of slurry are obviously improved and increase particle suspending power, the stability enhancing of slurry,
The average grain diameter of particle is also gradually reduced.
In the 0.5%-1.5% stage with the increase of dispersing agent additional amount, the average grain diameter of silicon powder is strongly reduced；
In the 1.5%-2.5% stage with the increase of dispersion dosage, then in the particle surface wrapped up, there are also surplus for dispersing agent
It is remaining, since the remaining dispersing agent not coated is little to the grain diameter influence of particle, dispersion dosage is continued growing, will be satiated
The case where with absorption, the excessive mutual bridging of dispersant molecule significantly limits the movement of particle at network structure, to make
The mobility of slurry is deteriorated and coagulation occurs, and Stability of Slurry is deteriorated, and grain diameter increases instead.
Minimum value is reached at 1.5%, dispersing agent additional amount reaches critical point, and all particles all coat, reach
Best dispersion effect.
Therefore the additional amount of cetyl trimethylammonium bromide ionic dispersants is optimal additional amount in embodiment 1, can be reached
To best dispersion effect and ball milling effect, embodiment 1 is optimum embodiment.
By research ultrasonic treatment after nano silica fume in high purity water pH-Zeta potential diagram it is known that working as pH=6
When, the absolute value of Zeta potential reaches maximum value.As pH=6, nano silica fume is capable of forming stable colloid, powder in water
Surface is negatively charged.Therefore, optional ionic dispersants increase the negative charge amount of particle surface, increase ξ, electrostatic repulsion increases
Greatly；Or non-ionic dispersing agent is selected to increase steric effect to play the effect of grinding aid, stable dispersion.Therefore we can select
Select triammonium citrate, oleic acid, cetyl trimethylammonium bromide, polyvinyl alcohol, calgon.
Comparative example 1
The present embodiment is substantially the same manner as Example 1, is only to change cetyl trimethylammonium bromide dispersing agent to make lemon
Sour three amine dispersants, the transmission electron microscope picture that nano-silicon is made after ball milling are as shown in Figure 3.Triammonium citrate is as ball milling dispersing agent
When, powder granule is had an effect with polar molecule, and grain spacing reduces, using electrostatic attraction as predominant intermolecular forces between particle, silicon
Powder particles dispersion is uneven, and the crystal grain of finished product is smaller, grows unbalanced.
Comparative example 2
The present embodiment is substantially the same manner as Example 1, is only to change cetyl trimethylammonium bromide dispersing agent to make oleic acid
Dispersing agent, the transmission electron microscope picture that nano-silicon is made after ball milling are as shown in Figure 4.When oleic acid is as ball milling dispersing agent, between powder granule
Away from consolidating that decentralized system electrostatic force is few, and particle is uniformly dispersed, and crystal grain is coarseer in a kind of relatively appropriately distance, liquid, have
A small amount of to reunite, growth is uniform.But oleic acid is that various polarity material mixing forms, and inside has electrostatic repulsion forces of different sizes,
It is capable of forming multi-level electrode potential layer in same volume, is unfavorable for the refinement of powder for a long time.
Comparative example 3
The present embodiment is substantially the same manner as Example 1, is only to change cetyl trimethylammonium bromide dispersing agent to make poly- second
Enol dispersing agent, the transmission electron microscope picture that nano-silicon is made after ball milling are as shown in Figure 5.When polyvinyl alcohol is as ball milling dispersing agent, gather
Hydroxyl on vinyl alcohol is tightly adsorbed in solid particles surface with hydrogen bond formation, has good intermiscibility with ball milling, in medium
In be fully extended to form space bit resistance layer, generate space steric effect between solid particle, particle hindered to roll into a ball because mutually colliding
Poly-, nano-silicon sample light obtained, piece diameter is big, and caking phenomenon is serious；But since single space steric effect more limits to,
It is difficult to overcome electrostatic effect.Therefore, the dispersion stabilization of PVA is not strong.
Comparative example 4
The present embodiment is substantially the same manner as Example 1, is only that cetyl trimethylammonium bromide dispersing agent is changed to work six partially
Sodium phosphate dispersing agent, the transmission electron microscope picture that nano-silicon is made after ball milling are as shown in Figure 6.When calgon is as dispersing agent, six
Sodium metaphosphate belongs to cyclic structure, and the current potential of powder surface can be made to increase, and realizes that generation is stronger by electrostatic stabilization mechanism
Electric double layer electrostatic repulsion forces, to silicon powder system have certain peptizaiton, but steric hindrance act on weaker, electronegative powder
Dispersant molecule of the body granular absorption with faint positive electricity, the nano-silicon sample light prepared, piece diameter is big, and partial size is uneven
One, there are caking phenomenon, particle depolymerization is not thorough, and distribution of particles is uneven.
Cetyl trimethylammonium bromide is chosen in optimum embodiment 1 as dispersing agent, cetyl trimethylammonium bromide
Easily ionizable goes out H+ ion, makes the electronegative silicon powder particle in surface, and particle and dispersing agent interact under the driving of electrostatic effect,
After the particle surface of this electrification has adsorbed the dispersing agent macromolecular of oppositely charged, the dispersant molecule layer of electrification had both passed through this
The electrically charged repulsion neighboring particles of body institute, and because space steric effect prevents the close of particle's Brownian movement, this electrostatic and space
The dual silicon powder system that acts on of steric hindrance generates composite diffusion stabilization.Cetyl trimethylammonium bromide has longer simultaneously
Hydrocarbon chain structure, be easy that winding arrangement occurs on the surface of particle, it is double between particle to form one layer of good protective layer
The repulsive force of electric layer structure and steric hindrance repulsive interaction increase, it is ensured that particle is in permanent suspended state without reuniting, such as
Shown in Fig. 1, individual particle is high-visible in figure, and particle diameter distribution is relatively uniform, does not have obvious agglomeration.This is hexadecane
Base trimethylammonium bromide dispersing agent reduces the surface tension of nano silica fume, and attraction is smaller between particle, to have preferable
Dispersed structure.
Nano silica fume system made from after being dispersed as cetyl trimethylammonium bromide ionic dispersants is at button electricity
Pond and do not disperse button cell made of nano silica fume body obtained and pass through blue electric electro-chemical test instrument respectively to make electrochemistry
It can test, the chemical property of both test experiments comparisons.
The first discharge specific capacity of button cell made from undispersed nano silica fume is 2424.7mAh/g, initial charge
Specific capacity is 1666.3mAh/g, coulombic efficiency 68.73%.
The first discharge specific capacity of button cell made from nano silica fume after cetyl trimethylammonium bromide disperses
For 3165.9mAh/g, initial charge specific capacity is 2681.2mAh/g, coulombic efficiency 84.69%.More undispersed nano-silicon
The discharging efficiency of powder improves 30.6%, and charge efficiency improves 60.9%, and coulombic efficiency improves 15.96%.
It is greatly mentioned it can be seen that being had using chemical property of the cetyl trimethylammonium bromide ionic dispersants to silicon powder
Height, this is because particle agglomeration forms bulky grain, and in charge and discharge process, particle be will receive accordingly when silicon powder does not disperse
Reunion stress, the stress that bulky grain group is subject to more greatly is also bigger, while corresponding volume expansion effect occurs for silicon powder
Also bigger, to cause electrode structure to destroy, specific capacity irreversible loss is larger.After powder granule is dispersed to break up,
The stress that small particle is subject to is relatively isolated, it is difficult to damage to electrode structure, occur in electrochemical reaction in this way
The lithium source amount of circular response is also just more, so that cycle efficieny is also bigger, so carrying out dispersing agent processing to nano silica fume can
It is effectively improved the chemical property of silicon electrode material, the specific capacity and coulomb effect of battery is improved, improves the cycle performance of battery.
The above is only the preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, any
The transformation and replacement carried out based on technical solution provided by the present invention and inventive concept should all be covered in protection model of the invention
In enclosing.
Claims (7)
1. a kind of dispersing method of nano-silicon, it is characterised in that: the following steps are included:
(1) SILICA FUME for being 3-5 μm through air-flow crushing to average grain diameter by thick silicon powder；
(2) SILICA FUME is dissolved in polar solvent and stirring is made into the silicon solution of solid content 10%-15%；
(3) it takes wet ball grinding technique to carry out ball milling silicon solution, and cetyl trimethyl bromination is added in mechanical milling process
Ammonium ion dispersing agent, up to nano-silicon powder after ball milling.
2. a kind of dispersing method of nano-silicon according to claim 1, it is characterised in that: the polar solvent in step (2)
Using dehydrated alcohol.
3. a kind of dispersing method of nano-silicon according to claim 1, it is characterised in that: the silicon being made into step (2) is molten
The solid content of liquid is 15%.
4. a kind of dispersing method of nano-silicon according to claim 1, it is characterised in that: the wet ball grinding in step (3)
Ratio of grinding media to material be 3:1, media diameters 1mm, rotational speed of ball-mill 1200r/min, Ball-milling Time 8h, ball milling temperature control at 26 DEG C -30
℃。
5. a kind of dispersing method of nano-silicon according to claim 1, it is characterised in that: hexadecane in the step (3)
The additional amount of base trimethylammonium bromide ionic dispersants is the 0.5%-2.5% of silicon solution total amount.
6. a kind of dispersing method of nano-silicon according to claim 1, it is characterised in that: hexadecane in the step (3)
The additional amount of base trimethylammonium bromide ionic dispersants is the 1.5% of silicon solution total amount.
7. nano-silicon powder made from any nano-silicon dispersing method described in -6 is used for lithium-ion electric according to claim 1
Pond negative electrode material.
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| CN1482183A (en) * | 2002-08-14 | 2004-03-17 | ��������ķ������ | Aqueous silica dispersion |
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