CN109860548A - A kind of preparation method and applications of nano silicon material - Google Patents
A kind of preparation method and applications of nano silicon material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of nano silicon material, comprising the following steps: (1) is ground thick silicon slurry to obtain micron silicon slurry material；(2) carbon material is added in the micron silicon slurry material to be ground, obtains nano silicone slurry material；(3) the nano silicone slurry material dried, be crushed, is sieved, except magnetic treatment, obtaining nano silicon material.During preparation method of the invention, carbon material is added as abrasive media, it is thinner on the one hand to can promote particulate abrasive；On the other hand, carbon material substitutes traditional dispersing agent, effectively avoids the generation of hard aggregation phenomenon between silicon nanoparticle, reduces dispersing agent residual, effectively promotes material conductivity, further promote material electrochemical performance.
Description
Technical field
The invention belongs to the preparation field of nano-powder more particularly to a kind of receiving applied to lithium ion battery negative material
The preparation method of rice silicon materials.
Background technique
Currently, commercial Li-ion battery negative electrode material is based on graphite-like, and theoretical specific capacity 372mAh/g, existing skill
Art development capacity 350-360mAh/g has been approached theoretical value, and potentiality to be exploited is limited.In addition, four ministries and commissions " are promoting automobile power electricity
Pond industry development action scheme " in clearly propose to realize single battery specific energy >=300Wh/kg target, it is negative using graphite
Pole is unable to satisfy this demand, thus the negative electrode material for developing Novel high-specific capacity flexible seems particularly critical.
Silicon materials are due to higher lithium storage content (theoretical specific capacity 4200mAh/g), lower discharge platform, rich reserves
Etc. advantages become solve 300Wh/kg target breach.However the low and cyclicity of head effect in charge and discharge process it is poor the problems such as at
For the stumbling-block for hindering silicon materials industrial applications: silicon materials have biggish expansion rate (> 300%) in charge and discharge process,
It will lead to the dusting of silicon particle and being continuously generated and consuming for SEI film, constantly decay so as to cause performance；As semiconductor material
Material, electron conduction and ionic conductivity are all relatively low, are unable to satisfy power battery related needs.
To solve the above problems, mainly carrying out nanosizing, alloying and cladding etc. to silicon materials.Nanosizing is to prepare nanometer
The silicon materials of size are the first steps that silicon carbon material is synthetically prepared；Charge and discharge can be greatly lowered in the nano-silicon of smaller size
Cubical expansivity in journey promotes the anti-expansive force of material, mitigates the adverse effect in charge and discharge process.Nano-scale is prepared at present
Silicon materials method mainly have mechanical milling method, vapour deposition process, hydrothermal synthesis method, sol-gal process, thermal reduction etc..It is above-mentioned
Method respectively has superiority and inferiority, wherein mechanical milling method is due to simple, at low cost, the easy realization batch production of apparatus and process and by numerous
The favor of technology developer.But there are following technological difficulties for the process: nano-silicon large specific surface area causes agglomeration tight
Weight；The contact of preparation process air frequently, easily causes silicon nanoparticle oxidation to generate silica, reduces silicon activity；It is added auxiliary
Though material or dispersing agent can solve agglomeration traits but be easily introduced other impurities reduction material property；In addition, nano-silicon partial size≤150nm
When, the easily oxidation remaining organic solvent that even ignites to its storage brings security risk under room temperature, and a degree of oxidation can
Problems are solved, therefore the Effective Regulation of oxidizability becomes another bottleneck being synthetically prepared.Such as patent document CN
A kind of method of nano silicone powder material fining preparation is disclosed in 105655570A, after this method is by being added dispersing agent,
The nanoscale silicon powder of 50-500nm is prepared in high speed grinding, though this method can realize the accuracy controlling of partial size, preparation dispersion
Uniform nano silica fume, dispersing agent additional amount quality accounting are 10%-20%, do not go associated dispersion agent in patent
It removes, this largely lowers material cell performance, limits nanosizing application and preparation.Patent document CN 107311181A is public
A kind of method that industrial silicon silicon ash prepares high-purity nano silicon particle of cloth.This method is raw material using industrial silicon silicon ash is collected, and is led to
Overpickling, corase grinding and wet method fine grinding obtain the silicon nanoparticle that partial size is 100nm.Though the invention is prepared using industrial waste
Nano-silicon, but acid cleaning process introduces the hydrogen ion of higher concentration, on the one hand increases equipment cost for industrial volume production and environment is dirty
Dye；On the other hand acidity will be presented by preparing nano silicon material, and material property will be greatly lowered.The invention simultaneously prepares 100nm
Silicon nanoparticle its milling time be more than 30h, very will reduce production capacity to limits, and be less useful for industrial production.
Therefore, it is simple, low in cost to develop a kind of process equipment, is suitble to industrialized production, oxidation, size be controllable,
The nanometer silicon preparation method of good dispersion seems particularly critical；The exploitation of the technology will generate the application of silicium cathode material far-reaching
Influence.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
Kind is applied to the preparation method of the nano silicon material of lithium ion battery negative material.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
A kind of preparation method of nano silicon material, comprising the following steps:
(1) thick silicon slurry is ground to obtain micron silicon slurry material；
(2) carbon material is added in the micron silicon slurry material to be ground, obtains nano silicone slurry material；
(3) the nano silicone slurry material dried, be crushed, is sieved, except magnetic treatment, obtaining nano silicon material.
Above-mentioned preparation method, it is preferred that in the step (1) and (2), process of lapping carries out in protective gas；Institute
Stating protective gas is inert gas, including one of high pure nitrogen, argon gas.
Above-mentioned preparation method, it is preferred that in the step (2), carbon material is graphite, pitch, carbosphere, carbon nanometer
One of pipe, graphene, graphene oxide, carbon fiber are a variety of；The addition quality of carbon material is micron silicon stock quality
0.01-10%.Still more preferably, the addition quality of the carbon material is the 0.01-2% of micron silicon stock quality.
Above-mentioned preparation method, it is preferred that in the step (1) and (2), abrasive media is added in process of lapping, described to grind
Grinding media includes one of zirconium oxide, titanium oxide, silicon nitride, silicon carbide, tungsten carbide, boron nitride, boron carbide, zirconium boride or several
Kind.
Above-mentioned preparation method, it is preferred that in the step (1), abrasive media size is the abrasive media of different-grain diameter
It freely arranges in pairs or groups, little particle abrasive media particle size distribution range is 0.1-1.0mm, and middle particulate grinding medium particle size distribution range is 3-
10mm；Bulky grain abrasive media particle size distribution range is 30-100mm.
Above-mentioned preparation method, it is preferred that in the step (1), thick silicon slurry is after thick silicon is broken into thick silicon powder, to add
Enter into nonaqueous solvents, stirs, be sieved resulting slurry.
Above-mentioned preparation method, it is preferred that the nonaqueous solvents be dehydrated alcohol, ethylene glycol, glycerol, isopropanol, butanol,
One of polyethylene glycol, polyvinylpyrrolidone, acetone, hexamethylene, butanone, benzene class are a variety of；The thick silicon is that industry is more
One of crystal silicon block, silicon crystallite, industrial silicon ash are a variety of；The mass ratio of the thick silicon powder and nonaqueous solvents be 1:(0.1~
50), the partial size of the thick silicon powder is 50-500um.
Above-mentioned preparation method, it is preferred that in the step (1), milling time 2-24h, abrasive parameters 500-
3000rpm；Micron silicon slurry material partial size is 1.0-30um；
In the step (2), milling time 2-10h, abrasive parameters 500-3000rpm；Nano silicone slurry material grain
Diameter is 30-500nm.
Above-mentioned preparation method, it is preferred that in the step (3), drying mode is forced air drying, vacuum drying, is sprayed
One of dry, freeze-drying；The sieving refers to be carried out using one of ultrasonic wave vibrating sieving machine or airflow shifting machine
Sieve.
The inventive concept total as one, the present invention also provides a kind of above-mentioned preparation methods to prepare resulting nano-silicon material
Expect the application on lithium ion battery negative material.
Compared with the prior art, the advantages of the present invention are as follows:
(1) during preparation method of the invention, carbon material is added as abrasive media, graininess is on the one hand can promote and grinds
It grinds thinner；On the other hand, carbon material substitutes traditional dispersing agent, effectively avoids the generation of hard aggregation phenomenon between silicon nanoparticle,
And dispersing agent residual is reduced, while the addition of carbon material can effectively promote material conductivity.
(2) preparation method of the invention is ground in oxygen-free environment, guarantees that nano grain surface oxidizability is lower；Together
When, nano-silicon milling time is greatly reduced using echelon grinding, is conducive to promote production capacity.
(3) preparation method of the invention solves silicon powder degree of oxidation height, group in nano-silicon preparation process in the prior art
Poly- serious, the problems such as storage security risk is big, prepare that purity is high, granularity be controllable, storage is pacified by the grinding of simple and mechanical echelon
Full nano-silicon.
(4) silicon materials of preparation method of the invention preparation are it in the good, first using dispersion effect is provided of battery material
Effect and the high silicon based composite material presoma of specific capacity, while preparation process of the present invention is simple, at low cost, raw material sources are extensive,
Can high volume applications in LITHIUM BATTERY silicon carbon material field.
In conclusion the present invention is ground with simple closed echelon, ambient oxygen content is ground by strict control, is added
Carbon material obtains the controllable nanoscale silicon powder of oxidizability, particle size distribution range as dispersion abrasive media, adjustment abrasive parameters；
Meanwhile on the one hand the addition of carbon material is conducive to the grinding of nano-silicon, reduce the generation of agglomeration, it on the other hand can be further
The electric conductivity for promoting nano silicon material promotes material electrochemical performance.This method is simple and convenient, efficient, at low cost, easy realization produces
Industry is, it can be achieved that LITHIUM BATTERY large-scale application.
Detailed description of the invention
Fig. 1 is the SEM figure of nano-silicon made from the embodiment of the present invention 2.
Fig. 2 is the XRD diagram of nano-silicon made from the embodiment of the present invention 2.
Fig. 3 is the SEM figure of nano-silicon made from comparison example 1 of the present invention.
Fig. 4 is the SEM figure of nano-silicon made from comparison example 2 of the present invention.
Specific embodiment
To facilitate the understanding of the present invention, invention herein is done below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
A kind of preparation method of nano silicon material of the invention, comprising the following steps:
(1) 1kg industry silicon ash is weighed, after being placed in the broken crusher machine 2h in Hubei Province, is placed in ball-grinding machine and crushes 3h, obtain thick silicon
Powder, partial size concentrate on 50-500um；
4kg dehydrated alcohol is added in resulting thick silicon powder, by crossing 32 mesh screens after the high-speed stirred of 500rpm, is made
Thick silicon powder slurry；
(2) into thick silicon powder slurry made from step (1) be added boron nitride ball (median particle diameter of boron nitride ball be 0.3mm,
3mm, 50mm, mass ratio 3:2:1), it is that 1:1 mode is matched according to quality of material ratio；
Slurry is placed in the high-energy planetary ball mill machine of closed logical protection gas (high pure nitrogen) and grinds 15h (revolving speed
800rpm), 325 mesh screens are crossed, the micron silicon slurry of uniform dispersion is obtained；
(3) 50g carbon nanotube is added into micron silicon slurry material obtained in step (2), passes through the high speed of 500rpm
It stirs to get and disperses uniform slurry；
The slurry is placed in the sand mill of closed logical protection gas (high pure nitrogen) and grinds 6h (3000rpm), is dispersed
Uniform nano silicone slurry material；
(4) by nano-silicon slurry obtained in step (3), 325 mesh screens are crossed by vacuum drying, crushing, ultrasonic vibration
It is sieved, except the nanoscale silicon powder for being prepared into partial size after magnetic as 30-100nm.
Embodiment 2:
A kind of preparation method of nano silicon material of the invention, comprising the following steps:
(1) 500g polysilicon block is weighed, after being placed in the broken crusher machine 2h in Hubei Province, as 2h is crushed in ball-grinding machine, obtains thick silicon
Powder, partial size concentrate on 50-500um；
9kg isopropanol will be added in resulting thick silicon powder, 32 mesh screens are crossed by high-speed stirred (500rpm) afterwards, is made thick
Silicon powder slurry；
(2) into thick silicon powder slurry made from step (1) be added zirconia ball (median particle diameter of zirconia ball be 0.5mm,
5mm, 80mm, mass ratio 3:2:1), it is that 1:1 mode is matched according to quality of material ratio；
Slurry is placed in the high-energy planetary ball mill machine of closed logical protection gas (high-purity argon gas) and grinds (revolving speed 800rpm)
10h crosses 325 mesh screens, obtains the micron silicon slurry of uniform dispersion；
(3) 15g graphene oxide is added into micron silicon slurry material obtained in step (2), passes through the height of 200rpm
Speed, which stirs to get, disperses uniform slurry；
The slurry is placed in the sand mill of closed high-purity argon gas, 6h is ground with the revolving speed of 3000rpm, obtains dispersing uniform
Nano silicone slurry material；
(4) by nano-silicon slurry obtained in step (3), by freeze-drying, crushing, vibration screening, except being prepared after magnetic
The nanoscale silicon powder for being 30-100nm at partial size, characterization are as depicted in figs. 1 and 2.
Comparative example 1:
The difference of the preparation method and embodiment 2 of the nano silicon material of this comparative example is only that, directly will be after step (2)
Micron silicon slurry is placed in open sand mill and grinds 6h, by vacuum drying, crushing, vibration screening, except being prepared into after magnetic
Partial size is the nanoscale silicon powder of 200-300nm, and characterization is as shown in Figure 3.
Comparative example 2:
The difference of the preparation method and embodiment 2 of the nano silicon material of this comparative example is only that, the mode of operation of step (3)
Difference replaces graphene oxide, specific step (3) mode of operation are as follows: to step (2) using dispersing agent sodium carboxymethylcellulose
Obtained in 50g dispersing agent sodium carboxymethylcellulose is added in nano silicone slurry, obtain dispersing by high-speed stirred uniform
Slurry；The slurry is placed in again in the high-energy planetary ball mill machine of closed logical protection gas and grinds 6h, obtains dispersing uniform nanoscale
Silicon powder slurry；By freeze-drying, crushing, vibration screening, except be prepared into after magnetic partial size be 100-200nm nanoscale silicon powder,
Characterization is as shown in Figure 4.
It is found that nanoscale silicon powder (Fig. 1) prepared by embodiment 2 compares comparative example 2 (Fig. 4), silicon powder grain divides the comparison of SEM characterization
It is substantially similar to dissipate property, there are twice dispersings a degree of soft-agglomerated, that the later period passes through the achievable silicon powder of ultrasonic treatment.Comparative example
Dispersing agent or carbon material (Fig. 3) is not added in 1, the nano silica fume partial size of grinding is thicker, reaches 200-300nm, and there are blocking
Hardened phenomenon, the dispersion again for influencing nano-silicon use.Cubic phase structure, the knot is presented in silicon powder (Fig. 2) prepared by embodiment 2
Structure is suitable for negative electrode material；There are not other peak positions in XRD simultaneously, also turns out that carbon material additional amount is few.
Embodiment 3:
A kind of preparation method of nano silicon material of the invention, comprising the following steps:
(1) 500g silicon crystallite is weighed, after being placed in the broken crusher machine 2h in Hubei Province, is placed in ball-grinding machine and crushes 3h, obtain thick silicon powder,
Thick silicon powder partial size concentrates on 50-500um；
5kg polyvinylpyrrolidone will be added in thick silicon powder obtained, 32 meshes are crossed by high-speed stirred (200rpm) afterwards
Thick silicon powder slurry is made in net；
(2) into thick silicon powder slurry made from step (1) be added tungsten-carbide ball (median particle diameter of tungsten-carbide ball be 1.0mm,
10mm, 50mm, wherein mass ratio is 3:2:1), it is that 1:1 mode is matched according to quality of material ratio；
Slurry is placed in the type taper grinder of closed logical protection gas (argon gas), 10h is ground with the revolving speed of 2000rpm, crosses 325 mesh
Sieve obtains the micron silicon slurry of uniform dispersion；
(3) 5g graphite is added into micron silicon slurry material obtained in step (2), passes through high speed (revolving speed 200rpm)
It stirs to get and disperses uniform slurry；
The slurry is placed in the high-energy planetary ball mill machine of closed logical protection gas (high pure nitrogen) and is ground with the revolving speed of 3000rpm
3h is ground, obtains dispersing uniform nano silicone slurry material；
(4) by nano-silicon slurry obtained in step (3), by forced air drying, crushing, vibration screening, except being prepared after magnetic
The nanoscale silicon powder for being 300-400nm at partial size.
Embodiment 4:
A kind of preparation method of nano silicon material of the invention, comprising the following steps:
(1) 200kg industry silicon ash is weighed, 5kgN- methyl pyrrolidone is added, after being placed in the broken crusher machine in Hubei Province, is placed in ball milling
3h is crushed in equipment, crosses 32 mesh screens, thick silicon powder slurry is made, and thick silicon grain diameter integrated distribution is 50-500um；
(2) into thick silicon powder slurry made from step (1) be added tungsten-carbide ball (median particle diameter of tungsten-carbide ball be 0.5mm,
30mm, 50mm, wherein mass ratio is 3:2:1), it is that 1:1 mode is matched according to quality of material ratio；
Slurry is placed in the tube mill of closed logical protection gas (high pure nitrogen), 8h is ground with the revolving speed of 3000rpm, crosses 325
Mesh screen obtains the micron silicon slurry of uniform dispersion；
(3) 50g asphalt powder is added into micron silicon slurry material obtained in step (2), by with the revolving speed of 200rpm
High-speed stirred obtains dispersing uniform slurry；
The slurry is placed in the sand mill of closed logical protection gas (high pure nitrogen), 3h is ground with the revolving speed of 3000rpm, obtained
The nano silicone slurry material uniform to dispersion；
(4) by nano-silicon slurry obtained in step (3), by vacuum drying, crushing, vibration screening, except being prepared after magnetic
The nanoscale silicon powder for being 200-300nm at partial size.
Electrochemistry is tested using following methods: cathode is used as after nano silica fume and artificial graphite are mixed according to 1:9
Then material is that 93:1:6 carries out slurrying with conductive agent, binder in mass ratio, slurry solid content is controlled 50%, then will slurry
Material is coated in copper foil current collector, and cathode pole piece is made, and pole piece compaction density is controlled in 1.5g/cm3；Using metal lithium sheet conduct
To electrode, the LiPF of 1mol/L6/ EC+DMC electrolyte, is assembled into 2032 button cells.Battery uses LAND battery testing body
System, constant current charge-discharge is tested at 0.1C, and voltage range 0.001-1.5V, test result is as follows shown in table 1:
Table 1: nano-silicon produced by the present invention, which is made, buckles Contrast of Electrical Parameter table；
As shown in Table 1, embodiment 2 is detained electric specific capacity compared with comparative example 2, made of the nano-silicon of embodiment 2 and is reached
597mAh/g, coulombic efficiency reaches 88.4% for the first time, shows that the addition of a small amount of carbon material can not only solve silicon powder agglomeration traits, together
When can solve the problems, such as that dispersing agent addition leads to material specific capacity and first effect decline；Embodiment 2 is compared with comparative example 1, nano-silicon system
At button electricity specific capacity otherness it is larger, essentially consist in embodiment 2 carry out environmental regulatory control promote nano-silicon degree of oxidation reduce, from
And guaranteeing that material specific capacity is more excellent, head effect is higher (oxidation generates silica, and head effect is low).
Using the oxygen content in oxygen-nitrogen analyzer ONH-801A test nano-silicon, comparative sample is that (oxygen content is lead oxide
9.9%): the nano-silicon of preparation is subjected to oxygen content test, test result is as follows shown in table 2:
Table 2: nano-silicon oxygen content contrast table produced by the present invention；
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| Oxygen content (%) | 9.8541 | 9.2641 | 10.3498 | 10.5276 | 15.6293 | 10.2457 |
Therefore, nano-silicon prepared by the present invention can effectively improve the initial charge specific capacity of battery as battery material
And coulombic efficiency: being on the one hand that the carbon medium being added can alleviate the reuniting effect of nano-silicon to a certain extent, increases material and leads
Electrically；Further aspect is that oxygen-free environment is managed, guarantee that the nano silica fume degree of oxidation of preparation is low.
Claims (10)
1. a kind of preparation method of nano silicon material, which comprises the following steps:
(1) thick silicon slurry is ground to obtain micron silicon slurry material；
(2) carbon material is added in the micron silicon slurry material to be ground, obtains nano silicone slurry material；
(3) the nano silicone slurry material dried, be crushed, is sieved, except magnetic treatment, obtaining nano silicon material.
2. preparation method as described in claim 1, which is characterized in that in the step (1) and (2), process of lapping is being protected
It is carried out in gas.
3. preparation method as described in claim 1, which is characterized in that in the step (2), carbon material is graphite, pitch, carbon
One of microballoon, carbon nanotube, graphene, graphene oxide, carbon fiber are a variety of；The addition quality of carbon material is micron order
The 0.01-10% of silicon stock quality.
4. preparation method as described in claim 1, which is characterized in that in the step (1) and (2), process of lapping addition is ground
Grinding media, the abrasive media include zirconium oxide, titanium oxide, silicon nitride, silicon carbide, tungsten carbide, boron nitride, boron carbide, boronation
One or more of zirconium.
5. preparation method as claimed in claim 4, which is characterized in that in the step (1), abrasive media is different-grain diameter
Abrasive media is freely arranged in pairs or groups, and little particle abrasive media particle size distribution range is 0.1-1.0mm, middle particulate grinding medium particle diameter distribution
Range is 3-10mm, and bulky grain abrasive media particle size distribution range is 30-100mm.
6. preparation method as described in any one in claim 1-5, which is characterized in that in the step (1), thick silicon slurry be by
After thick silicon is broken into thick silicon powder, it is added into nonaqueous solvents, stirs, be sieved resulting slurry.
7. preparation method as claimed in claim 6, which is characterized in that the nonaqueous solvents is dehydrated alcohol, ethylene glycol, sweet
One of oil, isopropanol, butanol, polyethylene glycol, polyvinylpyrrolidone, acetone, hexamethylene, butanone, benzene class are a variety of；Institute
Stating thick silicon is one of Commercial multicrystalline silico briquette, silicon crystallite, industrial silicon ash or a variety of；The quality of the thick silicon powder and nonaqueous solvents
Than for 1:(0.1~50), the partial size of the thick silicon powder is 50-500um.
8. preparation method as described in any one in claim 1-5, which is characterized in that in the step (1), milling time 2-
For 24 hours, abrasive parameters 500-3000rpm；Micron silicon slurry material partial size is 1.0-30um；
In the step (2), milling time 2-10h, abrasive parameters 500-3000rpm；Nano silicone slurry material partial size is
30-500nm。
9. preparation method as described in any one in claim 1-5, which is characterized in that in the step (3), drying mode is drum
Air-dry one of dry, vacuum drying, spray drying, freeze-drying；The sieving refers to using ultrasonic wave vibrating sieving machine or air-flow
One of screening machine is sieved.
10. one kind prepares resulting nano silicon material in lithium ion battery by the described in any item preparation methods of claim 1-5
Application in negative electrode material.
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| CN111180719A (en) * | 2020-01-07 | 2020-05-19 | 马鞍山科达普锐能源科技有限公司 | Method for preparing nano silicon by three-stage grinding |
| CN111392731A (en) * | 2020-04-08 | 2020-07-10 | 江苏新效新材料科技有限公司 | Preparation method of nano silica sand mill by taking polyvinylpyrrolidone as dispersing agent |
| CN111446431A (en) * | 2020-04-14 | 2020-07-24 | 南京宁智高新材料研究院有限公司 | Method for enhancing interface contact of silicon-oxygen-carbon cathode material of lithium ion battery through oxygen transfer reaction |
| CN112645333A (en) * | 2019-10-11 | 2021-04-13 | 洛阳阿特斯光伏科技有限公司 | Preparation method of nano silicon powder, prepared nano silicon powder and application |
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