CN110040734A - A kind of nano-silicon and preparation method thereof - Google Patents
A kind of nano-silicon and preparation method thereof Download PDFInfo
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- CN110040734A CN110040734A CN201910199107.6A CN201910199107A CN110040734A CN 110040734 A CN110040734 A CN 110040734A CN 201910199107 A CN201910199107 A CN 201910199107A CN 110040734 A CN110040734 A CN 110040734A
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/023—Preparation by reduction of silica or free silica-containing material
- C01B33/025—Preparation by reduction of silica or free silica-containing material with carbon or a solid carbonaceous material, i.e. carbo-thermal process
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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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- 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 present invention discloses a kind of nano-silicon and preparation method thereof, wherein the method includes the steps: SiO 2 powder and graphene powder are mixed and carry out first sintering under inert atmosphere or purification atmosphere, obtains the first sintered product；First time pickling and first time oxidation processes are carried out to first sintered product, obtain intermediate product；The intermediate product is mixed with SiO 2 powder and carries out second under inert atmosphere or purification atmosphere and is sintered, the second sintered product is obtained；After carrying out crushing and second of pickling processes to second sintered product, nano-silicon is made.Nanometer silicon preparation method simple process provided by the invention, lower to the quality requirements of raw material, cost is relatively low；And the nano-silicon prepared through the invention has very high purity (99.99%), and the features such as uniform particle sizes.
Description
Technical field
The present invention relates to field of material preparation more particularly to a kind of nano-silicon and preparation method thereof.
Background technique
1989, using petroleum coke as cathode, LiCoO2For the patent of the secondary lithium battery system of positive electrode, by day
This Sony Corporation successfully applies, and launches in 1991.This system is named as lithium ion battery (Lithium-ion
Battery ).Lithium ion battery is because having specific energy height, memory-less effect, long service life, operating voltage high and environment friend
The advantages that good a, it has also become emphasis of current new energy and new material research.Lithium ion battery is answered extensively as power battery
For new-energy automobile, but the security performance of lithium ion battery, energy density, big high rate performance and cycle life also need into
One step improves, and there is presently no a kind of materials can fully meet automobile dynamic system to lithium ion battery requirement.
In recent years, commercial Li-ion battery negative electrode material of the graphite as mainstream, because its specific capacity has reached the limit
It is worth (372 mAhg-1), and its intercalation potential platform is close to the deposition potential of lithium metal, in quick charge or low temperature charging process
Easily cause security risk, limits graphite in future social development to the application in high capacity cell field.Silicon is high by feat of it
In 10 times of graphite of theoretical specific capacity (4200 mAhg-1) and moderate de- lithium current potential (< 0.5 V vs Li+/ Li) and reserves
The features such as abundant (27.6%), has obtained the close attention of negative electrode of lithium ion battery researcher.
The method that micron silicon is prepared on Vehicles Collected from Market is mainly laser method and silane cracking process.The silicon prepared using laser method
Usually nano-silicon, partial size can be down to 30nm, and price is up to 24,000,000 yuan/ton to the silicon of 30nm in the market, is used
Equipment price it is very expensive, and can not produce in enormous quantities, the practical application that this strongly limits silicon materials in field of batteries；
Elementary silicon is prepared according to silane cracking process, the silicon of preparation can reach Nano grade, but to greatest extent be only 80nm, price
Up to 12,000,000 yuan/ton, although the silicon purity of the method preparation is higher, this method is more harsh to working condition, production
The SiH generated in the process4And H2Inflammable and explosive, whole system has to and oxygen-barrier, cannot contact with the external world, therefore, the party
There is also biggish security risks for method.For silicon-based anode lithium ion battery, the partial size of silicon is smaller, and bulk effect is to electrode
Destructiveness it is smaller, when the partial size of silicon is less than 100 nm, effective solution is can be obtained in the bulk effect problem of electrode.However, high
Expensive raw material makes silicon-based anode be difficult to realize commercial applications.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of nano-silicon and preparation method thereof, purports
Complicated, cost of material is excessively high, poor operability solving the existing technique for preparing nano-silicon there are processes, it is difficult to realize scale
The problem of production.
Technical scheme is as follows:
A kind of preparation method of nano-silicon, wherein comprising steps of
SiO 2 powder and graphene powder are mixed and carry out first sintering under inert atmosphere or purification atmosphere, is obtained
First sintered product；
First time pickling and first time oxidation processes are carried out to first sintered product, obtain intermediate product；
The intermediate product is mixed with SiO 2 powder and carries out second under inert atmosphere or purification atmosphere and is sintered, is obtained
To the second sintered product；
After carrying out crushing and second of pickling processes to second sintered product, nano-silicon is made.
The preparation method of the nano-silicon, wherein the SiO 2 powder is granite powder, sandstone powder, black silicon
One of rock powder end and diatomite powder are a variety of.
The preparation method of the nano-silicon, wherein the average grain diameter of the SiO 2 powder is 0.01-20 μm, described
The average grain diameter of graphene powder is 0.01-20 μm.
The preparation method of the nano-silicon, wherein the inert atmosphere is selected from helium, neon, argon gas, nitrogen or vacuum gas
One of atmosphere；The purification atmosphere is selected from that chlorine, fluorine chlorine is high and one of fluorine gas atmosphere or a variety of.
The preparation method of the nano-silicon, wherein by natural siliceous sand powder and graphene powder according to mass ratio be 1:
The ratio of 10-10:1 mixes 0.5-60 h, then carries out first sintering under inert atmosphere or purification atmosphere, obtains the first burning
Tie product.
The preparation method of the nano-silicon, wherein the temperature of the first sintering is 300-2200 DEG C, first sintering
Time is 1-60h；The temperature of second of sintering is 300-2200 DEG C, and second of sintering time is 1-60h.
The preparation method of the nano-silicon, wherein acid used in the first time pickling and second of pickling is independent
Selected from HCl, HClO, HClO4、HF、H2SO4、H2CO3、HNO3、H2C2O4And CH3One of COOH or a variety of.
The preparation method of the nano-silicon, wherein the temperature of the first time oxidation processes is 200-800 DEG C.
The preparation method of the nano-silicon, wherein by the intermediate product and SiO 2 powder according to mass ratio be 1:
The ratio of 10-10:1 mixes, and carries out second under inert atmosphere or purification atmosphere and be sintered, and obtains the second sintered product.
A kind of nano-silicon, wherein be prepared using the preparation method of nano-silicon of the present invention.
The utility model has the advantages that compared with prior art, nanometer silicon preparation method provided by the invention using SiO 2 powder as
Raw material, from a wealth of sources cost is relatively low；And present invention process is simple, the process of preparation lower to the quality requirements of raw material
In there are no pollution to the environment, and process control is accurate, no harsh conditions, the features such as being suitable for mass production；And through the invention
The nano-silicon of preparation has purity higher (99.99%), and the features such as uniform particle sizes.
Detailed description of the invention
Fig. 1 is a kind of flow chart of the preparation method preferred embodiment of nano-silicon provided by the invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of the nano-silicon of preparation of the embodiment of the present invention.
Specific embodiment
The present invention provides a kind of nano-silicons and preparation method thereof, to make the purpose of the present invention, technical solution and effect more
Add clear, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein only to
It explains the present invention, is not intended to limit the present invention.
Referring to Fig. 1, the present invention provides a kind of flow chart of the preparation method preferred embodiment of nano-silicon, as schemed institute
Show comprising step:
S10, SiO 2 powder and graphene powder are mixed and carry out first sintering under inert atmosphere or purification atmosphere,
Obtain the first sintered product；
S20, first time pickling and first time oxidation processes are carried out to first sintered product, obtains intermediate product；
S30, the intermediate product is mixed with SiO 2 powder and carries out second under inert atmosphere or purification atmosphere and is burnt
Knot, obtains the second sintered product；
S40, after carrying out crushing and second of pickling processes to second sintered product, nano-silicon is made.
The present invention is using SiO 2 powder as raw material, by the way that SiO 2 powder and graphene powder to be sintered
Then processing carries out pickling and oxidation processes, remove the partial impurities in natural siliceous sand powder, obtain intermediate product；Then
The intermediate product is mixed with SiO 2 powder and is sintered again, elemental silicon is obtained；Finally to the simple substance
Silicon crush and pickling processes can be prepared by the high-purity nano silicon that purity is up to 99.99% and uniform particle sizes.The present invention mentions
The nanometer silicon preparation method of confession has simple process, and lower to the quality requirements of raw material, cost is relatively low, right during preparation
Environment does not pollute, and process control is accurate, no harsh conditions, the features such as being suitable for mass production.
In some embodiments, the SiO 2 powder is one of granite, sandstone, black quartzite and diatomite
Or it is a variety of by being mechanically pulverized, air-flow crushing or grind to form the powder that average grain diameter is 0.01-20 μm.In some implementations
In mode, the average grain diameter of the graphene powder is 0.01-20 μm.Preferably, hammer slice type powder can be selected in the disintegrating apparatus
It is broken machine, pair roller pulverizer, medicinal herb grinder, high energy ball mill, mechanical sand mill, high speed machine impact grinder, tooth-like
One of pulverizer, turbine type crushing machine, pressure mill formula pulverizer, milling type pulverizer, airslide disintegrating mill or raymond mill,
But not limited to this.
In some embodiments, the ratio for being 1:10-10:1 according to mass ratio by SiO 2 powder and graphene powder
Then example mixing 0.5-60 h carries out first sintering under inert atmosphere or purification atmosphere, obtains the first sintered product.At this
In embodiment, the Graphene powder can provide enough carbons and be reacted with SiO 2 powder and partial impurities,
Generate silicon carbide, silicon and metal oxide etc..It is preferred that the SiO 2 powder and graphene powder are 1 according to mass ratio:
The ratio of 4-1:6 is mixed, in the proportional region, it is ensured that SiO 2 powder, which sufficiently reacts, generates silicon carbide, is convenient for
High-purity, efficient nano-silicon is made in later period, and extra graphene can carry out oxidation processes removal.In the present embodiment,
The protective gas is one of helium, neon, argon gas, nitrogen or vacuum atmosphere, but not limited to this；The purification gas
Atmosphere is that chlorine, fluorine chlorine is high and one of fluorine gas or a variety of, but not limited to this；Present embodiment can either guarantee Graphene powder with
SiO 2 powder sufficiently carries out redox reaction in first sintering processing, and a part of other impurities are removed, and
And it not will cause other side reactions and cause the loss of element silicon.
In some embodiments, the temperature of the first sintering is 300-2200 DEG C, and the first sintering time is 1-
60h can realize the redox reaction between graphene powder and SiO 2 powder at such a temperature, and will not make
It is lost at silicon.
In some embodiments, first time pickling and first time oxidation processes are carried out to first sintered product, obtained
To intermediate product.In the present embodiment, acid used in the first time pickling is selected from HCl, HClO, HClO4、HF、H2SO4、H2CO3、
HNO3、H2C2O4And CH3One of COOH or a variety of, but not limited to this；The concentration of the acid between 0.1-12mol/L, and
Heated (such as 30-90 DEG C), in pickling to increase pickling effect, accelerate pickling efficiency；Preferably, described first
The time of secondary pickling is control in 1-300min；It is furthermore preferred that first time pickling time is 10-20min, within this time range
It can complete acid cleaning process and cause impurity removal to be not thorough because pickling time is too short, it will influence the pure of SiC
Degree.
In some embodiments, the first sintered product after first time pickling is subjected to 1-240 through deionized water
Then the washing of min utilizes bag filter, batch filter, plate and frame filter press, box filter, film filtering, tubular type mistake
One of filter plants such as filter are filtered first sintered product, subsequently to the first sintered product of filtering into
Row is dried, the drying process can for constant pressure and dry, be dried under reduced pressure, fluidized drying, one of freeze-drying etc.；It is described
Drying equipment then can tell drying machine with centrifugal spray, bubble using box like dryer, transport band drying machine, rotary dryer, LPG
Foam layer drying machine, vacuum oven, KJG hollow blade dryer, PLG Continuous disc drying machine, XSG Rotatingandflashstreamingdrier etc.
In any one；Further, first time oxidation processes are carried out to the first sintered product after drying, removes extra graphite
Alkene powder and sulfur impurity etc., obtain intermediate product, and the intermediate product mainly includes SiC and a small amount of Si, SiO2、
SiOx, metal, metal oxide etc..Preferably, the temperature of the first time oxidation processes is 200-800 DEG C, is aoxidized for the first time
Equipment used in handling is using in air dry oven, Muffle furnace, resistance furnace, electric arc furnaces, electrothermal furnace, induction furnace, plasma heating furnace
Any one, but not limited to this.
It in some embodiments, is 1:10-10:1's according to mass ratio by the intermediate product and SiO 2 powder
Ratio mixing, and carry out second under inert atmosphere or purification atmosphere and be sintered, obtain the second sintered product.Preferably, described
Second temperature is 300-2200 DEG C, and second of sintering time is 1-60h, at such a temperature in the intermediate product it is main at
Divide SiC and SiO 2 powder that redox reaction occurs and generate the second sintered product, second sintered product includes mainly
Ingredient elemental silicon and a small amount of SiO2、SiC、SiOxAnd metal oxide.
In some embodiments, second of pickling processes is being carried out after carrying out pulverization process to second sintered product
To remove the impurity such as the metal oxide in the second sintered product, by the second sintered product after pickling successively by filtering, doing
It can be prepared by the nano-silicon that purity is 99.99% after dry processing.
Further, the present invention also provides a kind of nano-silicons, wherein is prepared using the preparation method of nano-silicon as described above
It obtains.
Explanation is further explained to a kind of preparation method of nano-silicon of the present invention below by specific embodiment:
Embodiment 1
00.0 g of silica 1 and 10.0 g of graphene powder that partial size is 5 μm are weighed, poly- 500 ml tetrafluoroethene tank is placed in
In, after addition 200.0 g of agate bead, 2 h of ball milling, solid mixture is obtained, solid mixture is placed in high temperature carbonization furnace, neon
Gas obtains pre-treatment sample as protective gas, 700 DEG C of 13 h of calcining.First pre-treatment sample is soaked in the HF solution of 1 mlol/L
In, after 50 min are mixed, it is transferred in Muffle furnace after bag filter, under air atmosphere, is obtained in 420 DEG C of 4 h of calcining
Intermediate sample.The intermediate sample for weighing silica 640.0 g and 80.0 g that partial size is 5 μm is scattered in 1.5 L deionized waters,
It carries out being spray-dried to obtain hybrid solid powder after 8 h of mechanical stirring.Hybrid solid powder is placed in high temperature carbonization furnace, neon is made
For protective atmosphere, high-purity micron silicon is obtained after 9 h are calcined at 1150 DEG C.High-purity micron silicon is crushed by pair roller pulverizer
Afterwards, it is transferred to the H of 1 mol/L2SO4It in solution, is filtered under diminished pressure after impregnating 4 h, and transfers the material into air dry oven and do
It is dry to get arrive high-purity nano-silicon.The scanning electron microscope (SEM) photograph of the nano-silicon is as shown in Figure 2.
Above-mentioned sample is crossed into 400 meshes, as active material, CMC is used as and leads as binder, SP as thickener, SBR
Electric agent, according to active material: CMC:SBR:S=90:3:3:4 quality proportioning after stirring, is coated on copper foil, first puts
Enter dry 8 h in 100 DEG C of air dry oven, is washed into pole piece with the formed punch that diameter is 12.5 mm, juxtaposition is in a vacuum drying oven
In 70 DEG C of dry 8 h.Pole piece is transferred in vacuum glove box, is anode with metal lithium sheet, PP is diaphragm, 1mol/L hexafluoro phosphorus
The ethylene carbonate of sour lithium and the mixed solution of propene carbonate are electrolyte, dress up CR2016 button cell, are tested in LAND
Constant current charge-discharge test is carried out in system, charge and discharge are carried out under the current density of 200 mAh/g, and the blanking voltage of charge and discharge is
0.01~1.0V。
Embodiment 2
00.0 g of silica 1 and 10.0 g of graphene powder that partial size is 5 μm are weighed, poly- 500 ml tetrafluoroethene tank is placed in
In, after addition 200.0 g of agate bead, 2 h of ball milling, solid mixture is obtained, solid mixture is placed in high temperature carbonization furnace, neon
Gas obtains pre-treatment sample as protective gas, 700 DEG C of 13 h of calcining.First pre-treatment sample is soaked in the HF solution of 1 mlol/L
In, after 50 min are mixed, it is transferred in Muffle furnace after bag filter, under air atmosphere, is obtained in 250 DEG C of 4 h of calcining
Intermediate sample.The intermediate sample for weighing silica 640.0 g and 80.0 g that partial size is 5 μm is scattered in 1.5 L deionized waters,
It carries out being spray-dried to obtain hybrid solid powder after 8 h of mechanical stirring.Hybrid solid powder is placed in high temperature carbonization furnace, neon is made
For protective atmosphere, high-purity micron silicon is obtained after 9 h are calcined at 1150 DEG C.High-purity micron silicon is crushed by pair roller pulverizer
Afterwards, it is transferred to the HNO of 1 mol/L3It in solution, is filtered under diminished pressure after impregnating 4 h, and transfers the material into air dry oven and do
It is dry to get arrive high-purity nano-silicon.
Above-mentioned sample is crossed into 400 meshes, as active material, CMC is used as and leads as binder, SP as thickener, SBR
Electric agent, according to active material: CMC:SBR:S=90:3:3:4 quality proportioning after stirring, is coated on copper foil, first puts
Enter dry 8 h in 100 DEG C of air dry oven, is washed into pole piece with the formed punch that diameter is 12.5 mm, juxtaposition is in a vacuum drying oven
In 70 DEG C of dry 8 h.Pole piece is transferred in vacuum glove box, is anode with metal lithium sheet, PP is diaphragm, 1 mol/L hexafluoro
The ethylene carbonate of lithium phosphate and the mixed solution of propene carbonate are electrolyte, dress up CR2016 button cell, are surveyed in LAND
Constant current charge-discharge test is carried out on test system, and charge and discharge, the blanking voltage of charge and discharge are carried out under the current density of 200 mAh/g
For 0.01 ~ 1.0V.
In conclusion nanometer silicon preparation method provided by the invention is using SiO 2 powder as raw material, source is wide
It is general that cost is relatively low；And present invention process is simple, and it is lower to the quality requirements of raw material, to environment without dirt during preparation
Dye, and process control is accurate, no harsh conditions, the features such as being suitable for mass production；And the nano-silicon tool prepared through the invention
It is higher (99.99%) there is purity, and the features such as uniform particle sizes.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of nano-silicon, which is characterized in that comprising steps of
SiO 2 powder and graphene powder are mixed and carry out first sintering under inert atmosphere or purification atmosphere, is obtained
First sintered product；
First time pickling and first time oxidation processes are carried out to first sintered product, obtain intermediate product；
The intermediate product is mixed with SiO 2 powder and carries out second under inert atmosphere or purification atmosphere and is sintered, is obtained
To the second sintered product；
After carrying out crushing and second of pickling processes to second sintered product, nano-silicon is made.
2. the preparation method of nano-silicon according to claim 1, which is characterized in that the SiO 2 powder is granite powder
One of end, sandstone powder, black quartzite powder and diatomite powder are a variety of.
3. the preparation method of nano-silicon according to claim 1, which is characterized in that the average grain diameter of the SiO 2 powder
It is 0.01-20 μm, the average grain diameter of the graphene powder is 0.01-20 μm.
4. the preparation method of nano-silicon according to claim 1, which is characterized in that the inert atmosphere be selected from helium, neon,
One of argon gas, nitrogen or vacuum atmosphere；The purification atmosphere is selected from that chlorine, fluorine chlorine is high and one of fluorine gas atmosphere or more
Kind.
5. the preparation method of nano-silicon according to claim 1, which is characterized in that by natural siliceous sand powder and Graphene powder
End mixes 0.5-60 h according to the ratio that mass ratio is 1:10-10:1, then carries out first under inert atmosphere or purification atmosphere
Secondary sintering obtains the first sintered product.
6. the preparation method of nano-silicon according to claim 1, which is characterized in that the temperature of the first sintering is 300-
2200 DEG C, the first sintering time is 1-60h；The temperature of second of sintering is 300-2200 DEG C, second of sintering time
For 1-60h.
7. the preparation method of nano-silicon according to claim 1, which is characterized in that the first time pickling and second of pickling
Acid used is independent to be selected from HCl, HClO, HClO4、HF、H2SO4、H2CO3、HNO3、H2C2O4And CH3One of COOH or
It is a variety of.
8. the preparation method of nano-silicon according to claim 1, which is characterized in that the temperature of the first time oxidation processes is
200-800℃。
9. the preparation method of nano-silicon according to claim 1, which is characterized in that by the intermediate product and silicon dioxide powder
End is mixed according to the ratio that mass ratio is 1:10-10:1, and is carried out second under inert atmosphere or purification atmosphere and be sintered, and is obtained
Second sintered product.
10. a kind of nano-silicon, which is characterized in that be prepared using the preparation method of any nano-silicon of claim 1-9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115196642A (en) * | 2022-07-04 | 2022-10-18 | 深圳市上欧新材料有限公司 | Method for purifying silicon dioxide |
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| CN104030290A (en) * | 2014-06-30 | 2014-09-10 | 金之坚 | Method for producing nanometer silicon by adopting rice hull |
| CN105347346A (en) * | 2015-12-08 | 2016-02-24 | 武汉科技大学 | Method for preparing porous nanometer silicon through air auxiliary |
| CN106044777A (en) * | 2016-06-01 | 2016-10-26 | 北京大学 | Novel method for preparing nanometer silicon from silicon dioxide |
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| CN101391772A (en) * | 2007-09-18 | 2009-03-25 | 晟茂（青岛）先进材料有限公司 | Method for preparing solar stage high purify nano silica flour and device system thereof |
| CN104030290A (en) * | 2014-06-30 | 2014-09-10 | 金之坚 | Method for producing nanometer silicon by adopting rice hull |
| CN105347346A (en) * | 2015-12-08 | 2016-02-24 | 武汉科技大学 | Method for preparing porous nanometer silicon through air auxiliary |
| CN106044777A (en) * | 2016-06-01 | 2016-10-26 | 北京大学 | Novel method for preparing nanometer silicon from silicon dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115196642A (en) * | 2022-07-04 | 2022-10-18 | 深圳市上欧新材料有限公司 | Method for purifying silicon dioxide |
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