CN109081350A - A kind of method that watery fusion salt medium prepares nano-silicon - Google Patents
A kind of method that watery fusion salt medium prepares nano-silicon Download PDFInfo
- Publication number
- CN109081350A CN109081350A CN201811053832.4A CN201811053832A CN109081350A CN 109081350 A CN109081350 A CN 109081350A CN 201811053832 A CN201811053832 A CN 201811053832A CN 109081350 A CN109081350 A CN 109081350A
- Authority
- CN
- China
- Prior art keywords
- silicon
- salt medium
- nano
- preparing nano
- watery fusion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
Abstract
The invention discloses a kind of methods for preparing nano-silicon using watery fusion salt medium; the preparation of the nano-silicon is using silica as silicon source; under vacuum or inert atmosphere protection, by silica, metal hydride and anhydrous aluminum chloride be in mass ratio 1:1~5:5~20 ratio mixed grinding it is uniform; it is placed in reactor; 100~700 DEG C are risen to the heating rate of 1~20 DEG C/min, reacts 1~60h；After reaction, it is cooled to room temperature, reaction product is impregnated, deionized water washing through diluted acid, then filtered, vacuum drying is up to nano-silicon powder body material.The characteristics of the method for the present invention be reducing agent, anhydrous aluminum chloride fuse salt using metal hydride be reaction medium, nano-silicon can be prepared at a lower temperature, significantly reduce energy consumption and cost, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to amorphous silicon preparation technical fields, and in particular to a kind of watery fusion salt medium prepares the side of nano-silicon
Method.
Background technique
Silicon is one of most widely used element of industry, microelectronic component, integrated circuit, solar power generation and lithium from
The fields such as sub- battery are with important application prospects.The crustal abundance of silicon is 27%, is only second to oxygen (46%), silicon is less with simple substance
Form occur in nature, mainly exist in the form of complicated silicate or silica.The method for preparing pure silicon is more,
Its silicon source is mostly silica, fluosilicate, halosilanes and its derivative etc..Currently, the method for industrially preparing silicon mainly has:
(1) carbothermic method restores silica (SiO using silica (its main component is silica) in electric arc furnaces2Content is greater than
99%) reducing agent, used is petroleum coke and charcoal etc., can directly produce the high quality silicon of manufacture silicon steel sheet.(2) trichlorine hydrogen
Silicon hydrogen reduction method is (Siemens) company of Siemens to be invented in 1954, also known as Siemens Method, principle be
With the high-purity trichlorosilane of high-purity hydrogen reduction on 1100 DEG C or so of HIGH-PURITY SILICON core, polysilicon deposition is generated on silicon core, is made half
Conductor grade high-purity polycrystalline silicon.(3) silane decomposition, by SiH4Gas imports silane dore furnace, in 800~900 DEG C of fever
It is decomposed on silicon core and deposits high purity polycrystalline silicon.Above-mentioned several preparation method reaction temperature height and in process of production energy consumption
Greatly, a large amount of by-products are generated, the requirement to equipment is also very high.Therefore, a kind of efficient, economic, safe, environmental-friendly silicon is probed into
Preparation method has important application and popularization value.
Summary of the invention
It is that reaction is situated between that in view of the deficiencies of the prior art, it is an object of the present invention to provide one kind with low temperature chlorination aluminium fuse salt
Matter, the method that reducing silica is synthesized to nano-silicon using metal hydride, simple process, synthesis temperature are low, react
It is high-efficient, environmentally friendly, it is easy to industrialized production.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of method that low-temperature molten salt medium prepares nano-silicon, includes the following steps:
S1, under vacuum or protective atmosphere, silica containing raw material, metal hydride and anhydrous aluminum chloride are ground equal
It is even, and mixture is transferred in closed reactor；
S2, reactor is heated to 100~700 DEG C with the heating rate of 1~20 DEG C/min, and keeps the temperature 1~60h；
S3, to after reaction, be cooled to room temperature, take out reactor in solid product, successively through diluted acid impregnate, go from
Then sub- water washing filters, vacuum drying obtains nano silicon material.
In the present invention, the purity of raw metal hydride and anhydrous aluminum chloride is pure not less than chemistry.
Preferably, the matter of silica containing raw material, metal hydride and anhydrous aluminum chloride in the step S1
Amount is than 1:1~5:5~20.
Preferably, the metal hydride in the step S1 is lithium hydride, sodium hydride, hydrofining, magnesium hydride, hydrogenation
One or more of calcium.
Preferably, the silica containing raw material in the step S1 is silica, flyash, quartz, diatom
One or more of soil, silica, sand.
Preferably, the heating rate in the step S2 is 1~5 DEG C/min.
More preferably, the heating rate in the step S2 is 1 DEG C/min.
Preferably, the heating temperature in the step S2 is 100~500 DEG C.
More preferably, the heating temperature in the step S2 is 200 DEG C.
Preferably, the soaking time in the step S2 is 5~50 hours.
More there is choosing, the soaking time in the step S2 is 10 hours.
Preferably, the diluted acid in the step S3 is dilute hydrochloric acid, dilute sulfuric acid or diluted hydrofluoric acid.
More there is choosing, the molar concentration of the diluted acid in the step S3 is 0.1M.
The beneficial effects of the present invention are:
(1) oxidation occurs in medium of fused salt anhydrous aluminum chloride also using metal hydride and silica in the present invention
Original reaction generation amorphous silicon, preparation method low, high conversion efficiency with reaction temperature, preparation process are simple, controllable, safe and reliable
The features such as property is good；
(2) present invention used in silica containing raw material sources it is extensive, it is at low cost, efficient, environmentally protective, be easy to industry
Change and implements；
(3) the method for the present invention can prepare the nano silicon material of a variety of microscopic appearances, the material by controlling reaction condition
Material can be applicable to the numerous areas such as lithium ion battery, solar power generation.
Detailed description of the invention
Fig. 1 is nano-silicon X-ray diffraction (XRD) diffraction pattern prepared by embodiment 1；
Fig. 2 is the temperature, pressure curve graph of 1 reaction process of embodiment；
Fig. 3 is nano-silicon scanning electron microscope (SEM) figure prepared by embodiment 1.
Specific embodiment
With specific embodiment, technical scheme is described further below, but protection scope of the present invention is unlimited
In this.
Embodiment 1
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 0.6g silica, 0.6g magnesium hydride, 12g anhydrous aluminum chloride in protective atmosphere condition
Lower grinding uniformly, mixture is transferred to and is vacuumized in closed reactor；
(2) reactor is risen to 200 DEG C with reactor with the heating rate of 1 DEG C/min, and keeps the temperature 10h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M hydrochloric acid solution, go
Ion water washing three times, then filters, vacuum drying obtains nano-silicon.
Embodiment 2
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 0.6g silica, 3g magnesium hydride, 12g anhydrous aluminum chloride under the conditions of protective atmosphere
Grinding uniformly, mixture is transferred to and is vacuumized in closed reactor；
(2) reactor is risen to 700 DEG C with reactor with the heating rate of 5 DEG C/min, and keeps the temperature 1h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M dilution heat of sulfuric acid,
Deionized water is washed three times, is then filtered, vacuum drying obtains nano-silicon.
Embodiment 3
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 0.6g silica, 1.2g lithium hydride, 10g anhydrous aluminum chloride in protective atmosphere condition
Lower grinding uniformly, mixture is transferred to and is vacuumized in closed reactor；
(2) reactor is risen to 300 DEG C with reactor with the heating rate of 10 DEG C/min, and keeps the temperature 30h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M dilution heat of sulfuric acid,
Deionized water is washed three times, is then filtered, vacuum drying obtains nano-silicon.
Embodiment 4
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 0.6g silica, 1.0g sodium hydride, 8.0g anhydrous aluminum chloride in protective atmosphere item
It is ground uniformly under part, mixture is transferred to and is vacuumized in closed reactor；
(2) reactor is risen to 500 DEG C with reactor with the heating rate of 15 DEG C/min, and keeps the temperature 5h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M dilution heat of sulfuric acid,
Deionized water is washed three times, is then filtered, vacuum drying obtains nano-silicon.
Embodiment 5
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 0.6g silica, 2.0g hydrofining, 5g anhydrous aluminum chloride in protective atmosphere condition
Lower grinding uniformly, mixture is transferred to and is vacuumized in closed reactor；
(2) reactor is risen to 100 DEG C with reactor with the heating rate of 20 DEG C/min, and keeps the temperature 60h；
(3) after reaction, it is cooled to room temperature, takes out the solid product in reactor, it is successively molten through 0.1M diluted hydrofluoric acid
Liquid, deionized water washing three times, then filter, vacuum drying obtains nano-silicon.
Embodiment 6
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under vacuum conditions, by 10g diatomite, with the ratio of grinding media to material of 10:1, ball milling is for 24 hours under the conditions of 500r/min；Then
The good diatomite of the above-mentioned ball milling of 0.6g, 3g magnesium hydride, 12g anhydrous aluminum chloride are ground uniformly under the conditions of protective atmosphere, it will be upper
It states mixture and is transferred to and vacuumize in closed reactor；
(2) reactor reaction device is risen to 200 DEG C with the heating rate of 20 DEG C/min, and keeps the temperature 10h；
(3) after reaction, it is cooled to room temperature, takes out the solid product in reactor, it is successively molten through 0.1M diluted hydrofluoric acid
Then liquid, deionized water washing filter, vacuum drying obtains nano-silicon.
Embodiment 7
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 10g flyash under air conditions with the heating rate of 5 DEG C/min rise to 800 DEG C into
Row calcining, heat preservation is for 24 hours；Then by the good flyash of above-mentioned calcining, with the ratio of grinding media to material of 10:1, ball milling is for 24 hours under the conditions of 500r/min；
Then the good flyash of the above-mentioned ball milling of 0.6g, 2g magnesium hydride, 10g anhydrous aluminum chloride are ground uniformly under the conditions of protective atmosphere,
Said mixture is transferred to and is vacuumized in closed reactor；
(2) reactor is risen to 200 DEG C with the heating rate of 1 DEG C/min, and keeps the temperature 15h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M dilution heat of sulfuric acid,
Deionized water is washed three times, and then vacuum drying obtains nano-silicon.
Embodiment 8
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 10g quartz with the ratio of grinding media to material of 20:1 ball milling 48h under the conditions of 500r/min, then will
The good quartz of above-mentioned ball milling impregnates for 24 hours in the hydrochloric acid solution of 0.1M, dries under the conditions of 80 DEG C after then filtering；It will be on 0.6g
It states the sand handled well, 2g calcium hydride, 8g anhydrous aluminum chloride to grind under the conditions of protective atmosphere uniformly, said mixture is shifted
To vacuumizing in closed reactor；
(2) reactor is risen to 300 DEG C with the heating rate of 20 DEG C/min, and keeps the temperature 40h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M hydrochloric acid solution, go
Three times, then vacuum drying obtains nano-silicon to ion water washing.
Embodiment 9
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 10g silica with the ratio of grinding media to material of 15:1 ball milling 48h under the conditions of 500r/min；Then will
The good silica of above-mentioned ball milling impregnates for 24 hours in the hydrochloric acid solution of 0.1M, dries under the conditions of 80 DEG C after then filtering；It will be on 0.6g
It states the sand handled well, 3g calcium hydride, 12g anhydrous aluminum chloride to grind under the conditions of protective atmosphere uniformly, said mixture is turned
It moves to and vacuumizes in closed reactor；
(2) reactor is risen to 200 DEG C with the heating rate of 5 DEG C/min, and keeps the temperature 50h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M hydrochloric acid solution, go
Three times, then vacuum drying obtains nano-silicon to ion water washing.
Embodiment 10
A kind of method that low-temperature molten salt medium prepares nano-silicon, comprising the following steps:
(1) under an argon atmosphere, by 10g sand with the ratio of grinding media to material of 10:1 ball milling 108h under the conditions of 500r/min；Then
By the good sand of above-mentioned ball milling in the hydrochloric acid solution of 0.1M, under the conditions of 150 DEG C hydro-thermal for 24 hours, then filter after in 80 DEG C of conditions
Lower drying；The above-mentioned sand handled well of 0.6g, 0.6g hydrofining, 10g anhydrous aluminum chloride are ground under the conditions of protective atmosphere
It is even, said mixture is transferred to and is vacuumized in closed reactor；
(2) reactor is risen to 500 DEG C with the heating rate of 10 DEG C/min, and keeps the temperature 5h；
(3) after reaction, be cooled to room temperature, take out reactor in solid product, successively through 0.1M hydrochloric acid solution, go
Three times, then vacuum drying obtains nano-silicon to ion water washing.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (10)
1. a kind of method for preparing nano-silicon using watery fusion salt medium, which is characterized in that the method for preparing nano-silicon
The following steps are included:
S1, under vacuum or protective atmosphere, silica containing raw material, metal hydride and anhydrous aluminum chloride are ground equal
It is even, and abrasive material is transferred in the closed reactor vacuumized；
S2, reactor is heated to 100~700 DEG C with the heating rate of 1~20 DEG C/min, and keeps the temperature 1~60h；
S3, to after reaction, be cooled to room temperature, take out reactor in reaction product, successively through diluted acid impregnate, deionized water
Then washing filters, vacuum drying obtains nano silicon material.
2. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 1, which is characterized in that institute
The mass ratio for stating the silica containing raw material in step S1, metal hydride and anhydrous aluminum chloride is 1:1~5:5~20.
3. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 1, which is characterized in that institute
Stating the metal hydride in step S1 is one or more of lithium hydride, sodium hydride, hydrofining, magnesium hydride and calcium hydride.
4. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 1, which is characterized in that institute
Stating the silica containing raw material in step S1 is one of silica, flyash, quartz, diatomite, silica and sand
Or it is several.
5. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 1, which is characterized in that institute
Stating the heating rate in step S2 is 1~5 DEG C/min.
6. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 5, which is characterized in that institute
Stating the heating rate in step S2 is 1 DEG C/min.
7. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 1, which is characterized in that institute
Stating the heating temperature in step S2 is 100~500 DEG C, and soaking time is 5~50h.
8. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 7, which is characterized in that institute
Stating the heating temperature in step S2 is 200 DEG C, soaking time 10h.
9. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 1, which is characterized in that institute
Stating the diluted acid in step S3 is dilute hydrochloric acid, dilute sulfuric acid or diluted hydrofluoric acid.
10. a kind of method for preparing nano-silicon using watery fusion salt medium according to claim 9, which is characterized in that
The molar concentration of diluted acid in the step S3 is 0.1M.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811053832.4A CN109081350A (en) | 2018-09-11 | 2018-09-11 | A kind of method that watery fusion salt medium prepares nano-silicon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811053832.4A CN109081350A (en) | 2018-09-11 | 2018-09-11 | A kind of method that watery fusion salt medium prepares nano-silicon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109081350A true CN109081350A (en) | 2018-12-25 |
Family
ID=64841079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811053832.4A Pending CN109081350A (en) | 2018-09-11 | 2018-09-11 | A kind of method that watery fusion salt medium prepares nano-silicon |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109081350A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721057A (en) * | 2018-12-29 | 2019-05-07 | 安徽工业大学 | A kind of high efficient cryogenic molten salt preparation method of nano-silicon |
| CN110171832A (en) * | 2019-06-20 | 2019-08-27 | 浙江工业大学 | A method of porous silicon is prepared based on metal hydride reduction |
| CN110233251A (en) * | 2019-06-20 | 2019-09-13 | 浙江工业大学 | A kind of preparation method and applications of porous silicon/carbon composite material |
| CN110518195A (en) * | 2019-07-03 | 2019-11-29 | 浙江工业大学 | A kind of preparation method and application of nano-silicon/graphene composite material |
| CN113213483A (en) * | 2021-04-14 | 2021-08-06 | 三峡大学 | Preparation method of amorphous silicon powder for lithium ion battery cathode material |
| CN114695863A (en) * | 2022-03-31 | 2022-07-01 | 湖北工程学院 | Preparation method and application of three-dimensional layered Fe/C material |
| CN114684821A (en) * | 2022-03-31 | 2022-07-01 | 湖北工程学院 | Preparation method and application of metal hydride in-situ synthesis silicon/carbon nano composite material |
| CN115465864A (en) * | 2022-10-26 | 2022-12-13 | 南京林业大学 | Nano silicon material prepared by low-temperature molten salt thermal method and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671247A (en) * | 2015-02-11 | 2015-06-03 | 武汉科技大学 | Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof |
| CN106946259A (en) * | 2017-04-17 | 2017-07-14 | 浙江工业大学 | A kind of non-crystalline silicon raw powder's production technology |
| CN107634199A (en) * | 2017-09-05 | 2018-01-26 | 惠州亿纬锂能股份有限公司 | A kind of nano-silicon, preparation method and its application in silicon-carbon composite cathode material and lithium ion battery |
-
2018
- 2018-09-11 CN CN201811053832.4A patent/CN109081350A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671247A (en) * | 2015-02-11 | 2015-06-03 | 武汉科技大学 | Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof |
| CN106946259A (en) * | 2017-04-17 | 2017-07-14 | 浙江工业大学 | A kind of non-crystalline silicon raw powder's production technology |
| CN107634199A (en) * | 2017-09-05 | 2018-01-26 | 惠州亿纬锂能股份有限公司 | A kind of nano-silicon, preparation method and its application in silicon-carbon composite cathode material and lithium ion battery |
Non-Patent Citations (1)
| Title |
|---|
| ZHENYU ZHANG ET AL.: "Phase transformation of single crystal silicon induced by grinding with ultrafine diamond grits", 《SCRIPTA MATERIALIA》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721057A (en) * | 2018-12-29 | 2019-05-07 | 安徽工业大学 | A kind of high efficient cryogenic molten salt preparation method of nano-silicon |
| CN110171832A (en) * | 2019-06-20 | 2019-08-27 | 浙江工业大学 | A method of porous silicon is prepared based on metal hydride reduction |
| CN110233251A (en) * | 2019-06-20 | 2019-09-13 | 浙江工业大学 | A kind of preparation method and applications of porous silicon/carbon composite material |
| CN110518195A (en) * | 2019-07-03 | 2019-11-29 | 浙江工业大学 | A kind of preparation method and application of nano-silicon/graphene composite material |
| CN113213483A (en) * | 2021-04-14 | 2021-08-06 | 三峡大学 | Preparation method of amorphous silicon powder for lithium ion battery cathode material |
| US11834339B2 (en) | 2021-04-14 | 2023-12-05 | China Three Gorges University | Method for preparing amorphous silicon powder for anode material of lithium ion battery |
| CN114695863A (en) * | 2022-03-31 | 2022-07-01 | 湖北工程学院 | Preparation method and application of three-dimensional layered Fe/C material |
| CN114684821A (en) * | 2022-03-31 | 2022-07-01 | 湖北工程学院 | Preparation method and application of metal hydride in-situ synthesis silicon/carbon nano composite material |
| CN115465864A (en) * | 2022-10-26 | 2022-12-13 | 南京林业大学 | Nano silicon material prepared by low-temperature molten salt thermal method and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109081350A (en) | A kind of method that watery fusion salt medium prepares nano-silicon | |
| CN100372762C (en) | Method for preparing solar grade polysilicon | |
| CN108358206B (en) | Three-dimensional cross-linked structure silicon nano material and preparation method and application thereof | |
| CN108199030A (en) | The preparation method of lithium rechargeable battery Nano-porous Si/Graphite/C Composite Anode Materials | |
| CN105347346A (en) | Method for preparing porous nanometer silicon through air auxiliary | |
| US20110262339A1 (en) | Production of solar-grade silicon from silicon dioxide | |
| CN105905908B (en) | A kind of method that nano-silicon is prepared based on galapectite raw material | |
| US20190127225A1 (en) | Carbon nitride modified with perylenetetracarboxylic dianhydride / graphene oxide aerogel composite material, preparation method and application thereof | |
| CN105845912A (en) | Method for porous silicon titanium dioxide composite negative electrode material of lithium ion battery by taking diatomite as raw material | |
| CN106946259B (en) | A kind of amorphous silicon raw powder's production technology | |
| CN101362600B (en) | Method for removing boron from polysilicon by wet metallargy | |
| AU2017239429B2 (en) | Reduction of metal/semi-metal oxides | |
| CN107611416A (en) | A kind of Si-C composite material, its preparation method and application | |
| CN109748282B (en) | Method for preparing nano silicon carbide at low temperature | |
| CN105271238B (en) | A kind of method that utilization mechanochemical reaction prepares silicon powder | |
| CN110171832A (en) | A method of porous silicon is prepared based on metal hydride reduction | |
| CN111850612A (en) | System and method for comprehensively recovering metal resources in fly ash through molten salt electrolysis | |
| CN107986795A (en) | A kind of preparation method of high-purity silicon oxynitride | |
| CN104961137A (en) | Method for preparing nanometer alkaline-earth metal boride | |
| CN101054722A (en) | Purification and preparation method for solar energy polycrystalline silicon raw material | |
| CN106450220B (en) | A kind of biomass-based carbon-silicon composite material novel preparation method | |
| CN111196604A (en) | Method for preparing high-purity silicon by using waste micro-silicon powder as raw material | |
| CN116002660B (en) | Preparation method of carbon-silicon composite material, carbon-silicon composite material and lithium battery | |
| CN111056556A (en) | Method for preparing polycrystalline silicon by taking silicon dioxide and hydrogen as raw materials | |
| CN109179444A (en) | A kind of preparation method of amorphous boron powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181225 |
|
| RJ01 | Rejection of invention patent application after publication |