CN105692623A - Method for preparing nanometer silicon through aluminum reduction - Google Patents
Method for preparing nanometer silicon through aluminum reduction Download PDFInfo
- Publication number
- CN105692623A CN105692623A CN201610025361.0A CN201610025361A CN105692623A CN 105692623 A CN105692623 A CN 105692623A CN 201610025361 A CN201610025361 A CN 201610025361A CN 105692623 A CN105692623 A CN 105692623A
- Authority
- CN
- China
- Prior art keywords
- powder
- product
- aluminium
- silicon
- sio
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to a method for preparing nanometer silicon through aluminum reduction. The method comprises the steps that at room temperature, aluminum powder and SiO2 powder are added into a ball mill, and mixed powder is obtained and put in a corundum boat; the corundum boat containing the mixed powder is put in a high temperature furnace, vacuumizing is performed till the pressure reaches 0.01 MPa, then the temperature is raised to reaction temperature within 3-5 hours under the protection of argon, natural cooling is performed till the temperature reaches the room temperature, and the reaction product is collected; diluted hydrochloric acid is added into the reaction product for a reaction, then centrifugal separation is performed, sediment is washed 2-4 times with deionized water after centrifugal separation, and the product is collected; hydrofluoric acid is added into the product for a reaction, then centrifugal separation is performed, sediment is washed 2-4 times with deionized water after centrifugal separation, and the nanometer silicon powder product is prepared. The method has the advantages that the process is simple, cost is low, and safety performance is high. The method is feasible for large-scale preparation of nanometer silicon.
Description
Technical field
The invention belongs to the preparation method technical field of nano-silicon, be specifically related to a kind of method that aluminium reducing prepares nano-silicon。
Background technology
Silicon is as the primary raw material of silicon electronic device, there is the incomparable superiority of other semi-conducting material and good application prospect, within following several years even time of more than ten years, all still position of mainstream will be occupied, silicon can as the negative material of lithium ion battery simultaneously, conventional lithium ion battery generally all uses graphite cathode, but the performance of this material has reached peak。Research finds that nano-silicon is likely to become graphite succedaneum, and its theoretical specific capacity, up to 4000mAh/g, is equivalent to the Li at room temperature synthesized15Si4, it is cathode material of lithium ion battery of future generation。Various silicon nanostructures are made negative material and are all illustrated excellent chemical property, but current manufacturing cost is high and affect its large-scale production application。
Prepare the method that nano-silicon adopts at present: (1) vapor phase method: plasma enhanced chemical vapor deposition (PECVD) (Cao Maosheng. ultramicro powder preparation science and technology, 1995,30,94), laser-induced chemical vapour deposition (UCVD) (Xiao Yiming. Laser Synthesized Ceramic, 1992), laser ablation deposition (LICVD) (a Peng outstanding person. the laser ablation deposition of Si-based quantum dots and VISIBLE LIGHT EMISSION characteristic, laser is with infrared, 2000,30 (2): 92-94)；The silicon source of vapor phase method is silane, and silane has high toxicity, the feature such as expensive and flammable, and prepares nano-silicon by chemical vapour deposition (CVD) (CVD) method, and its required manufacture equipment is much more expensive；(2) metal assisted chemical etch (MACE) method, the method processes the method for crystal silicon wafer and is widely studied, and recycling template and non-template method just may be utilized in fabricating height adjustable silicon nano material。But, the manufacturing cost of the other wafer of electron level is of a relatively high, and is still confined to a milligram level by the amount of the nano silicon material of MACE method manufacture；(3) pulse laser liquid phase deposition。The method is in the control of crystallite dimension and Density Distribution, the combination of the mcxst optimizing experimental parameters, and how still suffering from a lot of problem with the silicon planner technology aspect such as compatible mutually, the existence of these problems hinders the practical further of silicon nano material, and the method cost is also very high；(4) carbon thermal reduction silicon dioxide。The method reduction silicon dioxide needs the temperature of more than 1500 DEG C, but the fusing point of silicon is 1410 DEG C, and the silica flour of preparation very easily melts caking, so adopting carbon thermal reduction can prepare bulky crystal silicon, but it is infeasible to prepare nano-silicon；(5) magnesiothermic reduction silicon dioxide。The method is to prepare the main method of nano silicon material at present, and technique is relatively easy, due to magnesium powder price costly, and compares acutely with hydrochloric acid reaction in post processing, has explosion danger, bring potential safety hazard。
Summary of the invention
The purpose of the present invention shortcoming in order to overcome prior art, it is provided that a kind of technique is simple, cost is low, security performance is high and is applicable to the method that a kind of aluminium reducing of industrial mass production prepares nano-silicon。
For achieving the above object, the present invention provides following technical scheme, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 3～5 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 2～4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 2～4 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 50～500 orders, SiO2The particle diameter of powder is 10～100nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 1: 3～4: 1。Reaction temperature in described step 2 700～1200 DEG C, maintenance reaction temperature certain time is: 0.5～12 hour。The volume of the dilute hydrochloric acid in described step 3 is: 10～500mL, and concentration is: 0.1～6mol/L, and the response time is: 0.5～24 hour。Described in described step 4, the volume of Fluohydric acid. is: 10～500mL, and concentration is: 1～25mol/L, and the response time is: 0.5～24 hour。
The present invention scale can prepare nano-silicon, and advantage is in that: (1) raw materials used cost is low；(2) simple to operate, without dangerous, it is possible to large-scale use。Scanning electron microscope and X-ray diffraction is adopted to characterize pattern and the structure of nano-silicon。It is shown that the inventive method is compared with traditional preparation method, having technique simple, cost is low and security performance advantages of higher, provides feasible method to preparing nano-silicon on a large scale。
Accompanying drawing explanation
Fig. 1 is the exterior appearance figure preparing nano silica fume；
Fig. 2 is the electron scanning micrograph of the nano silica fume that embodiment 1 prepares；
Fig. 3 is the X-ray diffraction photo of the nano silica fume that embodiment 1 prepares。
Detailed description of the invention
The present invention is a kind of method that aluminium reducing prepares nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 3～5 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 2～4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 2～4 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 50～500 orders, SiO2The particle diameter of powder is 10～100nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 1: 3～4: 1。Reaction temperature in described step 2 700～1200 DEG C, maintenance reaction temperature certain time is: 0.5～12 hour。The volume of the dilute hydrochloric acid in described step 3 is: 10～500mL, and concentration is: 0.1～6mol/L, and the response time is: 0.5～24 hour。Described in described step 4, the volume of Fluohydric acid. is: 10～500mL, and concentration is: 1～25mol/L, and the response time is: 0.5～24 hour。
As it is shown in figure 1, preparing nano silica fume product by the present invention is bulk shape yellow powder。
For the more detailed explanation present invention, in conjunction with embodiment, the present invention is further elaborated。Specific embodiment is as follows:
Embodiment one
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 5 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, carry out centrifugation after removing unreacted SiO2 powder, by precipitate deionized water wash 4 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 200 orders, SiO2The particle diameter of powder is 20nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 5: 3。Reaction temperature in described step 2 1000 DEG C, maintenance reaction temperature certain time is: 2 hours。The volume of the dilute hydrochloric acid in described step 3 is: 100mL, and concentration is: 0.5mol/L, and the response time is: 24 hours。Described in described step 4, the volume of Fluohydric acid. is: 50mL, and concentration is: 1mol/L, and the response time is: 24 hours。
Fig. 2 show the electron scanning micrograph of the nano silica fume that embodiment one prepares, figure can clearly find that prepared sample is nano-silicon。Fig. 3 show the X-ray diffraction photo of the nano silica fume that embodiment one prepares, compared with the standard diffraction figure of nano-silicon, it is known that the product of embodiment one preparation is nano-silicon。
Embodiment two
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 3 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 2 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 2 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 200 orders, SiO2The particle diameter of powder is 100nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 1: 1。Reaction temperature in described step 2 800 DEG C, maintenance reaction temperature certain time is: 4 hours。The volume of the dilute hydrochloric acid in described step 3 is: 100mL, and concentration is: 0.5mol/L, and the response time is: 24 hours。Described in described step 4, the volume of Fluohydric acid. is: 50mL, and concentration is: 10mol/L, and the response time is: 24 hours。
Embodiment three
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 4 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 3 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 3 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 200 orders, SiO2The particle diameter of powder is 20nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 5: 3。Reaction temperature in described step 2 1000 DEG C, maintenance reaction temperature certain time is: 2 hours。The volume of the dilute hydrochloric acid in described step 3 is: 100mL, and concentration is: 0.5mol/L, and the response time is: 24 hours。Described in described step 4, the volume of Fluohydric acid. is: 50mL, and concentration is: 10mol/L, and the response time is: 24 hours。
Embodiment four
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 4 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 3 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 3 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 200 orders, SiO2The particle diameter of powder is 20nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 5: 3。Reaction temperature in described step 2 800 DEG C, maintenance reaction temperature certain time is: 4 hours。The volume of the dilute hydrochloric acid in described step 3 is: 10mL, and concentration is: 6mol/L, and the response time is: 6 hours。Described in described step 4, the volume of Fluohydric acid. is: 30mL, and concentration is: 20mol/L, and the response time is: 6 hours。
Embodiment five
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 3 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 2 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 100 orders, SiO2The particle diameter of powder is 50nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 4: 3。Reaction temperature in described step 2 900 DEG C, maintenance reaction temperature certain time is: 3 hours。The volume of the dilute hydrochloric acid in described step 3 is: 20mL, and concentration is: 3mol/L, and the response time is: 12 hours。Described in described step 4, the volume of Fluohydric acid. is: 30mL, and concentration is: 15mol/L, and the response time is: 12 hours。
Embodiment six
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 5 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 4 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 50 orders, SiO2The particle diameter of powder is 10nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 1: 3。Reaction temperature in described step 2 700 DEG C, maintenance reaction temperature certain time is: 12 hours。The volume of the dilute hydrochloric acid in described step 3 is: 10mL, and concentration is: 6mol/L, and the response time is: 0.5 hour。Described in described step 4, the volume of Fluohydric acid. is: 10mL, and concentration is: 25mol/L, and the response time is: 0.5 hour。
Embodiment seven
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 5 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 2 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 500 orders, SiO2The particle diameter of powder is 100nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 4: 1。Reaction temperature in described step 2 1200 DEG C, maintenance reaction temperature certain time is: 0.5 hour。The volume of the dilute hydrochloric acid in described step 3 is: 500mL, and concentration is: 0.1mol/L, and the response time is: 24 hours。Described in described step 4, the volume of Fluohydric acid. is: 500mL, and concentration is: 1mol/L, and the response time is: 24 hours。
Embodiment eight
A kind of aluminium reducing prepares the method for nano-silicon, and the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 5 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 4 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
The particle diameter of the aluminium powder in described step one is 275 orders, SiO2The particle diameter of powder is 55nm。Aluminium powder in described step one and SiO2The mol ratio of powder is 13: 6。Reaction temperature in described step 2 950 DEG C, maintenance reaction temperature certain time is: 6.25 hours。The volume of the dilute hydrochloric acid in described step 3 is: 255mL, and concentration is: 3.05mol/L, and the response time is: 12.25 hours。Described in described step 4, the volume of Fluohydric acid. is: 255mL, and concentration is: 15mol/L, and the response time is: 12.25 hours。
The a series of detailed description of those listed above is only for illustrating of the feasibility embodiment of the present invention; they also are not used to limit the scope of the invention, and all should be included within protection domain of the present utility model without departing from the skill of the present invention equivalent implementations made of spirit or change。
Claims (6)
1. the method that an aluminium reducing prepares nano-silicon, it is characterised in that: the method comprises the steps:
Step one: under room temperature, by aluminium powder and SiO2Powder joins in ball mill, after milled processed, obtains mixed-powder, is placed in corundum boat by above-mentioned mixed-powder；
Step 2: be positioned in high temperature furnace by corundum boat equipped with mixed-powder described in step one, is evacuated to after 0.01MPa under the protection of argon, is warmed up to reaction temperature in 3～5 hours; and after keeping reaction temperature certain time; naturally cool to room temperature again, stop logical argon, collecting reaction product；
Step 3: add dilute hydrochloric acid in the product described in step 2 and react, carry out centrifugation after removing unreacted aluminum and by-product aluminium oxide, by precipitate deionized water wash 2～4 times after centrifugation, through vacuum drying, finely ground, collect product；
Step 4: add Fluohydric acid. in the product described in step 3 and react, remove unreacted SiO2Centrifugation is carried out after powder, by precipitate deionized water wash 2～4 times after centrifugation, then through vacuum drying, finely ground, namely prepare nano silica fume product。
2. the method that a kind of aluminium reducing according to claim 1 prepares nano-silicon, it is characterised in that: the particle diameter of the aluminium powder in described step one is 50～500 orders, SiO2The particle diameter of powder is 10～100nm。
3. the method that a kind of aluminium reducing according to claim 1 prepares nano-silicon, it is characterised in that: aluminium powder in described step one and SiO2The mol ratio of powder is 1: 3～4: 1。
4. the method that a kind of aluminium reducing according to claim 1 prepares nano-silicon, it is characterised in that: the reaction temperature in described step 2 700～1200 DEG C, maintenance reaction temperature certain time is: 0.5～12 hour。
5. the method that a kind of aluminium reducing according to claim 1 prepares nano-silicon, it is characterised in that: the volume of the dilute hydrochloric acid in described step 3 is: 10～500mL, and concentration is: 0.1～6mol/L, and the response time is: 0.5～24 hour。
6. the method that a kind of aluminium reducing according to claim 1 prepares nano-silicon, it is characterised in that: described in described step 4, the volume of Fluohydric acid. is: 10～500mL, and concentration is: 1～25mol/L, and the response time is: 0.5～24 hour。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610025361.0A CN105692623A (en) | 2016-04-21 | 2016-04-21 | Method for preparing nanometer silicon through aluminum reduction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610025361.0A CN105692623A (en) | 2016-04-21 | 2016-04-21 | Method for preparing nanometer silicon through aluminum reduction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105692623A true CN105692623A (en) | 2016-06-22 |
Family
ID=56226415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610025361.0A Pending CN105692623A (en) | 2016-04-21 | 2016-04-21 | Method for preparing nanometer silicon through aluminum reduction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105692623A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109384231A (en) * | 2018-11-07 | 2019-02-26 | 苏州宇量电池有限公司 | A kind of preparation method of nano silicon material |
| CN109607544A (en) * | 2018-12-27 | 2019-04-12 | 王子衿 | A kind of method of synthesizing flaky nano elementary silicon |
| CN109694075A (en) * | 2018-12-18 | 2019-04-30 | 安徽工业大学 | A kind of low temperature ball milling nano silica fume, preparation method and application |
| CN110759521A (en) * | 2019-10-16 | 2020-02-07 | 中南大学 | Method for treating low-concentration copper-containing wastewater |
| CN112867692A (en) * | 2018-10-23 | 2021-05-28 | 斯科奥有限公司 | Integrated production of high purity silicon and alumina |
| CN113118450A (en) * | 2019-12-31 | 2021-07-16 | 拓米(成都)应用技术研究院有限公司 | Preparation method of nano-scale and submicron-scale metal powder |
-
2016
- 2016-04-21 CN CN201610025361.0A patent/CN105692623A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112867692A (en) * | 2018-10-23 | 2021-05-28 | 斯科奥有限公司 | Integrated production of high purity silicon and alumina |
| CN109384231A (en) * | 2018-11-07 | 2019-02-26 | 苏州宇量电池有限公司 | A kind of preparation method of nano silicon material |
| CN109694075A (en) * | 2018-12-18 | 2019-04-30 | 安徽工业大学 | A kind of low temperature ball milling nano silica fume, preparation method and application |
| CN109694075B (en) * | 2018-12-18 | 2021-02-23 | 安徽工业大学 | Low-temperature ball-milling nano silicon powder, preparation method and application |
| CN109607544A (en) * | 2018-12-27 | 2019-04-12 | 王子衿 | A kind of method of synthesizing flaky nano elementary silicon |
| CN110759521A (en) * | 2019-10-16 | 2020-02-07 | 中南大学 | Method for treating low-concentration copper-containing wastewater |
| CN110759521B (en) * | 2019-10-16 | 2020-09-25 | 中南大学 | Method for treating low-concentration copper-containing wastewater |
| CN113118450A (en) * | 2019-12-31 | 2021-07-16 | 拓米(成都)应用技术研究院有限公司 | Preparation method of nano-scale and submicron-scale metal powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105692623A (en) | Method for preparing nanometer silicon through aluminum reduction | |
| Yuda et al. | Advances of the top-down synthesis approach for high-performance silicon anodes in Li-ion batteries | |
| CN106784692B (en) | Graphene array loads lithium titanate/carbon/carbon nano tube composite array electrode material and its preparation method and application | |
| Liu et al. | Silica-derived hydrophobic colloidal nano-Si for lithium-ion batteries | |
| US10439206B2 (en) | Method and material for lithium ion battery anodes | |
| Zhu et al. | Hydrothermal synthesis of Zn2SnO4 nanorods in the diameter regime of sub-5 nm and their properties | |
| CN104036878B (en) | A kind of preparation method of graphene and CNT three-dimensional structure material | |
| JP2017514273A5 (en) | ||
| CN108946744A (en) | A kind of lithium ion battery preparation method for aoxidizing sub- silicium cathode material | |
| CN107098344A (en) | A kind of preparation method of two-dimensional layer MXene materials | |
| CN103626179A (en) | Method for preparing nanometer zirconium carbide powder | |
| CN106629685B (en) | A kind of three-dimensional graphene foam and preparation method thereof with multilevel structure | |
| CN115974550A (en) | Preparation method of tetragonal-phase nano-doped zirconia ceramic powder material with particle size D50 smaller than 100nm | |
| CN109494399A (en) | A kind of silicon/solid electrolyte nanocomposite and its preparation method and application | |
| CN109411730A (en) | A kind of lithium ion battery silicon substrate composite negative pole material and preparation method thereof | |
| Chundi et al. | Single layer hollow MgF2 nanoparticles as high-performance omnidirectional broadband antireflective coating for solar application | |
| CN107055606A (en) | A kind of preparation method of red schorl phase titanium dioxide nano ball | |
| CN109761239A (en) | It is a kind of sensing, photoelectricity or lithium ion battery composite material and preparation method | |
| CN101635320B (en) | Method for manufacturing titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device | |
| CN105948057B (en) | A kind of nano silicon particles and its preparation method and application | |
| CN113637941B (en) | Preparation method of zinc-gallium oxide magnetron sputtering target material | |
| CN108736006A (en) | A method of preparing silico-carbo composite material | |
| CN105016314A (en) | Preparation method for zinc selenide nano hollow spheres | |
| CN112645333B (en) | Preparation method of nano silicon powder, prepared nano silicon powder and application | |
| Kanaphan et al. | Multilayer Silicene Nanosheets Derived from a Recycling Process Using End-of-Life Solar Cells Producing a Silicene/Graphite Composite for Anodes in Lithium-Ion Batteries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160622 |