CN105712350A - Preparation method of nanometer silicon material - Google Patents
Preparation method of nanometer silicon material Download PDFInfo
- Publication number
- CN105712350A CN105712350A CN201610050619.2A CN201610050619A CN105712350A CN 105712350 A CN105712350 A CN 105712350A CN 201610050619 A CN201610050619 A CN 201610050619A CN 105712350 A CN105712350 A CN 105712350A
- Authority
- CN
- China
- Prior art keywords
- mixture
- ball
- mill
- silicon material
- preparation
- 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
-
- 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
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention relates to a preparation method of a nanometer silicon material. The preparation method includes mixing industrial silicon powder with absolute ethyl alcohol with stirring to obtain a mixture, wherein solid content of the mixture is 10-50%; subjecting the mixture to rough grinding by a planetary ball mill so as to obtain a rough ground mixture A; after ball grinding is terminated, taking out the mixture A, measuring the solid content of the mixture A, and supplementing the absolute ethyl alcohol to adjust the solid content of the mixture A to 1-20% so as to obtain a mixture B; filling a nano ball mill with the mixture B, adding a dispersing agent into the nano ball mill and performing ball grinding so as to obtain the nanometer silicon material, wherein the weight ratio of the dispersing agent to the mixture B is not more than 10%. The nanometer silicon material is for sale by being subjected to vacuum drying to form powder or being soaked by ethyl alcohol. The preparation method of the nanometer silicon material has the advantages of easiness and simplicity in operation, low cost, high efficiency, high safety and the like.
Description
Technical field
The preparation method of nano silicon material.
Background technology
Silicon has the theoretical specific capacity of up to 3000mAh/g as the negative material of lithium ion battery, and silicon is generally considered the lithium ion battery negative material of new generation substituting graphite.But when silicon is as the negative material of lithium ion battery, battery exists bigger bulk effect in charge and discharge process, being easily caused silicon materials efflorescence and lost efficacy, silicon is poor as the cyclical stability of the negative material of lithium ion battery.And the nanorize of silicon advantageously reduces bulk effect, improve the impact of cyclical stability of battery it is considered to be realize the business-like important channel of silicium cathode material.It addition, nano silicon material is widely used in the fields such as photovoltaic solar cell.
At present, prepare nano-silicon raw powder's production technology mainly use the siliceous Organic substances such as silane are carried out chemical vapour deposition technique (CVD) reduction, it is low that the method prepares nano-silicon efficiency, easily produce the danger of blast, preparation cost is high, and product there will be the various form such as tubulose, graininess, as shown in Figure 1.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide the preparation method of a kind of nano silicon material, have simple to operation, low cost, efficiency is high, the feature that safety is high.
In order to achieve the above object, the present invention is achieved in that it is the preparation method of a kind of nano silicon material, it is characterised in that preparation method is as follows:
Step one
Being mixed and stirred for obtaining mixture by the industrial silica fume of d50 >=10 μm and dehydrated alcohol, the solid content of mixture is 10%-50%；
Step 2
With planetary ball mill, the mixture in step one is carried out corase grind 5-30 hour, the mixture A after being roughly ground；The ratio of grinding media to material of planetary ball mill is 5:1-20:1, and the sphere diameter in planetary ball mill is the zirconia ball less than 5mm ± 10%, and the rotating speed of planetary ball mill is 200-400 rev/min；
Step 3
After ball milling terminates, the mixture A obtained by step 2 is taken out and the solid content of test mixing thing A, supplements dehydrated alcohol and the solid content of mixture A is adjusted to 1%-20%, obtain mixture B；
Step 4
Mixture B obtained by step 3 is loaded in nanon ball-mill and adds dispersant, the weight of dispersant is less than or equal to 10% with the weight ratio of mixture B, then ball milling is carried out 5-60 hour, ball milling obtains nano silicon material after terminating, nano silicon material vacuum drying powdering is sold, or sells by the form of soak with ethanol；The ratio of grinding media to material of nanon ball-mill is 2:1-5:1, and the sphere diameter of nanon ball-mill is the zirconia ball less than 0.1mm ± 10%, and the rotating speed of nanon ball-mill is 800-1800 rev/min.
Described dispersant can be sodium tripolyphosphate, methyl anyl alcohol, sodium hexameta phosphate, sodium pyrophosphate, polyacrylamide, Polyethylene Glycol, Polyethylene Glycol to isooctyl phenyl ether, fatty acid polyethylene glycol ester, polyvinylpyrrolidone, polyacrylic acid, sodium polyacrylate, sodium lauryl sulphate, dodecyl sodium sulfate, Polyetherimide, polyethenoxy sorbitan monoester one or more.
Present invention advantage compared with prior art is: simply and easily operate, low cost, and efficiency is high, and safety is high.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of nano-silicon prepared by prior art；
Fig. 2 is the shape appearance figure of the nano-silicon of the embodiment of the present invention one；
Fig. 3 is the shape appearance figure of the nano-silicon of the embodiment of the present invention two；
Fig. 4 is the shape appearance figure of the nano-silicon of the embodiment of the present invention three；
Fig. 5 is the shape appearance figure of the nano-silicon of the embodiment of the present invention four；
Fig. 6 is the shape appearance figure of the nano-silicon of the embodiment of the present invention five.
Detailed description of the invention
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is described further.At this it should be noted that be adapted to assist in for the explanation of these embodiments and understand the present invention, but it is not intended that limitation of the invention.As long as just can be combined with each other additionally, technical characteristic involved in each embodiment of invention described below does not constitutes conflict each other.
Embodiment one
It is the preparation method of a kind of nano silicon material, and preparation method is as follows:
Step one
Being mixed and stirred for obtaining mixture by the industrial silica fume of d50 >=10 μm and dehydrated alcohol, the solid content of mixture is 50%；
Step 2
Carry out roughly grinding 30 hours by the mixture in step one with planetary ball mill, the mixture A after being roughly ground；The ratio of grinding media to material of planetary ball mill is 20:1, and the sphere diameter in planetary ball mill is the zirconia ball of 4.5mm, and the rotating speed of planetary ball mill is 400 revs/min；
Step 3
After ball milling terminates, the mixture A obtained by step 2 is taken out and the solid content of test mixing thing A, supplements dehydrated alcohol and the solid content of mixture A is adjusted to 20%, obtain mixture B；
Step 4
Mixture B obtained by step 3 is loaded in nanon ball-mill and adds fatty acid polyglycol second two
Alcohol ester, fatty acid polyethylene glycol ester is 10% with the mass ratio of mixture B, then carries out ball milling 25 hours, ball milling obtains nano silicon material after terminating, the particulate form of nano silicon material is as in figure 2 it is shown, sell nano silicon material vacuum drying powdering, or sells by the form of soak with ethanol；The ratio of grinding media to material of nanon ball-mill is 5:1, and the sphere diameter of nanon ball-mill is the zirconia ball less than 0.09mm, and the rotating speed of nanon ball-mill is 800 revs/min.
Embodiment two
It is the preparation method of a kind of nano silicon material, and preparation method is as follows:
Step one
Being mixed and stirred for obtaining mixture by the industrial silica fume of d50 >=10 μm and dehydrated alcohol, the solid content of mixture is 40%；
Step 2
Carry out roughly grinding 20 hours by the mixture in step one with planetary ball mill, the mixture A after being roughly ground；The ratio of grinding media to material of planetary ball mill is 15:1, and the sphere diameter in planetary ball mill is the zirconia ball less than 5mm, and the rotating speed of planetary ball mill is 350 revolutions per seconds；
Step 3
After ball milling terminates, the mixture A obtained by step 2 is taken out and the solid content of test mixing thing A, supplements dehydrated alcohol and the solid content of mixture A is adjusted to 15%, obtain mixture B；
Step 4
Mixture B obtained by step 3 is loaded in nanon ball-mill and adds lauryl sulphate acid
Sodium, is 8% with the mass ratio of mixture B, then carries out ball milling 30 hours, and ball milling obtains nano silicon material after terminating, and the particulate form of nano silicon material is as it is shown on figure 3, sell nano silicon material vacuum drying powdering, or sells by the form of soak with ethanol；The ratio of grinding media to material of nanon ball-mill is 3:1, and the sphere diameter of nanon ball-mill is the zirconia ball less than 0.1mm, and the rotating speed of nanon ball-mill is 1200 revs/min.
Embodiment three
It is the preparation method of a kind of nano silicon material, and preparation method is as follows:
Step one
Being mixed and stirred for obtaining mixture by the industrial silica fume of d50 >=10 μm and dehydrated alcohol, the solid content of mixture is 30%；
Step 2
Carry out roughly grinding 15 hours by the mixture in step one with planetary ball mill, the mixture A after being roughly ground；The ratio of grinding media to material of planetary ball mill is 10:1, and the sphere diameter in planetary ball mill is the zirconia ball less than 5mm ± 10%, and the rotating speed of planetary ball mill is 300 revs/min；
Step 3
After ball milling terminates, the mixture A obtained by step 2 is taken out and the solid content of test mixing thing A, supplements dehydrated alcohol and the solid content of mixture A is adjusted to 10%, obtain mixture B；
Step 4
Mixture B obtained by step 3 is loaded in nanon ball-mill and adds Polyetherimide, it is 5% with the mass ratio of mixture B, then ball milling is carried out 40 hours, ball milling obtains nano silicon material after terminating, the particulate form of nano silicon material is as shown in Figure 4, nano silicon material vacuum drying powdering is sold, or sells by the form of soak with ethanol；The ratio of grinding media to material of nanon ball-mill is 2:1, and the sphere diameter of nanon ball-mill is the zirconia ball less than 0.11mm, 1400 revs/min of nanon ball-mill.
Embodiment four
It is the preparation method of a kind of nano silicon material, and preparation method is as follows:
Step one
Being mixed and stirred for obtaining mixture by the industrial silica fume of d50 >=10 μm and dehydrated alcohol, the solid content of mixture is 20%；
Step 2
Carry out roughly grinding 10 hours by the mixture in step one with planetary ball mill, the mixture A after being roughly ground；The ratio of grinding media to material of planetary ball mill is 5:1, and the sphere diameter in planetary ball mill is the zirconia ball less than 5mm ± 10%, and the rotating speed of planetary ball mill is 250 revs/min；
Step 3
After ball milling terminates, the mixture A obtained by step 2 is taken out and the solid content of test mixing thing A, supplements dehydrated alcohol and the solid content of mixture A is adjusted to 5%, obtain mixture B；
Step 4
Mixture B obtained by step 3 is loaded in nanon ball-mill and adds dodecyl sodium sulfate and Polyethylene Glycol, wherein dodecyl sodium sulfate is 3% with the mass ratio of mixture B, poly-diethanol is 2% with the mass ratio of mixture B, then ball milling is carried out 40 hours, ball milling obtains nano silicon material after terminating, the particulate form of nano silicon material is as it is shown in figure 5, sell nano silicon material vacuum drying powdering, or sells by the form of soak with ethanol；The ratio of grinding media to material of nanon ball-mill is 2:1, and the sphere diameter of nanon ball-mill is the zirconia ball less than 0.11mm, 1600 revs/min of nanon ball-mill.
Embodiment five
It is the preparation method of a kind of nano silicon material, and preparation method is as follows:
Step one
Being mixed and stirred for obtaining mixture by the industrial silica fume of d50 >=10 μm and dehydrated alcohol, the solid content of mixture is 10%；
Step 2
Carry out roughly grinding 5 hours by the mixture in step one with planetary ball mill, the mixture A after being roughly ground；The ratio of grinding media to material of planetary ball mill is 5:1, and the sphere diameter in planetary ball mill is the zirconia ball less than 5mm ± 10%, and the rotating speed of planetary ball mill is 200 revs/min；
Step 3
After ball milling terminates, the mixture A obtained by step 2 is taken out and the solid content of test mixing thing A, supplements dehydrated alcohol and the solid content of mixture A is adjusted to 3%, obtain mixture B；
Step 4
Mixture B obtained by step 3 is loaded in nanon ball-mill and adds sodium lauryl sulphate, polyethenoxy sorbitan monoester and Polyethylene Glycol to isooctyl phenyl ether, it is respectively 1% with the mass ratio of mixture B, then ball milling is carried out 40 hours, ball milling obtains nano silicon material after terminating, the particulate form of nano silicon material is as shown in Figure 6, nano silicon material vacuum drying powdering is sold, or sells by the form of soak with ethanol；The ratio of grinding media to material of nanon ball-mill is 2:1, and the sphere diameter of nanon ball-mill is the zirconia ball less than 0.11mm, 1800 revs/min of nanon ball-mill.
Above in association with accompanying drawing, embodiments of the present invention are explained in detail, but the present invention is not limited to described embodiment.For the ordinary skill in the art, in the case of without departing from the principle of the present invention and objective, these embodiments are carried out multiple change, revises, replace and deform and still fall within the scope of the present invention.
Claims (2)
1. the preparation method of a nano silicon material, it is characterised in that preparation method is as follows:
Step one
Being mixed and stirred for obtaining mixture by the industrial silica fume of d50 >=10 μm and dehydrated alcohol, the solid content of mixture is 10%-50%；
Step 2
With planetary ball mill, the mixture in step one is carried out corase grind 5-30 hour, the mixture A after being roughly ground；The ratio of grinding media to material of planetary ball mill is 5:1-20:1, and the sphere diameter in planetary ball mill is the zirconia ball less than 5mm ± 10%, and the rotating speed of planetary ball mill is 200-400 rev/min；
Step 3
After ball milling terminates, the mixture A obtained by step 2 is taken out and the solid content of test mixing thing A, supplements dehydrated alcohol and the solid content of mixture A is adjusted to 1%-20%, obtain mixture B；
Step 4
Mixture B obtained by step 3 is loaded in nanon ball-mill and adds dispersant, the weight of dispersant is less than or equal to 10% with the weight ratio of mixture B, then ball milling is carried out 5-60 hour, ball milling obtains nano silicon material after terminating, nano silicon material vacuum drying powdering is sold, or sells by the form of soak with ethanol；The ratio of grinding media to material of nanon ball-mill is 2:1-5:1, and the sphere diameter of nanon ball-mill is the zirconia ball less than 0.1mm ± 10%, and the rotating speed of nanon ball-mill is 800-1800 rev/min.
The preparation method of nano silicon material the most according to claim 1, it is characterised in that described dispersant be sodium tripolyphosphate, methyl anyl alcohol, sodium hexameta phosphate, sodium pyrophosphate, polyacrylamide, Polyethylene Glycol, Polyethylene Glycol to isooctyl phenyl ether, fatty acid polyethylene glycol ester, polyvinylpyrrolidone, polyacrylic acid, sodium polyacrylate, sodium lauryl sulphate, dodecyl sodium sulfate, Polyetherimide, polyethenoxy sorbitan monoester one or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610050619.2A CN105712350A (en) | 2016-01-26 | 2016-01-26 | Preparation method of nanometer silicon material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610050619.2A CN105712350A (en) | 2016-01-26 | 2016-01-26 | Preparation method of nanometer silicon material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105712350A true CN105712350A (en) | 2016-06-29 |
Family
ID=56154104
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610050619.2A Pending CN105712350A (en) | 2016-01-26 | 2016-01-26 | Preparation method of nanometer silicon material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105712350A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021117567A1 (en) * | 2019-12-10 | 2021-06-17 | 三菱マテリアル株式会社 | Fine silicon particles and production method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979317A (en) * | 2010-10-09 | 2011-02-23 | 武汉理工大学 | Low-temperature ball milling preparation method for nano crystal silicon powder |
| US20110318250A1 (en) * | 2010-06-08 | 2011-12-29 | Kaner Richard B | Rapid solid-state metathesis routes to nanostructured silicon-germainum |
| CN102910630A (en) * | 2012-10-15 | 2013-02-06 | 江苏博迁光伏材料有限公司 | Production method of nano silicon powder |
| CN103466645A (en) * | 2013-09-27 | 2013-12-25 | 上海冠旗电子新材料股份有限公司 | Method for preparing nano-silica by wet grinding |
| CN103531761A (en) * | 2013-10-28 | 2014-01-22 | 上海利物盛企业集团有限公司 | Preparation method for nanometer silicon |
-
2016
- 2016-01-26 CN CN201610050619.2A patent/CN105712350A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110318250A1 (en) * | 2010-06-08 | 2011-12-29 | Kaner Richard B | Rapid solid-state metathesis routes to nanostructured silicon-germainum |
| CN101979317A (en) * | 2010-10-09 | 2011-02-23 | 武汉理工大学 | Low-temperature ball milling preparation method for nano crystal silicon powder |
| CN102910630A (en) * | 2012-10-15 | 2013-02-06 | 江苏博迁光伏材料有限公司 | Production method of nano silicon powder |
| CN103466645A (en) * | 2013-09-27 | 2013-12-25 | 上海冠旗电子新材料股份有限公司 | Method for preparing nano-silica by wet grinding |
| CN103531761A (en) * | 2013-10-28 | 2014-01-22 | 上海利物盛企业集团有限公司 | Preparation method for nanometer silicon |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021117567A1 (en) * | 2019-12-10 | 2021-06-17 | 三菱マテリアル株式会社 | Fine silicon particles and production method thereof |
| JP7396009B2 (en) | 2019-12-10 | 2023-12-12 | 三菱マテリアル株式会社 | Silicon fine particles and their manufacturing method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103618070B (en) | A kind of nano silicon-based composite negative pole material and preparation method | |
| CN103311522B (en) | A kind of silicon/carbon composite microsphere negative electrode material and its production and use | |
| CN103367726B (en) | Si-C composite material and preparation method thereof, lithium ion battery | |
| CN105060281A (en) | Nano-graphite slurry preparation method | |
| CN110137466B (en) | Preparation method of silicon carbon-carbon nanotube composite microsphere negative electrode material of lithium ion battery | |
| CN102983313B (en) | Si-C composite material and preparation method thereof, lithium ion battery | |
| CN107634208A (en) | A kind of preparation method of lithium ion battery silicon-carbon cathode material | |
| CN105375030B (en) | A kind of preparation method of low temperature high multiplying power electrokinetic cell graphite cathode material | |
| CN103633295A (en) | Silicon-carbon composite material, lithium ion battery, and preparation method and application of silicon-carbon composite material | |
| CN107799728A (en) | A kind of hollow Si-C composite material for lithium ion battery and preparation method thereof | |
| CN108281634A (en) | A kind of method and its application of graphene coated graphite negative material of lithium ion battery | |
| CN104124437B (en) | Iron phosphate compound anode material of lithium of Surface coating titanium nitride and Graphene and its preparation method and application | |
| CN104393266B (en) | A kind of silico-carbo combination electrode material of nucleocapsid structure and preparation method thereof | |
| CN105655570A (en) | Refining preparation method of nanoscale silicon powder material | |
| CN105185964B (en) | A kind of Si/TiO of more ball packed structures2Composite material and preparation method | |
| CN111180719A (en) | Method for preparing nano silicon by three-stage grinding | |
| CN110148743A (en) | A kind of silicon-carbon composite cathode material and preparation method thereof and lithium ion battery | |
| CN106374085A (en) | Lithium ion battery material preparation method | |
| CN103236517A (en) | Lithium ion battery silicon-based negative material and preparation method thereof | |
| CN110104652A (en) | A kind of ball-milling preparation method of nano silica fume | |
| CN103531761A (en) | Preparation method for nanometer silicon | |
| CN105789564B (en) | A kind of Fe for lithium ion battery negative material3O4/ C composite and its preparation method and application | |
| CN109273700A (en) | A kind of silicon based composite material and its preparation method and application | |
| CN107706397A (en) | Nickel-cobalt-manganese ternary combination electrode material of modified carbon nano-tube modification and preparation method thereof | |
| CN101853939B (en) | Cathodic active material as well as preparation method and battery thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160629 |
|
| RJ01 | Rejection of invention patent application after publication |