CN108101061A - The preparation method of nano silica fume - Google Patents
The preparation method of nano silica fume Download PDFInfo
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- CN108101061A CN108101061A CN201711172592.5A CN201711172592A CN108101061A CN 108101061 A CN108101061 A CN 108101061A CN 201711172592 A CN201711172592 A CN 201711172592A CN 108101061 A CN108101061 A CN 108101061A
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- Prior art keywords
- silica fume
- nano silica
- preparation
- silane
- silicon nanoparticle
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- 229910021487 silica fume Inorganic materials 0.000 title claims description 26
- 238000002360 preparation method Methods 0.000 title claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 13
- 229910000077 silane Inorganic materials 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000006911 nucleation Effects 0.000 claims description 2
- 238000010899 nucleation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910008045 Si-Si Inorganic materials 0.000 description 1
- 229910006411 Si—Si Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- -1 start flowmeter 60 Substances 0.000 description 1
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
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/029—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to material chemistry technical fields, and in particular to a kind of preparation method of nano silica fume；Include the following steps：(1) silane is introduced into plasma generator, is decomposed through ionization, nucleation obtains silicon nanoparticle again；(2) silicon nanoparticle obtains nano silica fume after gas solid separation and cooling；Above steps carries out in a nitrogen environment；Preparation method provided by the invention is simple, superior product quality, and production cost is low.
Description
Technical field
The invention belongs to material chemistry technical fields, and in particular to a kind of preparation method of nano silica fume.
Background technology
Nano silica fume is a kind of semiconductor material for being widely used in the fields such as microelectronics, electrode material and solar cell
Material, has that surface area is big, high surface, the performance advantages such as apparent density is low.It is presently used for preparing the common side of nano silica fume
Method has mechanical attrition method, plasma evaporation condensation method and chemical vapour deposition technique.Wherein, mechanical attrition method is relatively simple, cost
It is low but low there are product purity, the shortcomings of crystal defect is more, and time-consuming, and distribution of particles is uneven.Plasma evaporation condensation method is former
Expect that price is low, without post processing, but the quality of product is influenced big be subject to material quality, and is difficult to ensure that yield and product are pure
Degree.The reaction mechanism of chemical vapour deposition technique is not clear and definite enough, and reaction safety has to be solved, and products obtained therefrom shape is mostly without fixed
Type.
The content of the invention
It is an object of the invention to provide a kind of methods of preparation of industrialization high quality nano silica flour.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of nano silica fume, includes the following steps：
(1) silane is introduced into plasma generator, is decomposed through ionization, nucleation obtains silicon nanoparticle again；
(2) silicon nanoparticle obtains nano silica fume after gas solid separation and cooling；
Above steps carries out in a nitrogen environment.
The advantageous effect that above-mentioned technical proposal generates is：Using the silane of high-purity as raw material, the high-purity of product ensure that
Degree.From raw material to product, centre pertains only to ionize, is nucleated and the processes such as gas solid separation, and raw material need not be cleaned and pre-treatment,
Catalyst and other raw materials need not be added in during simultaneous reactions, method is simple, suitable for industrialized production, to environment without dirt
Dye.The intensity of Si-H and Si-Si bond is relatively low in silane, and using nitrogen as the working gas of plasma arc, the energy of acquisition is real enough
The ionization and decomposition of existing silane, therefore production cost can be reduced while product quality is ensured.From the point of view of scanning electron microscope (SEM) photograph, production
The lattice of product is completely regular.
Description of the drawings
Fig. 1 is the structure diagram of preparation system of the present invention；
Fig. 2 is the XRD diagram of nano silica fume made from embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of nano silica fume made from embodiment 1；
Fig. 4 is the XRD diagram of nano silica fume made from embodiment 2；
Fig. 5 is the scanning electron microscope (SEM) photograph of nano silica fume made from embodiment 2；
Fig. 6 is the XRD diagram of nano silica fume made from embodiment 3；
Fig. 7 is the scanning electron microscope (SEM) photograph of nano silica fume made from embodiment 3.
Specific embodiment
1-3 is further described technical solution disclosed by the invention with reference to embodiments.
In following embodiment, as shown in Figure 1：The preparation system of nano silica fume includes the plasma generator of sequential communication
10, separator 20, cooling system 30 traps tower 40 and powder collector 50.Nitrogen source gases and silane source of the gas by flowmeter 60 with etc.
The inlet end of plasma generator 10 is connected, and the outlet side of plasma generator 10 is connected with separator 20.
Embodiment 1：The preparation of nano silica fume
(1) entire preparation system is vacuumized, at the same add in nitrogen be rinsed with protection until entire preparation system all
For nitrogen environment；
(2) start plasma generator 10, adjust to air pressure be 0.3MPa, operating voltage 300V, work
Make electric current as 300A, working flow 70m3/h；
(3) using the silane that purity is 99.99% as raw material, start flowmeter 60, raw material is made to be worn with the feed rate of 5kg/h
Cross plasma arc and enter plasma generator 10, under action of plasma, silane rapidly ionization be decomposed to form silicon ion with
Hydrogen ion, silicon ion recombine into karyomorphism into silicon nanoparticle again；
(4) under stream of nitrogen gas drive, silicon nanoparticle, which enters, carries out gas solid separation in separator, the gas isolated leads to
It crosses emptying after filter or recycles, silicon nanoparticle is then under the drive of stream of nitrogen gas, into cooling system, after cooling
Into trapping tower, under the effect of gravity, it is deposited in powder collector；
(5) stopping being passed through silane, plasma generator 10 continues to run with 60 minutes to ensure that the reaction was complete, closes power supply,
It opens powder collector and can obtain nano silica fume.
The obtained nano silica fume of the present embodiment is brownish-yellow powder, through X-ray diffraction analysis, obtains XDR figures such as Fig. 2 institutes
Show, test value is as shown in table 1：
Table 1：
| 2-Theta | 28.53 | 47.33 | 56.22 |
| Intensity | 3668 | 1348 | 908 |
Through electron-microscope scanning, as shown in figure 3, average grain diameter is 67nm, specific surface area 89.5m2/g。
Embodiment 2：The preparation of nano silica fume
It is prepared by the preparation method according to embodiment 1, unlike, step (2) the plasma generator 10
Air pressure be 0.4MPa, operating voltage 300V, operating current 350A, working flow 75m3/h；Step (3)
The feeding speed of middle raw material silane is 7kg/h；The time that plasma generator 10 continues to run in step (5) is 70 minutes.
The obtained nano silica fume of the present embodiment is brownish-yellow powder, through X-ray diffraction analysis, obtains XDR figures such as Fig. 4 institutes
Show, test value is as shown in table 2：
Table 2：
| 2-Theta | 28.56 | 47.42 | 56.24 |
| Intensity | 35400 | 18880 | 9880 |
Through electron-microscope scanning, as shown in figure 5, average grain diameter is 84nm, specific surface area 78.1m2/g。
Embodiment 3：The preparation of nano silica fume
It is prepared by the preparation method according to embodiment 1, unlike, step (2) the plasma generator 10
Air pressure 0.5MPa, operating voltage 350V, operating current 350A, working flow 80m3/h；In step (3)
The feeding speed of raw material silane is 10kg/h；The time that plasma generator 10 continues to run in step (5) is 90 minutes.
The obtained nano silica fume of the present embodiment is brownish-yellow powder, through X-ray diffraction analysis, obtains XDR figures such as Fig. 6 institutes
Show, test value is as shown in table 3：
Table 3：
| 2-Theta | 28.60 | 47.48 | 56.30 |
| Intensity | 5413 | 2260 | 1066.67 |
Through electron-microscope scanning, as shown in fig. 7, average grain diameter is 93nm, specific surface area 65.7m2/g。
Claims (4)
1. a kind of preparation method of nano silica fume, it is characterised in that：Include the following steps：
(1) silane is introduced into plasma generator, is decomposed through ionization, nucleation obtains silicon nanoparticle again；
(2) silicon nanoparticle obtains nano silica fume after gas solid separation and cooling；
Above steps carries out in a nitrogen environment.
2. the preparation method of nano silica fume according to claim 1, it is characterised in that：Plasma is sent out in the step (1)
The operating voltage of raw device is 300-350V, operating current 300-350A, operating pressure 0.3-0.5MPa.
3. the preparation method of nano silica fume according to claim 1, it is characterised in that：Silane is pure in the step (1)
It spends for 99.99%.
4. the preparation method of nano silica fume according to claim 1, it is characterised in that：In the step (1) silane into
Material speed is 5kg/h-10kg/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711172592.5A CN108101061A (en) | 2017-11-22 | 2017-11-22 | The preparation method of nano silica fume |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711172592.5A CN108101061A (en) | 2017-11-22 | 2017-11-22 | The preparation method of nano silica fume |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108101061A true CN108101061A (en) | 2018-06-01 |
Family
ID=62206537
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711172592.5A Pending CN108101061A (en) | 2017-11-22 | 2017-11-22 | The preparation method of nano silica fume |
Country Status (1)
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| CN (1) | CN108101061A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607545A (en) * | 2019-01-02 | 2019-04-12 | 河南硅烷科技发展股份有限公司 | A kind of high purity silane CVD method continuously prepares the industrial method of nano silica fume |
| CN110492091A (en) * | 2019-07-01 | 2019-11-22 | 徐州硕祥信息科技有限公司 | A kind of lithium battery production negative electrode material and preparation method thereof |
| CN111261864A (en) * | 2020-02-10 | 2020-06-09 | 马鞍山科达普锐能源科技有限公司 | Silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
| CN114031082A (en) * | 2021-12-22 | 2022-02-11 | 中国有色桂林矿产地质研究院有限公司 | A method for preparing nano-silicon powder by induction plasma pyrolysis of silane |
| CN116282034A (en) * | 2023-02-24 | 2023-06-23 | 江苏鑫华半导体科技股份有限公司 | Nano-silicon and its preparation method and lithium-ion battery negative electrode material |
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2017
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607545A (en) * | 2019-01-02 | 2019-04-12 | 河南硅烷科技发展股份有限公司 | A kind of high purity silane CVD method continuously prepares the industrial method of nano silica fume |
| CN110492091A (en) * | 2019-07-01 | 2019-11-22 | 徐州硕祥信息科技有限公司 | A kind of lithium battery production negative electrode material and preparation method thereof |
| CN111261864A (en) * | 2020-02-10 | 2020-06-09 | 马鞍山科达普锐能源科技有限公司 | Silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
| CN114031082A (en) * | 2021-12-22 | 2022-02-11 | 中国有色桂林矿产地质研究院有限公司 | A method for preparing nano-silicon powder by induction plasma pyrolysis of silane |
| WO2023115762A1 (en) * | 2021-12-22 | 2023-06-29 | 中国有色桂林矿产地质研究院有限公司 | Method for preparing nano silicon powder by means of pyrolysis of silane with inductive plasma |
| CN114031082B (en) * | 2021-12-22 | 2023-10-31 | 中国有色桂林矿产地质研究院有限公司 | A method for preparing nanosilica powder by induction plasma pyrolysis of silane |
| CN116282034A (en) * | 2023-02-24 | 2023-06-23 | 江苏鑫华半导体科技股份有限公司 | Nano-silicon and its preparation method and lithium-ion battery negative electrode material |
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Application publication date: 20180601 |
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