CN107285322A - A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder - Google Patents
A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder Download PDFInfo
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- CN107285322A CN107285322A CN201710525404.6A CN201710525404A CN107285322A CN 107285322 A CN107285322 A CN 107285322A CN 201710525404 A CN201710525404 A CN 201710525404A CN 107285322 A CN107285322 A CN 107285322A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Silicon Compounds (AREA)
Abstract
The method for preparing sub- nanometer spherical silicon powder, including silica flour grinding, screening, pre-reaction, reaction, cooling step are improved the invention discloses a kind of plasma.Wherein silica flour grinding lapping liquid and abrasive disk are operated, the silica flour screening certain particle size scope ground, silica flour enters plasma reactor, vacuumize, first preheat at a lower temperature, temperature programming again after applying argon gas, insulation is melted after heating, oxygen is filled with rapidly, product powder is collected in then rapid cooling.Present invention process is flexible, obtained silicon powder good sphericity, Subnano-class granularity, and is evenly distributed, and product quality reaches world lead level.
Description
Technical field
Improve the present invention relates to technical field of nano material, more particularly to a kind of plasma and prepare sub- nanometer spherical silicon powder
Method.
Background technology
Silicon powder is just made for after carrying out mechanical crushing processing with quartz mine.It is divided into again：Melt silicon powder and silicon metal
Micro mist.Subnano-class ball-shaped silicon micro powder refers to：Particle diameter is between 30~900nm.Due to nanometer（1~20nm）Silicon powder（Conductor）
With silicon powder（Insulator）Surface physical and chemical performance it is entirely different, so application field is also different.Because ball-shaped silicon micro powder is different
In angle powder shape silicon powder, its good fluidity is small to object table bulk damage, and has valency again relative to thinner nano silicon micronization
Lattice cost advantage.Therefore sub-nano silica micro mist is widely used in plastic packaging material, organosilicon, coating, ink, high-grade plastics, material for repairing etc.
Field.
Preparing the method for sub- nanometer spherical silicon powder at present has the methods such as plasma method, high-temperature combustion method, arc process.Deng
Processes are the high temperature thermal fields using plasma, angular silicon powder is melted in high temperature thermal field space, at the same using
Surface tension during liquid, rush form it into it is spherical, and in instantaneous cooling so as to as spherical shape.High-temperature combustion method is to utilize second
Alkynes or liquefied petroleum gas, oxygen and silica flour, are reacted in combustion chamber, and form spherical powder in high temperature thermal field space.Electricity
Arc method is the high arc temperature that produces when utilizing positive or negative high voltage discharge of electricity, in high arc temperature interval by angular silicon powder, make its
Moment melts to form spherical powder.These current methods still in improvement, sphericity and particle diameter distribution be it is most important be also quite to be difficult to
The performance indications of revolution.
The content of the invention
The method for preparing sub- nanometer spherical silicon powder is improved it is an object of the invention to provide a kind of plasma, to improve work
Skill, enable it is simple efficiently and the sphericity and particle diameter of silicon powder can be strengthened narrow, asked with overcoming present in prior art
Topic.
In order to realize the above object the technical scheme is that：
A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder, comprises the steps of：
（1）, silica flour grinding：High-purity silica flour is chosen, lapping liquid is immersed, 2.5 ~ 4h is ground in special abrasive disk, obtains thin silicon
Powder, thoroughly cleaning removes lapping liquid；
（2）, screening：Multistage screen tray sieves fine silica powder, chooses the fine silica powder of 50-300 mesh, inserts in plasma reactor；
（3）, pre-reaction：Plasma reactor is evacuated to 1 ~ 3Pa, is electrically heated to 300 ~ 525 DEG C, keeps 10 ~ 15min；
（4）Reaction：Be filled with argon gas to plasma reactor, plasma reactor first with 15 ~ 20 DEG C/min, again with 7.5 ~ 12 DEG C/
It is 2.4 ~ 7.0MPa that min, the last speed with 3 ~ 5 DEG C/min, which are warming up to gross pressure after 1420-1470 DEG C, heating, treats fine silica powder
Melting, keeps 3 ~ 12min, oxygen is then filled with rapidly；
（5）, cooling：It is filled with the melting fine silica powder after oxygen and rapidly becomes silica micronic dust, quenching is brought into blower unit
Device is cooled down, and forms spherical particle, with cloth bag, whirlwind or electrostatic precipitation, obtains high-purity, sub- nanometer spherical silicon powder.
Preferably, step（2）In, the silicon particle size scope of screening is 70-250 mesh.Granulate scope is beneficial to reaction
Optimization.
Preferably, step（4）In, final temperature is 1446 ~ 1452 DEG C after heating.Refining temperature scope makes to be more easy to refinement
Silicon powder particle.
Preferably, step（3）In, it is 7.5 ~ 18% that oxygen, which is filled with and finishes the volume fraction of moment,.Partial pressure of oxygen control reaction
Speed.
Preferably, having magnetic force adjusting in the plasma reactor.Magnetic force adjusting passes through magnetic force adjustment
Surface tension.
The beneficial effects of the present invention are：Step of the present invention is clear, and silicon powder quality is high.Sieve the silica flour of certain particle size again
The controlling and stability of the reaction of increased response；Pre-reaction acts on crucial to the lattice transformation in silica flour；The control of reaction condition
System and the type of cooling have the distinctive feature of design, take full advantage of the special nature of nano material preparation.Present invention process is flexible,
Obtained silicon powder good sphericity, Subnano-class granularity, and be evenly distributed, product quality reaches world lead level.
Brief description of the drawings
Fig. 1 is the electron microscope image that sub- nanometer spherical silicon powder is made in the embodiment of the present invention 1.
Embodiment
In order to illustrate more clearly of the embodiment of the present application or technical scheme of the prior art, letter will be made to embodiment below
Singly introduce.
Embodiment 1
A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder, comprises the steps of：
（1）, silica flour grinding：High-purity silica flour is chosen, lapping liquid is immersed, 2.5 ~ 4h is ground in special abrasive disk, obtains thin silicon
Powder, thoroughly cleaning removes lapping liquid；
（2）, screening：Multistage screen tray sieves fine silica powder, chooses the fine silica powder of 50-300 mesh, inserts in plasma reactor；
（3）, pre-reaction：Plasma reactor is evacuated to 1 ~ 3Pa, is electrically heated to 300 DEG C, keeps 10 ~ 15min；
（4）Reaction：Be filled with argon gas to plasma reactor, plasma reactor first with 15 ~ 20 DEG C/min, again with 7.5 ~ 12 DEG C/
Min, 1450 DEG C finally are warming up to 3 ~ 5 DEG C/min speed, gross pressure is 6.3-7.0MPa after heating, opens plasma reaction
The magnetic force adjusting having in stove, regulation magnetic force treats that fine silica powder is melted, keeps 3 ~ 12min, then fill rapidly to proper range
Enter oxygen；
（5）, cooling：It is filled with the melting fine silica powder after oxygen and rapidly becomes silica micronic dust, quenching is brought into blower unit
Device is cooled down, and forms spherical particle, with cloth bag, whirlwind or electrostatic precipitation, obtains high-purity, sub- nanometer spherical silicon powder.
Preferably, step（2）In, the silicon particle size scope of screening is 70-250 mesh；Step（3）In, oxygen, which is filled with, to be finished
The volume fraction of moment is 7.5-9%.
Embodiment 2
A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder, comprises the steps of：
（1）, silica flour grinding：High-purity silica flour is chosen, lapping liquid is immersed, 2.5 ~ 4h is ground in special abrasive disk, obtains thin silicon
Powder, thoroughly cleaning removes lapping liquid；
（2）, screening：Multistage screen tray sieves fine silica powder, chooses the fine silica powder of 50-300 mesh, inserts in plasma reactor；
（3）, pre-reaction：Plasma reactor is evacuated to 1 ~ 3Pa, is electrically heated to 410 DEG C, keeps 10 ~ 15min；
（4）Reaction：Be filled with argon gas to plasma reactor, plasma reactor first with 15 ~ 20 DEG C/min, again with 7.5 ~ 12 DEG C/
Min, 1470 DEG C finally are warming up to 3 ~ 5 DEG C/min speed, gross pressure is 5.2MPa after heating, is opened in plasma reactor
The magnetic force adjusting having, regulation magnetic force treats that fine silica powder is melted, keeps 3 ~ 12min, oxygen is then filled with rapidly to proper range
Gas；
（5）, cooling：It is filled with the melting fine silica powder after oxygen and rapidly becomes silica micronic dust, quenching is brought into blower unit
Device is cooled down, and forms spherical particle, with cloth bag, whirlwind or electrostatic precipitation, obtains high-purity, sub- nanometer spherical silicon powder.
Preferably, step（2）In, the silicon particle size scope of screening is 70-250 mesh；Step（3）In, oxygen, which is filled with, to be finished
The volume fraction of moment is 11-12%.
Embodiment 3
A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder, comprises the steps of：
（1）, silica flour grinding：High-purity silica flour is chosen, lapping liquid is immersed, 2.5 ~ 4h is ground in special abrasive disk, obtains thin silicon
Powder, thoroughly cleaning removes lapping liquid；
（2）, screening：Multistage screen tray sieves fine silica powder, chooses the fine silica powder of 50-300 mesh, inserts in plasma reactor；
（3）, pre-reaction：Plasma reactor is evacuated to 1 ~ 3Pa, is electrically heated to 525 DEG C, keeps 10 ~ 15min；
（4）Reaction：Be filled with argon gas to plasma reactor, plasma reactor first with 15 ~ 20 DEG C/min, again with 7.5 ~ 12 DEG C/
Min, 1420 DEG C finally are warming up to 3 ~ 5 DEG C/min speed, gross pressure is 2.4MPa after heating, is opened in plasma reactor
The magnetic force adjusting having, regulation magnetic force treats that fine silica powder is melted, keeps 3 ~ 12min, oxygen is then filled with rapidly to proper range
Gas；
（5）, cooling：It is filled with the melting fine silica powder after oxygen and rapidly becomes silica micronic dust, quenching is brought into blower unit
Device is cooled down, and forms spherical particle, with cloth bag, whirlwind or electrostatic precipitation, obtains high-purity, sub- nanometer spherical silicon powder.
Preferably, step（2）In, the silicon particle size scope of screening is 70-250 mesh；Step（3）In, oxygen, which is filled with, to be finished
The volume fraction of moment is 18%.
Experimental result：Product master drawing is shown in Fig. 1, parameter made from the embodiment of the present invention 1：HITACHI electron microscopes, amplification
30000 times.Particle mean size 390nm, specific surface area 23.7m2/ g, μ s/cm, the U contents 0.1ppb of electrical conductivity 2.
Above example is only to illustrate the preferred technical solution of the present invention, it is noted that for the general of the art
For logical technical staff, under the premise without departing from the principles of the invention, some improvement made or equivalent substitution are accordingly to be regarded as this
The protection domain of invention, should cover in scope of the presently claimed invention.
Claims (5)
1. a kind of plasma improves the method for preparing sub- nanometer spherical silicon powder, it is characterised in that comprise the following steps：
（1）, silica flour grinding：High-purity silica flour is chosen, lapping liquid is immersed, 2.5 ~ 4h is ground in abrasive disk, obtains fine silica powder, thoroughly
Cleaning removes lapping liquid；
（2）, screening：Multistage screen tray sieves fine silica powder, chooses the fine silica powder of 50-300 mesh, inserts in plasma reactor；
（3）, pre-reaction：Plasma reactor is evacuated to 1 ~ 3Pa, is electrically heated to 300 ~ 525 DEG C, keeps 10 ~ 15min；
（4）, reaction：Be filled with argon gas to plasma reactor, plasma reactor first with 15 ~ 20 DEG C/min, again with 7.5 ~ 12 DEG C/
It is 2.4 ~ 7.0MPa that min, the last speed with 3 ~ 5 DEG C/min, which are warming up to gross pressure after 1420-1470 DEG C, heating, treats fine silica powder
Melting, keeps 3 ~ 12min, oxygen is then filled with rapidly；
（5）, cooling：It is filled with the melting fine silica powder after oxygen and rapidly becomes silica micronic dust, quenching is brought into blower unit
Device is cooled down, and forms spherical particle, with cloth bag, whirlwind or electrostatic precipitation, obtains high-purity, sub- nanometer spherical silicon powder.
2. a kind of plasma according to claim 1 improves the method for preparing sub- nanometer spherical silicon powder, it is characterised in that
Step（2）In, the silicon particle size scope of screening is 70-250 mesh.
3. a kind of plasma according to claim 1 improves the method for preparing sub- nanometer spherical silicon powder, it is characterised in that
Step（4）In, final temperature is 1446 ~ 1452 DEG C after heating.
4. a kind of plasma according to claim 1 improves the method for preparing sub- nanometer spherical silicon powder, it is characterised in that
Step（3）In, it is 7.5 ~ 18% that oxygen, which is filled with and finishes the volume fraction of moment,.
5. a kind of plasma according to claim 1 improves the method for preparing sub- nanometer spherical silicon powder, it is characterised in that
There is magnetic force adjusting in the plasma reactor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710525404.6A CN107285322A (en) | 2017-06-30 | 2017-06-30 | A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder |
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| CN201710525404.6A CN107285322A (en) | 2017-06-30 | 2017-06-30 | A kind of plasma improves the method for preparing sub- nanometer spherical silicon powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423686A (en) * | 2018-03-08 | 2018-08-21 | 苏州硅纳电子基材有限公司 | A kind of preparation method of high-purity sub-nanometer grade spherical silicon micropowder |
| CN112299420A (en) * | 2020-06-12 | 2021-02-02 | 将乐三晶新材料有限公司 | Process for preparing spherical metal silicon powder by using plasma flame gun |
| CN112573910A (en) * | 2020-12-16 | 2021-03-30 | 徐州亚苏尔高新材料有限公司 | Wear-resistant quartz ceramic material and preparation method thereof |
| CN112811889A (en) * | 2021-03-02 | 2021-05-18 | 徐州亚苏尔高新材料有限公司 | Wear-resistant ceramic roller and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0492810A (en) * | 1990-08-08 | 1992-03-25 | I S I:Kk | Production of superfine spherule of anhydrous silica free from silanol group and disperesed composition thereof |
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2017
- 2017-06-30 CN CN201710525404.6A patent/CN107285322A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0492810A (en) * | 1990-08-08 | 1992-03-25 | I S I:Kk | Production of superfine spherule of anhydrous silica free from silanol group and disperesed composition thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王翔 等: "高频等离子法制备球形硅微粉的工艺研究", 《科技资讯》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423686A (en) * | 2018-03-08 | 2018-08-21 | 苏州硅纳电子基材有限公司 | A kind of preparation method of high-purity sub-nanometer grade spherical silicon micropowder |
| CN112299420A (en) * | 2020-06-12 | 2021-02-02 | 将乐三晶新材料有限公司 | Process for preparing spherical metal silicon powder by using plasma flame gun |
| CN112573910A (en) * | 2020-12-16 | 2021-03-30 | 徐州亚苏尔高新材料有限公司 | Wear-resistant quartz ceramic material and preparation method thereof |
| CN112811889A (en) * | 2021-03-02 | 2021-05-18 | 徐州亚苏尔高新材料有限公司 | Wear-resistant ceramic roller and preparation method thereof |
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