CN107473228A - A kind of nanoscale crystalline silicon and preparation method thereof - Google Patents
A kind of nanoscale crystalline silicon and preparation method thereof Download PDFInfo
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- CN107473228A CN107473228A CN201710947779.1A CN201710947779A CN107473228A CN 107473228 A CN107473228 A CN 107473228A CN 201710947779 A CN201710947779 A CN 201710947779A CN 107473228 A CN107473228 A CN 107473228A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
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- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
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Abstract
The present invention relates to crystalline silicon preparing technical field, discloses a kind of nanoscale crystalline silicon and preparation method thereof.The preparation method of nanoscale crystalline silicon includes the silicon-containing gas mixing hydrogen such as chlorosilane, silane being passed into plasma generator, mixed gas is set to form plasma using the electromagnetic field of plasma generator, it has higher activity and reacted, and nano level silicon grain is produced in plasma generator.Nanoscale crystalline silicon is prepared using this method, because silicon grain is directly to be generated by the reactant reaction of plasma state, without the process such as broken, course of reaction is in plasma generator, so being not likely to produce dust, is not easy to introduce impurity.The nanoscale crystalline silicon purity produced is high, high income, and lattice defect is few, superior performance.
Description
Technical field
The present invention relates to a kind of crystalline silicon preparing technical field, and more particularly to a kind of nanoscale crystalline silicon and its preparation side
Method.
Background technology
Nanocrystalline silicon is photoelectric semiconductor material of new generation, be with wider gap can semiconductor, and Gao Gong
Rate source material.Nanocrystalline silicon have crystal structure it is complete, without lattice defect, without it is broken, purity is high, particle diameter is small, compares table
The features such as area is big, high surface, low apparent density.Nanocrystalline silicon is applied to photovoltaic industry, can effectively improve photoelectricity
Transformation efficiency.Nanocrystalline silicon is used in microelectronic industry, can effectively reduce cost, increases the electronic component life-span.
By taking microelectronic industry nanocrystalline silicon as an example, prior art is to prepare symbol by broken block polycrystalline silicon material
The crystal silicon particle of desired Nano grade is closed, the nanoscale crystalline silicon, which crushes technology of preparing, to be had introducing impurity, produce silicon
Dust, cause crystal structure defects, the problem of yield is low.
The content of the invention
It is an object of the invention to provide a kind of preparation method of nanoscale crystalline silicon, the method is not easily introduced impurity, no
Silica soot is also easy to produce, and the high income of crystalline silicon, purity are high, lattice defect is few.
Another object of the present invention is to provide a kind of nanoscale crystalline silicon, its crystal structure is complete, has less crystalline substance
Lattice defect, purity are high.
The present invention is solved its technical problem and realized using following technical scheme.
A kind of preparation method of nanoscale crystalline silicon, it includes：
Reactions steps：Silicon-containing gas and hydrogen are together formed into plasma simultaneously under the electromagnetic field of plasma generator
Reaction, produce nanoscalar silicon particles and tail gas；Silicon-containing gas include at least one of chlorosilane gas, silane gas.
In an embodiment of the present invention, the chlorosilane in the preparation method of above-mentioned nanoscale crystalline silicon is silicon tetrachloride
(SiCl4), trichlorosilane (SiHCl3), dichlorosilane (SiH2Cl2), the hydrogen silicon (SiH of a chlorine three3Cl it is one or more in)
Mixture；Silane is silicon tetrahydride (SiH4)。
In an embodiment of the present invention, the silicon-containing gas in the preparation method of above-mentioned nanoscale crystalline silicon and hydrogen
It is 1 to mix mol ratio:1~1:25.
In an embodiment of the present invention, the silicon-containing gas in the preparation method of above-mentioned nanoscale crystalline silicon and hydrogen
It is 1 to mix mol ratio:5~1:20.
In an embodiment of the present invention, the silicon-containing gas in the preparation method of above-mentioned nanoscale crystalline silicon and hydrogen
It is 1 to mix mol ratio:10~1:15.
In an embodiment of the present invention, plasma generator in the preparation method of above-mentioned nanoscale crystalline silicon
Electrode uses dielectric barrier discharge, and dielectric is high-purity ceramic material.
In an embodiment of the present invention, the preparation method of above-mentioned nanoscale crystalline silicon also includes：
Collection step：Nanoscalar silicon particles are separated with the tail gas of reactions steps under electrostatic field environment.
In an embodiment of the present invention, the plasma producing apparatus in the preparation method of above-mentioned nanoscale crystalline silicon
Offgas outlet downstream be provided with electrostatic adsorption device, electrostatic field of the tail gas with nanoscalar silicon particles in electrostatic adsorption device is made
With lower separation.
In an embodiment of the present invention, the circulation of tail gas in the preparation method of above-mentioned nanoscale crystalline silicon is to plasma
Reused in body generator.
The present invention also provides a kind of nanoscale crystalline silicon, and it is made by the preparation method of above-mentioned nanoscale crystalline silicon.
The beneficial effect of the nanoscale crystalline silicon of the embodiment of the present invention and preparation method thereof is：
The preparation method of nanoscale crystalline silicon includes the silicon-containing gas mixing hydrogen such as chlorosilane, silane being passed into plasma
In body generator, mixed gas is set to form plasma using the electromagnetic field of plasma generator, it has higher activity
And react, nano level silicon grain is produced in plasma generator.Nanoscale crystalline silicon is prepared using this method, due to
Silicon grain is directly to be generated by the reactant reaction of plasma state, and without the process such as broken, course of reaction is sent out in plasma
In raw device, so being not likely to produce dust, it is not easy to introduce impurity.The nanoscale crystalline silicon purity produced is high, high income, lattice
Defect is few, superior performance.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional production that can be obtained by commercially available purchase
Product.
Nanoscale crystalline silicon of the embodiment of the present invention and preparation method thereof is specifically described below.
The preparation method of the nanoscale crystalline silicon of the present invention includes：
First, reactions steps
By silicon-containing gas and hydrogen according to 1:1~1:25 mixed in molar ratio.The silicon-containing gas are in chlorosilane, silane
At least one, or the mixture of the two.
A certain proportion of silicon-containing gas and hydrogen are passed through in plasma generator, mixed gas is sent out in plasma
Electric discharge forms plasma in raw device.Specifically, hydrogen ionizes first in plasma generator, forms the strong hydrogen of activity certainly
By base, hydroperoxyl radical can induce chlorosilane or silane to ionize, that is, reduce the firing potential needed for chlorosilane/silane,
Silicon-containing gas are made to be easier to ionize.With silane (SiH4) exemplified by, in the presence of hydroperoxyl radical, hydroperoxyl radical is ionized out step by step,
Si atoms are finally given, Si atoms re-form the crystalline silicon with certain lattice structure, and the tail gas of ionization is hydrogen.Course of reaction
It is as follows：
H2→2H·；
SiH4+H·→SiH3·+H2；
SiH3·+H→SiH2·+H2；
SiH2·+H·→SiH·+H2；
SiH·+H·→Si(atom)+H2；
Si(atom)+Si(atom)→2Si(s-Nano)。
The ionization steps of chlorosilane are similar with silane, and are progressively ionized in the presence of hydroperoxyl radical, the difference is that electricity
From tail gas in contain HCl.The hydrogen carrier gas i.e. as silicon-containing gas in the present invention, also serve as inducing silicon-containing gas ionization
Pre-ionization gas.
In embodiments of the invention, it is 10~100kV that the electrode of plasma generator, which has crest voltage, frequency 5
~12kHz sinusoidal voltage.The discharging gap of plasma generator is 1~10mm.It should be appreciated that crest voltage and putting
Electric gap can do corresponding adjustment according to gas componant, should can be ionized by mixed gas and be defined for plasma.Deng from
The temperature of caused plasma is 40~60 DEG C in daughter generator.
In order to prevent metal electrode from ionizing, avoid introducing metal impurities.The electrode of plasma generator is provided with electric Jie
Matter, using the form of dielectric barrier discharge.Dielectric uses high-purity ceramic material, such as high purity aluminium oxide, high purity quartz.
Forming the mixed gas of plasma has higher activity, therefore at least part mixed gas reaction generation nanometer
The silicon grain of level, nano level silicon grain are mixed with tail gas, sent out from plasma generator.
2nd, collection step
The tail gas for being blended with nanoscalar silicon particles is discharged out of plasma generator and is passed into electrostatic adsorption device
In.Because nanoscalar silicon particles have larger surface area, and activity is enhanced in plasma generator, nano silicone
Particle is easy to be adsorbed under electrostatic field.Plasma generator is alternatively recycled to after tail gas discharge electrostatic adsorption device
In continue to participate in reaction, or through processing row outwardly.In this way, the separation of nanoscalar silicon particles and tail gas is completed, in Electrostatic Absorption
The nanoscale crystalline silicon obtained in the embodiment of the present invention is collected in device.The particle diameter of nanoscale crystalline silicon is less than 900nm.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH41 is pressed with hydrogen:1 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 2
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH41 is pressed with hydrogen:5 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 3
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH41 is pressed with hydrogen:10 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Interior electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 4
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH41 is pressed with hydrogen:15 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Interior electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 5
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH41 is pressed with hydrogen:20 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Interior electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 6
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH41 is pressed with hydrogen:25 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Interior electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 7
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH41 is pressed with hydrogen:12 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Interior electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 8
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
Silicon-containing gas and hydrogen are pressed 1:12 mixed in molar ratio, is passed through in plasma reactor, is sent out in plasma
Discharged in raw device, form plasma；And react generation nanoscalar silicon particles.Wherein silicon-containing gas are SiHCl3With SiH4It is mixed
Close gas.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 9
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiHCl31 is pressed with hydrogen:12 mixed in molar ratio, is passed through in plasma reactor, occurs in plasma
Discharged in device, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 10
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH2Cl21 is pressed with hydrogen:12 mixed in molar ratio, is passed through in plasma reactor, occurs in plasma
Discharged in device, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 11
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiH3Cl presses 1 with hydrogen:12 mixed in molar ratio, is passed through in plasma reactor, occurs in plasma
Discharged in device, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 12
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
By SiCl41 is pressed with hydrogen:12 mixed in molar ratio, is passed through in plasma reactor, in plasma generator
Interior electric discharge, form plasma；And react generation nanoscalar silicon particles.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 13
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
Silicon-containing gas and hydrogen are pressed 1:12 mixed in molar ratio, is passed through in plasma reactor, is sent out in plasma
Discharged in raw device, form plasma；And react generation nanoscalar silicon particles.Wherein silicon-containing gas are SiHCl3With SiH3Cl's
Mixed gas.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
Embodiment 14
The present embodiment provides a kind of preparation method of nanoscale crystalline silicon, and it comprises the following steps：
S1, reactions steps
Silicon-containing gas and hydrogen are pressed 1:15 mixed in molar ratio, is passed through in plasma reactor, is sent out in plasma
Discharged in raw device, form plasma；And react generation nanoscalar silicon particles.Wherein silicon-containing gas are SiCl4、SiHCl3And
SiH4Mixed gas.
In the present embodiment, the electrode of plasma generator uses dielectric barrier discharge, and dielectric selects high pure oxygen
Change aluminium or high purity quartz, discharging gap 5mm.The crest voltage of electrode is 50kV, frequency 10kHz.
S2, collection step
Tail gas containing nanoscalar silicon particles is passed through into the electrostatic adsorption device of plasma generator outlet downstream,
Nanoscalar silicon particles are adsorbed in electrostatic adsorption device, and tail gas separates discharge electrostatic adsorption device with silicon grain, and is recycled to
In plasma generator, reaction is continued to participate in.The nanoscalar silicon particles in electrostatic adsorption device are collected, that is, obtain nanoscale crystalline substance
Body silicon.The average grain diameter of nanoscale crystalline silicon is 10nm.
In summary, the preparation method of the nanoscale crystalline silicon of the embodiment of the present invention includes chlorosilane, silane etc. is siliceous
Gas mixing hydrogen is passed into plasma generator, makes mixed gas formation etc. using the electromagnetic field of plasma generator
Gas ions, it has higher activity and reacted, and nano level silicon grain is produced in plasma generator.Utilize the party
Method prepares nanoscale crystalline silicon, because silicon grain is directly to be generated by plasma state reactant reaction, without the process such as broken,
Course of reaction is in plasma generator, so being not likely to produce dust, is not easy to introduce impurity.The nano crystals produced
Silicon purity is high, high income, and lattice defect is few, superior performance.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of preparation method of nanoscale crystalline silicon, it is characterised in that it includes：
Reactions steps：Silicon-containing gas and hydrogen are together formed to plasma and anti-under the electromagnetic field of plasma generator
Should, produce nanoscalar silicon particles and tail gas；The silicon-containing gas include at least one of chlorosilane gas, silane gas.
2. the preparation method of nanoscale crystalline silicon according to claim 1, it is characterised in that the chlorosilane is four chlorinations
Silicon (SiCl4), trichlorosilane (SiHCl3), dichlorosilane (SiH2Cl2), the hydrogen silicon (SiH of a chlorine three3Cl the one or more in)
Mixture；The silane is silicon tetrahydride (SiH4)。
3. the preparation method of nanoscale crystalline silicon according to claim 1, it is characterised in that the silicon-containing gas with it is described
The mixing mol ratio of hydrogen is 1:1~1:25.
4. the preparation method of nanoscale crystalline silicon according to claim 1, it is characterised in that the silicon-containing gas with it is described
The mixing mol ratio of hydrogen is 1:5~1:20.
5. the preparation method of nanoscale crystalline silicon according to claim 1, it is characterised in that the silicon-containing gas with it is described
The mixing mol ratio of hydrogen is 1:10~1:15.
6. the preparation method of nanoscale crystalline silicon according to claim 1, it is characterised in that the plasma generator
Electrode use dielectric barrier discharge, the dielectric is high-purity ceramic material.
7. the preparation method of nanoscale crystalline silicon according to claim 1, it is characterised in that the nanoscale crystalline silicon
Preparation method also includes：
Collection step：The nanoscalar silicon particles are separated with the tail gas of the reactions steps under electrostatic field environment.
8. the preparation method of nanoscale crystalline silicon according to claim 7, it is characterised in that the plasma fills
The offgas outlet downstream put is provided with electrostatic adsorption device, and the tail gas fills with the nanoscalar silicon particles in the Electrostatic Absorption
Put and separated under interior electrostatic field.
9. the preparation method of nanoscale crystalline silicon according to claim 7, it is characterised in that the circulation of tail gas is to described
Reused in plasma generator.
A kind of 10. nanoscale crystalline silicon, it is characterised in that its nano crystals any one of by claim 1-9
The preparation method of silicon is made.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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