CN102260908B - Device for growing nanometer crystal silicon powder - Google Patents
Device for growing nanometer crystal silicon powder Download PDFInfo
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- CN102260908B CN102260908B CN 201110202784 CN201110202784A CN102260908B CN 102260908 B CN102260908 B CN 102260908B CN 201110202784 CN201110202784 CN 201110202784 CN 201110202784 A CN201110202784 A CN 201110202784A CN 102260908 B CN102260908 B CN 102260908B
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Abstract
The invention discloses a device for growing nanometer crystal silicon powder. The device comprises a reaction cavity, an air inlet pipeline arranged on the top of the reaction cavity, a collection cavity formed at the bottom of the reaction cavity, a radio frequency source positioned outside the reaction cavity and a collection net arranged inside the collection cavity. The key points include: a pair of electrodes is arranged in the reaction cavity vertically; quartz sheets serving as medium barrier layers are fixed to two ends corresponding to the electrodes to form a pair of parallel plates; a vacuum pump is connected to the bottom of the collection cavity; and an adjustable barrier plate is arranged on the lower side of the collection net inside the collection cavity. In the device, the growth time of nanometer crystal silicon can be controlled by adjusting air flow and/or adjusting the air pressure of the reaction cavity by the vacuum pump and the barrier plate, so that the sizes of nanometer crystal silicon granules can be controlled. The device is easy to operate and low in cost, and is an economic and practical device for producing the nanometer crystal silicon powder.
Description
Technical field
The present invention relates to a kind of device for preparing the nanocrystal silicon powder, grow the continuously device of mono-dispersed nano crystal silicon powder of especially a kind of plasma body that utilizes the frequency medium barrier discharge to produce.
Background technology
Because the quantum limitation effect of nanostructure, the energy level that the silicon nanostructure material has presented wide region can be in harmonious proportion room temperature luminous characteristic, and the field has the huge applications potentiality in that photoelectric device, panchromatic demonstration, solar cell, biological fluorescent labelling, optical communication and silica-based light is integrated etc.
At present, multiple technologies have been applied to the preparation of the nanocrystal silicon powder of nano-scale, and preparation method commonly used mainly contains chemical Vapor deposition process, sol-gel method, the chemical solution precipitator method, pulse laser ablation method etc.Wherein, sol-gel method and the chemical solution precipitator method all belong to the aqueous chemical reaction, do not need complicated equipment, but the particle agglomeration phenomenon are more serious, and the acquisition particle diameter is little, the particle of narrowly distributing is difficult to; The pulse laser ablation subtraction unit is complicated, need expensive superpower laser, and output is few; Compare, chemical Vapor deposition process decomposes unstripped gas and is condensed into nucleus again, and nucleus grows up to particle in the heating zone, and this method is simple to operate, can realize industrialization production, is the most a kind of methods of normal employing of present people.
Plasma enhanced chemical vapor deposition unit major part commonly used all is used for deposit film, electrode all is up and down parallel placement, put substrate at lower electrode, unstripped gas deposits at substrate after forming plasma body, form at last film, generally also need to heat at electrode, be conducive to film and form.Usually the pressure of deposit film requires to be lower than 100pa.Also have the such device of small part to be used for the growing nano particle, but need high-vacuum apparatus and heating unit, aftertreatment also needs annealing device, so the production technique more complicated, and control size of particles can only realize by opening, close radio frequency source.Generate plasma body when opening radio frequency source, begin the particle of growing, close the radio frequency source particle and stop growing, so control the purpose that the residence time reaches control size of particles.
Document " L.Mangolini; E.Thimsen; U.Kortshagen. High-Yield Plasma Synthesis of Luminescent Silicon Nanocrystals; NANO LETTERS; 2005; 5 (4): 655-659. " discloses a kind of method and apparatus based on the standby nanocrystal silicon powder of plasma enhanced chemical vapor deposition legal system, produce dielectric barrier discharge plasma with a kind of jet apparatus, the copper ring that wherein serves as electrode is enclosed within on the breather line, the plasma slab that unstripped gas forms through energising from top to down, decomposing gas grows into the nanocrystal silicon particle, then finish collection at the collecting net of bottom, the plasma stability that this method produces is poor, unstripped gas can not fully be decomposed, and the homogeneity of the nanocrystal silicon powder that generates can't guarantee, namely can not accurately control nanocrystal silicon size of particles, therefore is not suitable for large-scale industrialized production.
Summary of the invention
The technical problem to be solved in the present invention provides that a kind of production process is simple, unstripped gas is decomposed fully, and can accurately control the device of the continuous growing nanocrystalline silicon powder of nanocrystal silicon size of particles.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of device of growing nanocrystalline silicon powder, comprise reaction chamber, be arranged on the intake ducting at reaction chamber top, be arranged on the collecting chamber of reaction chamber bottom, be positioned at the radio frequency source of reaction chamber outside, and the collecting net that is arranged on collecting chamber inside; Its key is: pair of electrodes vertically arranges in reaction chamber, the two ends that electrode pair is answered are fixed with the quartz plate that serves as dielectric barrier and form the pair of parallel plate, the bottom of described collecting chamber is connected with vacuum pump, is positioned at the inside of collecting chamber and is provided with fender plate below collecting net.
Be provided with rate of flow meter on the described intake ducting.
The internal sleeve of described intake ducting is equipped with the quartzy thrust-augmenting nozzle in order to current limliting.
Described pair of parallel plate electrode is the outside aluminium bar that is surrounded by one deck isolator.
The inside of described aluminium bar is provided with in order to logical water coolant in case the overheated blind hole of burning of aluminium bar.
Being provided with two in the described blind hole is respectively applied to into the thin conduit of water and water outlet.
Be provided with the glass current limiting tube that prevents that the nanocrystal silicon powder from flying away between described reaction chamber and the collecting chamber.
Described collecting net is stainless (steel) wire.
The outside of described collecting chamber is provided with the pressure gauge of surveying its air pressure inside.
The beneficial effect that adopts technique scheme to produce is:
Frequency medium barrier discharge of the present invention has low temperature, high atmospheric pressure, nonequilibrium characteristics, it is compared with other plasma generating device have unique advantage: stop under the condition at frequency medium to produce more active particle, the quantity of electronics is more, the energy of electronics is higher, so can make more abundant that the process such as excite, ionize, dissociate carries out, and then can produce more ion, free radical, molecule, atom isoreactivity particle, be conducive to unstripped gas and fully decompose; And the cold plasma that this method produces is nonthermal plasma, and electronic temp is up to 20 000-50,000 K (～2-5 eV), and particle and gas temperature are near room temperature.When electronics and ionic bond, can produce thermopositive reaction, make the ion surface temperature rise to hundreds of K, be conducive to the formation of nanocrystal silicon particle.
The electrode that the present invention uses can make things convenient for real estate to give birth to large-area low-temperature plasma under higher pressure, and discharge can be carried out for a long time, and discharge evenly, is a kind of effective means that obtains nonequilibrium plasma under atmospheric pressure.And the radio frequency source energy even that is added on the electrode as the easier handle of the parallel plate on blocking layer is coupled in the reaction chamber.Parallel plate is relatively vertically placed, and can realize that one is heading straight for radio frequency source, reaches the purpose of the control residence time by gas mobile, and reactant gases grows into through plasma slab to flow on the following collecting net by air-flow behind the particle of several nanometers again and collects.
The present invention is simple to operate, and equipment cost is low, is a kind of device of economical and practical production nanocrystal silicon powder.Adjust gas flow and/or adjust the pressure of reaction chamber by vacuum pump and fender plate by rate of flow meter, the control reactant gases is in the residence time of plasma zone, namely control the growth time of nanocrystal silicon, obtain production even particle size distribution, controlled nanocrystal silicon powder, can realize large-scale industrialized production.
Description of drawings
Fig. 1 is structural representation of the present invention;
Fig. 2 is the Local map of the reaction chamber among Fig. 1;
Fig. 3 is the synoptic diagram of the logical water coolant of electrode among Fig. 1;
Among the figure, 1, reaction chamber, 2, intake ducting, 3, collecting chamber, 4, quartzy thrust-augmenting nozzle, 5, collecting net, 6, radio frequency source, 7, vacuum pump, 8, fender plate, 9, electrode, 10, quartz plate, 11, plasma zone, 12, the glass current limiting tube, 13, pressure gauge, 14, rate of flow meter, 15, cooling water inlet pipe, 16, copper ring, 17, polytetrafluorethylecoatings coatings, 18, cooling water outlet pipe.
Embodiment
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
The device of a kind of growing nanocrystalline silicon powder as shown in Figure 1, comprise reaction chamber 1, be arranged on the intake ducting 2 at reaction chamber 1 top, be arranged on the collecting chamber 3 of reaction chamber 1 bottom, be positioned at the radio frequency source 6 of reaction chamber 1 outside, and the collecting net 5 that is arranged on collecting chamber 3 inside; Its key is: pair of electrodes 9 vertically arranges in reaction chamber 1, the two ends of electrode 9 correspondences are fixed with the quartz plate 10 that serves as dielectric barrier and form the pair of parallel plate, the bottom of described collecting chamber 3 is connected with vacuum pump 7, is positioned at the inside of collecting chamber 3 and is provided with fender plate 8 below collecting net 5.
Be provided with rate of flow meter 14 on the described intake ducting 2.
The internal sleeve of described intake ducting 2 is equipped with the quartzy thrust-augmenting nozzle 4 in order to current limliting.
Shown in Fig. 2,3, described electrode 9 is the outside aluminium bar that is surrounded by one deck isolator.Isolator can adopt polytetrafluorethylecoatings coatings 17, adopts elargol bonding between the end of aluminium bar and the quartz plate 10, guarantees the part that aluminium bar does not expose in reaction chamber 1.Copper ring 16 is being overlapped in the outer end of aluminium bar, and copper ring 16 is connected with radio frequency source 6.After described radio frequency source 6 was opened, the radio frequency alternating-current entered in the reaction chamber 1 by aluminium bar, and the discharge of the top of aluminium bar when passing into discharge gas, sees through quartz plate 10, forms plasma slab 11 in reaction chamber 1.The frequency of the radio frequency alternating-current that uses is 13.56 MHz, and radio frequency power is 18-100 W.
The inside of described aluminium bar is provided with in order to logical water coolant in case the overheated blind hole of burning of described aluminium bar.
Be provided with two thin conduits 15,18 that are respectively applied to into water and water outlet in the described blind hole.Blind hole is opened on the central axis of aluminium bar, insert two thin conduits when needing cooling in the blind hole, and water inlet one is being headed straight in the process of growth, reaches the purpose of circulating water.
Be provided with the glass current limiting tube 12 that prevents that the nanocrystal silicon powder from flying away between described reaction chamber 1 and the collecting chamber 3.
Described collecting net 5 is stainless (steel) wire.
The outside of described collecting chamber 3 is provided with the pressure gauge 13 of surveying its air pressure inside.
Zone between the described a pair of quartz plate 10 is for forming the plasma zone 11 of nanocrystal silicon powder; After passing into mixed gas from intake ducting 2 to reaction chamber 1, reactant gases is wherein decomposed by plasma through plasma zone 11, and the fragment that decomposes in several milliseconds forms nanocrystal silicon nuclear, and grows, and process of growth is as follows:
After reactant gases flowed out plasma zone 11, nanocrystal silicon stopped growing, and these particles can be drawn into collecting chamber 3 subsequently, finish collection with the form of nano-silicon powder at stainless (steel) wire.Be exactly to control reactant gases to flow through time of plasma zone 11 for the control of growth time, this time is called residence time t:
Therefore, by adjusting gas flow L and/or adjusting the pressure of reaction chamber 1, just can adjust to residence time t the final control that realizes Nanoparticle Size, acquisition production even particle size distribution, controlled nanocrystal silicon powder.
The pressure of reaction chamber 1 is that the fender plate 8 by mobile collecting chamber 3 inside is realized, and is because the pumping speed of vacuum pump 7 is certain, if fender plate 8 is opened just take out fast entirely, slow if fender plate 8 closes and just takes out.The demonstration of pressure shows by the pressure gauge 13 that links to each other with collecting chamber 3.
Claims (6)
1. the device of a growing nanocrystalline silicon powder, comprise reaction chamber (1), be arranged on the intake ducting (2) at reaction chamber (1) top, be arranged on the collecting chamber (3) of reaction chamber (1) bottom, be positioned at the outside radio frequency source (6) of reaction chamber (1), and be arranged on the inner collecting net (5) of collecting chamber (3); It is characterized in that: pair of electrodes (9) vertically arranges in reaction chamber (1), and each electrode (9) all is vertically to arrange; The two ends that electrode (9) is corresponding are fixed with the quartz plate (10) that serves as dielectric barrier and form the pair of parallel plate, the bottom of described collecting chamber (3) is connected with vacuum pump (7), in the inside of collecting chamber (3) and be provided with fender plate (8) below collecting net (5);
Described electrode (9) is the outside aluminium bar that is surrounded by one deck isolator;
The inside of described aluminium bar is provided with in order to logical water coolant in case the overheated blind hole of burning of aluminium bar;
Be provided with two thin conduits (15,18) that are respectively applied to into water and water outlet in the described blind hole.
2. the device of a kind of growing nanocrystalline silicon powder according to claim 1 is characterized in that: be provided with rate of flow meter (14) on the described intake ducting (2).
3. the device of a kind of growing nanocrystalline silicon powder according to claim 1, it is characterized in that: the internal sleeve of described intake ducting (2) is equipped with the quartzy thrust-augmenting nozzle (4) in order to current limliting.
4. the device of a kind of growing nanocrystalline silicon powder according to claim 1 is characterized in that: be provided with the glass current limiting tube (12) that prevents that the nanocrystal silicon powder from flying away between described reaction chamber (1) and the collecting chamber (3).
5. the device of a kind of growing nanocrystalline silicon powder according to claim 1, it is characterized in that: described collecting net (5) is stainless (steel) wire.
6. the device of a kind of growing nanocrystalline silicon powder according to claim 1 is characterized in that: the outside of described collecting chamber (3) is provided with the pressure gauge (13) of surveying its air pressure inside.
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| CN 201110202784 CN102260908B (en) | 2011-07-20 | 2011-07-20 | Device for growing nanometer crystal silicon powder |
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| CN 201110202784 CN102260908B (en) | 2011-07-20 | 2011-07-20 | Device for growing nanometer crystal silicon powder |
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| CN102260908B true CN102260908B (en) | 2013-04-10 |
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| CN103224237B (en) * | 2013-05-23 | 2014-12-17 | 苏州金瑞晨科技有限公司 | Preparation method and device of phosphorus-doped nano silicon material |
| CN104211066B (en) * | 2013-06-05 | 2018-02-02 | 福建省辉锐材料科技有限公司 | A kind of Preparation equipment of silica flour |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245447A (en) * | 2007-02-14 | 2008-08-20 | 北京行者多媒体科技有限公司 | Plasma deposition method of nanocrystalline silicon |
| CN101559946A (en) * | 2009-04-27 | 2009-10-21 | 浙江大学 | Method and device for preparing silicon nanoparticles by utilizing plasma body |
| CN102320606A (en) * | 2011-07-20 | 2012-01-18 | 河北大学 | Method for growing nanocrystalline silicon powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101053836B1 (en) * | 2009-02-10 | 2011-08-03 | 한국에너지기술연구원 | Silicon nanoparticle manufacturing apparatus using IC |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245447A (en) * | 2007-02-14 | 2008-08-20 | 北京行者多媒体科技有限公司 | Plasma deposition method of nanocrystalline silicon |
| CN101559946A (en) * | 2009-04-27 | 2009-10-21 | 浙江大学 | Method and device for preparing silicon nanoparticles by utilizing plasma body |
| CN102320606A (en) * | 2011-07-20 | 2012-01-18 | 河北大学 | Method for growing nanocrystalline silicon powder |
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