CN103585939A - Laser-assisted nano-particle preparation method, and apparatus thereof - Google Patents
Laser-assisted nano-particle preparation method, and apparatus thereof Download PDFInfo
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- CN103585939A CN103585939A CN201310611785.1A CN201310611785A CN103585939A CN 103585939 A CN103585939 A CN 103585939A CN 201310611785 A CN201310611785 A CN 201310611785A CN 103585939 A CN103585939 A CN 103585939A
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- laser
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Abstract
The invention discloses a laser-assisted nano-particle preparation method, and an apparatus thereof, and belongs to the nano-material preparation field. The method comprises the following steps: a gaseous precursor is introduced into a plasma generating device and is activated by the plasma generating device, and the obtained activated gaseous precursor enters a reaction chamber; and laser beams emitted by a laser generating device pass are gathered through a lens on the wall of the reaction chamber, the gathered laser beams enter the reaction chamber and heat the activated gaseous precursor in the reaction chamber to crack the activated gaseous precursor in order to obtain active nano-particles, and the active nano-particles are collected by a collector. The nano-particle preparation method and the apparatus have the advantages of substantial reduction of the production cost, simple apparatus and good technological stability; and the prepared nano-particles have the advantages of high purity, good stability, uniform morphological particle size, high quality reliability and high yield.
Description
Technical field
The present invention relates to field of nano material preparation, be specifically related to the method and apparatus that a kind of laser assisted is prepared nano particle.
Background technology
In recent years, the preparation of nano particle and performance study thereof have caused people's extensive concern (J.Seo, Y.Kuk, et al.Appl.Phys.Lett.85 (2004) 3235 for J.H.Chio, T.-H.Kim).Nano particle has the features such as small-size effect, skin effect, quantum size effect and macro quanta tunnel effect, show the performance (W.Lu such as optical, electrical, thermal and magnetic, power that is different from traditional material, W.Wang, Y.Su, J.Li, L.Jiang, Nanotechnology16 (2005) 2582), therefore at numerous areas such as chemical industry, material, electronics, machinery, environmental protection and biomedical engineerings, there is important application.
The method of preparing at present nano particle mainly contains the (R.Buckmaster such as sol-gel process, electrochemistry, chemical precipitation method, pyrolysismethod, ion implantation, plasma method, self assembly, template, T.Hanada, Y.Kawazoe, et al.Nano Lett.5 (2005) 771).Sol-gel process can obtain a large amount of nano-powders, and cost is also lower, but is very easy to reunite, and affects practical application effect.Nano particle prepared by chemical precipitation method, its purity, pattern and size are difficult to control.Template can access large-area nano-grain array, but technique is relatively loaded down with trivial details, especially removes comparatively difficulty of template.The methods such as ion implantation, pyrolysismethod, plasma method, electrochemistry need experimental facilities and technological procedure or the higher temperature of relative complex, improved the preparation cost of nano particle, simultaneously, due to limitation separately, have influence on the practical application of nano particle.Therefore, must a kind of simple controlled method of research, obtain that purity is high, good stability, the controlled nano particle of pattern size distribution, and reduce preparation cost, avoid the reunion of nano particle.
Summary of the invention
For in prior art, nano particle preparation cost is high, purity is lower, the problem such as poor stability, pattern size be uncontrollable, the invention provides a kind of laser assisted and prepare the method for nano particle, the method is simple to operate, cost is low, and higher, the good stability of nano particle purity of preparation, pattern particle diameter are even, can be widely used in various metals or the preparation of nonmetallic nano particle.The present invention further provides a kind of equipment of preparing nano particle for laser assisted, this equipment can reduce the preparation cost of nano particle greatly.
Laser assisted is prepared a method for nano particle, and gaseous state precursor is passed into plasma producing apparatus, after plasma producing apparatus activation, forms and enters reaction chamber; The laser beam that generating device of laser sends also enters into reaction chamber after the lens in reactor wall converge; At reaction chamber inner laser, heat active gaseous state precursor, make it cracking, produce nano particle, nano particle is collected by collector.
Wherein, described gaseous state precursor is to comprise required gaseous state or the liquid organic compound of preparing nano particle, and this organic compound boiling point is lower, and LASER HEATING can cracking.In general, can be used for the organic compound of CVD, MOCVD etc., can be as the predecessor of this method.
Wherein, the lens in described reactor wall are a straight long and narrow lens window, laser beam are pooled to the laser band with one fixed width, are irradiated to the conversion zone of chamber interior, produce higher temperature in conversion zone, play the object that adds thermal decomposition predecessor.
Wherein, described reaction chamber inner laser heating-up temperature is by regulating laser power to control.
In addition,, when passing into gaseous state precursor, also pass into protective gas and sensitization gas.Protective gas is preferably H
2(super blunt rank) can also be He, Ar or N
2deng, or their gaseous mixture; Protective gas is confined to reacting gas and sensitization gas near the center of reaction chamber, prevents its accumulation of other parts corner at reactor; And the temperature that can improve particle nucleation, prevents particle aggregation.Sensitization gas is preferably SF
6or SiF
4deng, for specific laser power, can greatly improve the temperature of generation.
In the present invention, the diameter of the nano particle of preparation is in 3-100nm scope.
Laser assisted is prepared an equipment for nano particle, comprising: reaction chamber, laser generation and receiving system, plasma producing apparatus, gas access equipment, particle collection device;
Wherein, described reaction chamber is cross structure, and the laser level that described generating device of laser sends passes reaction chamber, and is received by the receiving system of the other end; Described plasma producing apparatus is positioned at the lower end of reaction chamber; Described particle collection device is positioned at the upper end of reaction chamber, relative with described plasma producing apparatus; Described gas access equipment is connected with plasma producing apparatus.
Described generating device of laser and reaction chamber connecting portion have lens window, and described lens window is inlayed long and narrow straight lens.
Described generating device of laser is such as but not limited to CO
2laser instrument.
Described plasma producing apparatus is such as but not limited to ICP, CCP etc.
Alternatively, described plasma producing apparatus quantity and arrangement mode can arrange as required and arrange, to meet the multiple different situations of preparing nano particle.
Alternatively, described particle collection device is filter membrane, filter plate, metal forming etc., can be also directly plated film substrate.
As preferably, described reaction chamber inside is provided with cooling device.
Compared with prior art, the present invention has following beneficial effect:
Because vacuum requirement in preparation process is lower, greatly reduce production cost, and equipment is simple, technology stability is good, higher, the good stability of nano particle purity of preparation, pattern particle diameter are even, and product quality reliability is high, can obtain higher nano particle productive rate simultaneously.
Accompanying drawing explanation
Fig. 1 is the equipment schematic diagram of preparing nano particle in the first embodiment of the present invention.
Fig. 2 is the light path schematic diagram that lens window of the present invention converges laser.
Fig. 3 prepares the equipment schematic diagram of nano particle in the second embodiment of the present invention.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, describe the present invention in detail, but the present invention is not limited to this.
Embodiment 1
Take and prepare nano silicon particles as example, nanometer grain preparation method of the present invention is described.It is raw material that the organic precursors of silicon is take in the preparation of nano silicon particles, as silane, such as but not limited to: SiH
4, Si
2h
6, Si
3h
8deng; Chlorosilane, for example SiH
2cl
2, SiHCl
3, SiCl
4, Si
2cl
6deng.
The organosilane precursor gas of silicon is entered into plasma generator by gas access equipment, after being activated by plasma generator, enter into reaction chamber, in reaction chamber, the LASER HEATING of being sent by laser beam, organosilicon generation cracking, produce nano silicon particles, through the gathering-device of reaction chamber top, collect.In addition, pass into protective gas H
2with sensitization gas SF
6, H
2reacting gas and sensitization gas are confined near the center of reaction chamber, prevent its accumulation of other parts corner at reactor, improve the temperature of particle nucleation simultaneously, prevent particle aggregation.Sensitization gas SF
6can improve laser temperature.The nano silicon particles diameter of preparation is about 3-100nm.
Accompanying drawing 1 is the schematic diagram of nano silicon particles Preparation equipment.Reaction chamber 100 left sides of cross structure are generating device of laser 102, right side is laser receiver (not marking in figure), the laser scioptics window 103 that laser generator 102 sends converges and incides chamber, and the conversion zone 104 at chamber center reacts; The below of reaction chamber 100 is plasma producing apparatus 105, and reaction chamber and plasma producing apparatus are all with some gaseous state access equipments 106; The nano particle producing after 104 reactions in chamber central area is collected by the particle collection device 107 above reaction chamber.
Lens window is inlaid with straight lens, as Fig. 2 (a) (b) as shown in.Fig. 2 (a) converges the front view of laser optical path for lens, the laser beam 201 that laser instrument is launched after lens 202 converge, the light beam 203 that height of formation is very little in chamber; Fig. 2 (b) converges the top view of laser optical path for lens, and the laser beam 201 that laser instrument is launched is after lens 202 converge, and light beam 203 width that form in chamber are constant.The shape that can find out lens 202 in conjunction with front view 2 (a) and top view 2 (b), lens 202 are conventional lenses shape in the vertical direction, are straight mirror in the horizontal direction.
In the present embodiment, the organosilane precursor raw materials such as silane pass into mouthfuls 106 by gas and enter in the quartz conduit of plasma generator 105, in conduit, by Ar plasma strike, are activated, and form anisotropy, with the particle of like charges, enter reaction chamber 100; While protective gas H
2, sensitization gas SF
6via the gas on side, pass into mouthfuls 106 respectively and enter reaction chamber.Laser instrument is chosen as CO
2laser instrument, power selection is 60W.Laser beam converges to 104 places, central reaction district 104， central reaction district through window lens 103 and produces high temperature.This temperature can be decomposed organic precursors, produces the nano particle of silicon.Nano particle is collected by the particle collection device 107 of reaction chamber top.
In the present embodiment, the nano silicon particles diameter of preparation is about 3-100nm.
Embodiment 2
Take and prepare copper-indium-gallium-selenium nanoparticles as example, further illustrate the present invention.
Copper-indium-gallium-selenium nanoparticles is the compound that multiple element forms, and precursor gas has organic copper, organo indium, Organogallium and selenium steam etc.For example, the organic precursors of cupric includes but not limited to: Cu (C
11h
19o
2)
2, Cu (CF
3cOCHCOCF
3)
2, (C
5h
5) CuP (C
2h
5)
3, Cu (CF
3cOCHCOCH
3)
2, Cu (CF
3cOCHCOCF
3) P (CH
3)
3deng; Organic precursors containing indium includes but not limited to: triphenyl indium (C
18h
15in), triphenyl pyridine indium (C
23h
20inN), p-methylphenyl indium (C
21h
21in) etc.; Organic precursors containing gallium includes but not limited to: dimethyl gallium fluoride (C
2h
6fGa), trimethyl gallium (C
3h
9ga), triethyl-gallium (C
6h
15ga), tripropyl gallium (C
9h
21ga), triisopropyl gallium (C
9h
21ga) etc.
The organosilane precursor gas of copper, indium, gallium and selenium steam are entered into respectively to plasma generator by gas access equipment, after being activated by plasma generator, enter into reaction chamber, in reaction chamber, the LASER HEATING of being sent by laser beam, organosilane precursor gas generation cracking, produce the nano particle of copper, indium, gallium, interact with the selenium nano particle after activation, form copper-indium-gallium-selenium nanoparticles.Copper-indium-gallium-selenium nanoparticles is collected through the gathering-device of reaction chamber top.In addition, pass into protective gas H
2with sensitization gas SF
6, H
2reacting gas and sensitization gas are confined near the center of reaction chamber, prevent its accumulation of other parts corner at reactor, improve the temperature of particle nucleation simultaneously, prevent particle aggregation.Sensitization gas SF
6can improve laser temperature.The copper-indium-gallium-selenium nanoparticles diameter of preparation is about 3-100nm.
Accompanying drawing 3 is the schematic diagram of copper-indium-gallium-selenium nanoparticles Preparation equipment.Reaction chamber 300 left sides of cross structure are generating device of laser 302, right side is laser receiver (not marking in figure), the laser scioptics window 303 that laser generator 302 sends converges and incides chamber, and the conversion zone 304 at chamber center reacts; The below of reaction chamber 300 is plasma producing apparatus 305, and owing to there being multiple precursor gas, plasma generator device 305 also has several; Reaction chamber and plasma producing apparatus are all with some gaseous state access equipments 306; The nano particle producing after 304 reactions in chamber central area is collected by the particle collection device 307 above reaction chamber.The shape of lens window and light path are identical with Fig. 2.
In the present embodiment, organic copper, organo indium, Organogallium predecessor raw material and selenium steam pass into mouth 306 by gas respectively and enter in the quartz conduit of plasma generator 305, in conduit, by Ar plasma strike, activated, form anisotropy, with the particle of like charges, enter reaction chamber 300; While protective gas H
2, sensitization gas SF
6via the gas on side, pass into mouthfuls 306 respectively and enter reaction chamber.Laser instrument is chosen as CO
2laser instrument, power selection is 80W, laser beam converges to 304 places, central reaction district 304， central reaction district through window lens 303 and produces high temperature.This temperature can be decomposed organic precursors, produces the nano particle of copper, indium, gallium and selenium.Nano particle interacts and forms CIGS particle, and copper-indium-gallium-selenium nanoparticles is collected by the particle collection device 307 of reaction chamber top.
In the present embodiment, the copper-indium-gallium-selenium nanoparticles diameter of preparation is about 3-100nm.
The foregoing is only several embodiment of the present invention, not in order to limit the present invention, to those of ordinary skill in the art, can to method of the present invention or equipment, do multiple variation, replacement and modification as required.All within spiritual scope of the present invention and principle, any modification of doing, be equal to replacement, improvement etc., all belong to the covering scope of the claims in the present invention.
Claims (9)
1. laser assisted is prepared a method for nano particle, it is characterized in that, gaseous state precursor is passed into plasma producing apparatus, after plasma producing apparatus activation, enters reaction chamber; The laser beam that generating device of laser sends also enters into reaction chamber after the lens in reactor wall converge; At reaction chamber inner laser, heat active gaseous state precursor, make it cracking, produce nano particle, nano particle is collected by collector.
2. laser assisted as claimed in claim 1 is prepared the method for nano particle, it is characterized in that, described gaseous state precursor is to comprise the required organic compound of preparing nano particle, and this organic compound boiling point is lower, and LASER HEATING can cracking.
3. laser assisted as claimed in claim 2 is prepared the method for nano particle, it is characterized in that, the temperature of described reaction chamber inner laser heating is by regulating laser power to control.
4. laser assisted as claimed in claim 2 is prepared the method for nano particle, it is characterized in that, also passes into protective gas and sensitization gas.
5. laser assisted as claimed in claim 2 is prepared the method for nano particle, it is characterized in that, the diameter of described nano particle is in 3-100nm scope.
6. laser assisted is prepared an equipment for nano particle, it is characterized in that, comprising: reaction chamber, laser generation and receiving system, plasma producing apparatus, gas access equipment, particle collection device;
Wherein, described reaction chamber is cross structure, and the laser level that described generating device of laser sends passes reaction chamber, and is received by the receiving system of the other end; Described plasma producing apparatus is positioned at the lower end of reaction chamber; Described particle collection device is positioned at the upper end of reaction chamber, relative with described plasma producing apparatus; Described gas access equipment is connected with plasma producing apparatus.
7. laser assisted as claimed in claim 6 is prepared the equipment of nano particle, it is characterized in that, described generating device of laser and reaction chamber connecting portion have lens window, and described lens window is inlayed long and narrow straight lens.
8. laser assisted as claimed in claim 6 is prepared the equipment of nano particle, it is characterized in that, described particle collection device is filter membrane, filter plate, metal forming, plated film substrate.
9. laser assisted as claimed in claim 6 is prepared the equipment of nano particle, it is characterized in that, described reaction chamber is provided with cooling device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272048A (en) * | 2019-06-17 | 2019-09-24 | 西安电子科技大学 | A kind of preparation method of two-dimensional layer nano material MXene quantum dot |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2510154Y (en) * | 2001-10-26 | 2002-09-11 | 吴征威 | Plasma mixed gas-phase-method nanometer-particle preparation appatatus |
| US20060225534A1 (en) * | 2004-10-13 | 2006-10-12 | The Research Foundation Of State University Of New York | Production of nickel nanoparticles from a nickel precursor via laser pyrolysis |
| US20100012032A1 (en) * | 2008-07-19 | 2010-01-21 | Yung-Tin Chen | Apparatus for high-rate chemical vapor deposition |
-
2013
- 2013-11-25 CN CN201310611785.1A patent/CN103585939A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2510154Y (en) * | 2001-10-26 | 2002-09-11 | 吴征威 | Plasma mixed gas-phase-method nanometer-particle preparation appatatus |
| US20060225534A1 (en) * | 2004-10-13 | 2006-10-12 | The Research Foundation Of State University Of New York | Production of nickel nanoparticles from a nickel precursor via laser pyrolysis |
| US20100012032A1 (en) * | 2008-07-19 | 2010-01-21 | Yung-Tin Chen | Apparatus for high-rate chemical vapor deposition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272048A (en) * | 2019-06-17 | 2019-09-24 | 西安电子科技大学 | A kind of preparation method of two-dimensional layer nano material MXene quantum dot |
| CN110272048B (en) * | 2019-06-17 | 2022-04-22 | 西安电子科技大学 | Preparation method of two-dimensional layered nano material MXene quantum dots |
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Application publication date: 20140219 |