CN102335580A - Apparatus and method for preparing group IV nanoparticles with capacitive coupling plasma - Google Patents
Apparatus and method for preparing group IV nanoparticles with capacitive coupling plasma Download PDFInfo
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- CN102335580A CN102335580A CN2011101674629A CN201110167462A CN102335580A CN 102335580 A CN102335580 A CN 102335580A CN 2011101674629 A CN2011101674629 A CN 2011101674629A CN 201110167462 A CN201110167462 A CN 201110167462A CN 102335580 A CN102335580 A CN 102335580A
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Abstract
The invention discloses an apparatus and method for preparing group IV nanoparticles with capacitive coupling plasma. According to the apparatus, centers of an internal electrode and an external electrode superpose each other, and a radio frequency electrode and a ground electrode with a concentric structure are formed; a cavity between the internal electrode and the external electrode is a reaction cavity; when a radio frequency power supply works, plasma is produced between the internal electrode and the external electrode. The apparatus provided in the invention has the advantages of simple construction, a larger plasma occurrence area and capacity of maintaining continuous stabilized production. Using the apparatus for preparation of group IV nanoparticles with capacitive coupling plasma enables density and uniformity of plasma to be guaranteed; prepared nanoparticles have good uniformity; the apparatus can carry out continuous and stable production and is suitable for popularization for industrial production.
Description
Technical field
The present invention relates to technical field of nano material, relate in particular to the device and method that a kind of capacitance coupling plasma prepares four family's nano particles.
Background technology
In recent years, four family's nano particles are because it in the boundless application prospect of electronics, photoelectron, photovoltaic and biomedical sector, more and more causes people's interest.On the one hand, they can easily incorporate in traditional device fabrication, strengthen the function of traditional devices; On the other hand, they have greatly promoted the generation of new technology and new unit.For example, will profoundly change the manufacturing process of silicon device, reduce the cost of various silicon devices such as transistor and solar cell greatly based on the printing electronics of nano silicon particles.
Aspect the research and application and development of four family's nano particles, the problem that at first relates to is exactly the preparation of nano particle.At present, four family's nano particles, for example nano silicon particles can prepare through solid phase method, liquid phase method and vapor phase method.The nano particle (like silicon) of solid phase method preparation is to be embedded in matrix (like silica membrane) lining (like U.S. Pat 7220609).Because they are not freely to disperse, their application has limitation.Liquid phase method prepares nano particle productivity ratio generally very low (is Chinese invention patent application and the U.S. Pat 7214599 of CN1456678A, CN1356259A like publication number).
Current preparation four family's the highest methods of nano particle productive rate are vapor phase methods; For example: utilize laser (like Li etc.; Process for preparing macroscopic quantities of brightly photoluminescent silicon nanoparticles with emission spanning the visible spectrum; Langmuir 19 (2003), 8490-8496) or plasma (like Magonili etc., High-yield plasma synthesis of luminescent silicon nanocrystals; Nano Letters 5 (2005), 655-659; Ryan Gresback etc., Nonthermal plasma synthesis of size-controlled, monodisperse, freestanding germanium nanocrystals, Applied Physics Letters 91 (2007), 093119; Publication number is the U.S. Patent application United States Patent (USP) of US20060051505A1 and US20070172406A1) decompose the gas molecule of siliceous or germanium, decompose and atom combine to form nano particle again.Wherein, Plasma method is as a kind of four novel family's preparation of nanoparticles modes; Normally place radio-frequency electrode and ground electrode at the quartz ampoule outer wall that is connected with reaction gas; Provocative reaction gas produces plasma between two electrodes, utilizes the reactivity of plasma height, synthetic four family's nano particles.Because it is simple, with low cost that the using plasma method prepares four family's nano particle methods, and the four family's nanoparticle size that obtain are little, are evenly distributed, and are not prone to the agglomeration traits in the chemical synthesis process, therefore more and more receive people's attention.
But; In the above-mentioned plasma apparatus, thereby nano particle can form continuous film attached to the inwall of plasma chamber between radio-frequency electrode and ground electrode, causes the conducting between the electrode; The final stability that influences plasma makes the preparation of nano particle be difficult to continue carry out.In addition, unsettled plasma also is difficult to guarantee to obtain high-quality nano particle.Therefore, preparing four family's nano particles about plasma method at present mainly is to be applied to the scientific research aspect, and low output is the main bottleneck that restriction four family's nano particles are used in wider scope.In the face of the shortcoming of plasma method in four family's preparation of nanoparticles, people attempt to adopt new plasma producing apparatus, solve that four family's nano particles are assembled and the problem that limits continuity production between radio-frequency electrode and ground electrode.
Summary of the invention
The invention provides the device and method that a kind of capacitance coupling plasma prepares four family's nano particles; Adopt the radio-frequency electrode and the ground electrode of concentric structure to be coupled as electric capacity; Between two electrodes, produce plasma and prepare four family's nano particles; This apparatus structure is simple, can produce sustainedly and stably, is fit to the popularization of suitability for industrialized production.
A kind of capacitance coupling plasma prepares the device of four family's nano particles; Comprise: external electrode and interior electrode; Described external electrode is made up of the shell of a hollow; Described shell is provided with air inlet and gas outlet, described in electrode be fixed on the inside of described shell, described inside and outside electrode shape is identical, vary in size, the center overlaps; Described external electrode ground connection is ground electrode, and described interior electrode and external radio-frequency drive device are connected to radio-frequency electrode, and the cavity between described interior electrode and the external electrode is reaction cavity (plasma chamber).
In the optimized technical scheme, described inside and outside electrode is the symmetry structure, can guarantee the density of plasma like this, also can guarantee the uniformity of plasma, and the nano particle of preparation is occurred than big difference.
In the optimized technical scheme, described inside and outside electrode is spherical structure.
In the optimized technical scheme, described inside and outside electrode is square, described square be rectangle or square structure.
In the optimized technical scheme, described inside and outside electrode is oval structure.
In the optimized technical scheme, described inside and outside electrode is triangular structure.
In the optimized technical scheme, described inside and outside electrode is cylindrical structural.
In conditions such as process technology and facility environments not simultaneously, can not select to adopt inside and outside electrode according to actual needs with above difform symmetry structure.
In the optimized technical scheme, the material of described inside and outside electrode is copper or stainless steel.
In the optimized technical scheme, the outer surface of described interior electrode and the inner surface of external electrode are coated with insulating barrier, to prevent the pollution of the nano particle that electrode pair prepares.Described insulating barrier is silica, silicon nitride, borosilicate, carborundum or gathers acetate fat-aluminium oxide, preferably adopts silicon nitride, and is relatively low because of its sputtering raste, is optimal insulating materials.
In the optimized technical scheme, the spacing of described interior electrode and external electrode is the 5-50 millimeter, to guarantee to obtain highdensity plasma.
Among the present invention, described in electrode can be for solid, also can be for hollow; Described excitation apparatus comprises RF match case and the radio-frequency power supply that links to each other with the RF match case; Described RF match case also links to each other with described interior electrode through cable or short metal (like copper) lead simultaneously; Described radio-frequency power supply can adopt rf frequency general in the prior art, is preferably 13.56MHz.
Capacitance coupling plasma of the present invention prepares the device of four family's nano particles, can be used for preparing four different family's nano particles, comprises nano silicon particles, germanium nano particle, sige alloy nano particle.Simultaneously, through changing reactant gas source, can also in the preparation process of nano particle, realize mixing.For example, in the process of synthetic nano silicon particles,, be implemented in the nano silicon particles boron-doping or mix phosphorus through in reacting gas, adding borine or phosphine.
Capacitance coupling plasma of the present invention prepares the device of four family's nano particles; The center of inside and outside electrode overlaps; Constitute the radio-frequency electrode and the ground electrode of concentric structure; Cavity between the inside and outside electrode is reaction cavity (plasma chamber), after radio-frequency power supply work, between inside and outside electrode, produces plasma.Because inside and outside electrode provides the chamber wall of reaction cavity, apparatus of the present invention are simple in structure; Simultaneously, in the preparation process of four family's nano particles, the nano particle that produces in the reaction cavity may accumulate between the electrode, but the nanometer particle film on two electrodes can mutual conduction, thereby can keep continuous steady production; Because inside and outside electrode is a concentric structure, and takes Capacitance Coupled, can guarantee the density of plasma, also can guarantee the uniformity of plasma, the nano particle good evenness of preparation; In addition; Owing to be between the total inner surface of the whole outer surface of interior electrode and external electrode, to produce plasma; With respect between two annular electrodes, producing plasma in the prior art, the electrode arrangement mode in apparatus of the present invention has bigger plasma generation area.Therefore, the device that capacitance coupling plasma of the present invention prepares four family's nano particles can guarantee the density of plasma for a long time, realizes serialization production.
Capacitance coupling plasma of the present invention prepares the device of four family's nano particles; Can also be through changing the relative size of radio-frequency electrode (interior electrode) and ground electrode (external electrode); Perhaps under the ground electrode rigid condition, change the internal radio frequency electrode size; Can change the size of reaction cavity easily, thus the parameter that can regulate cold plasma, thus the nano particle of demands of different is satisfied in preparation.Therefore, utilize capacitance coupling plasma of the present invention to prepare the device of four family's nano particles, can prepare four family's nano particles of different sizes, different degree of crystallizations.
With respect to prior art, the device that capacitance coupling plasma of the present invention prepares four family's nano particles has following beneficial technical effects:
(1) simplifies the structure, reduced cost;
(2) avoided in the preparation process of four family's nano particles nano particle between electrode, to assemble the defective that forms continuous film, steady operation constantly;
(3) have bigger plasma generation area, can guarantee the density of plasma for a long time, realize serialization production.
(4) can guarantee the density of plasma, also can guarantee the uniformity of plasma, the nano particle good evenness of preparation.
Utilize above-mentioned apparatus of the present invention capacitance coupling plasma to prepare the method for four family's nano particles, comprising: reacting gas enters into described reaction cavity through described air inlet; Under vacuum condition, described reacting gas is excited by rf wave to be plasma state, and generates four family's nano particles continuously; Described four family's nano particles flow out through described gas outlet and are collected.Described reacting gas comprises reactant gas source and inert gas, and described reactant gas source is all gases that can be used for preparing four family's nano particles in the prior art, comprises the silane (SiH that is used to prepare nano silicon particles
4) or chlorosilane (SiHCl
3Or SiCl
4), be used to prepare the germane (GeH of germanium nano particle
4) or chlorine germane (GeCl
4) etc.When using chlorosilane or chlorine germane, hydrogen (H
2) also need be used simultaneously, if there is not hydrogen, the nano particle that makes can contain a large amount of chlorine (Cl), this is disadvantageous to nano particle in the application aspect a lot.Described inert gas can be helium (He), neon (Ne) or argon gas gases such as (Ar).
When needs are nano-particle doped to four families, can also in plasma chamber, feed impurity gas.Impurity gas can be the gas that contains the 3rd major element or the 5th major element, like borine (B
2H
6), phosphine (PH
3).
Compared with prior art, the inventive method has following beneficial technical effects:
1, utilizes method of the present invention in the preparation process of four family's nano particles, to avoid the continuous film forming of nano particle between electrode, make plasma steady operation constantly.
2, adopt method of the present invention to prepare four family's nano particles, can guarantee the density of plasma, also can guarantee the uniformity of plasma, the nano particle good evenness of preparation.
3, adopt method of the present invention can prepare four family's nano particles, comprise nano silicon particles, germanium nano particle, sige alloy nano particle, and can carry out the 3rd major element or the doping of the 5th major element them with different characteristic.
Description of drawings
Fig. 1 prepares the sketch map of first kind of embodiment of the device of four family's nano particles for capacitance coupling plasma of the present invention.
Fig. 2 prepares the sketch map of second kind of embodiment of the device of four family's nano particles for capacitance coupling plasma of the present invention.
Fig. 3 prepares the sketch map of the third embodiment of the device of four family's nano particles for capacitance coupling plasma of the present invention.
Fig. 4 is the XRD figure spectrum of embodiment 1 preparation nano silicon particles.
Fig. 5 is the XRD figure spectrum of embodiment 2 preparation nano silicon particles.
The specific embodiment
Specify the present invention below in conjunction with embodiment and accompanying drawing, but the present invention is not limited to this.
Embodiment 1:
As shown in Figure 1, a kind of capacitance coupling plasma prepares the device of four family's nano particles, comprising: external electrode 2 and interior electrode 1.External electrode 2 is the spherical housing of a hollow, and spherical housing one end is provided with air inlet 3, is connected with reacting gas, and the other end is provided with gas outlet 4, is connected with the nano particle gathering-device, and external electrode 2 links to each other with earth connection 7, is ground electrode.Interior electrode 1 is the hollow sphere structure, is fixed on the inside of shell, and a lead links to each other with radio-frequency power supply 8 with the matching box of outside, is radio-frequency electrode.The center of external electrode 2 and interior electrode 1 overlaps.Cavity between external electrode 2 and the interior electrode 1 is reaction cavity (plasma chamber).
Wherein, the material of external electrode 2 and interior electrode 1 is a stainless steel.Be coated with insulating barrier 6 at the outer surface of interior electrode 1 and the inner surface of external electrode 2.Insulating barrier 6 materials are silicon nitride.Radio-frequency power supply adopts the radio-frequency power supply of 13.56MHz to excite discharge, through adaptation radio-frequency power and reacting gas is complementary, and provocative reaction gas produces plasma.
For the ease of the plasma situation of observing response inside cavity, on spherical housing external electrode 2, establish an observation window 5.
It is following to utilize device capacitance coupling plasma as shown in Figure 1 to prepare the method for four family's nano particles:
The external diameter of electrode 1 is 80mm in selecting, and the external diameter of external electrode 2 is 130mm.The silane gas of 10sccm (standard milliliter per minute), the argon gas of 300sccm are mixed the back through in the air inlet 3 entering plasma reaction chambers.Pneumatic pipe cleaner in the plasma chamber is crossed the vavuum pump that gathering-device was connected that is connected with gas outlet 4 and is adjusted to about 500Pa.The effective radio-frequency power that is applied on the plasma is 80W.
Gas is activated into plasma state in the plasma chamber under radio-frequency drive, and generates nano silicon particles continuously, and is collected by the gathering-device that links to each other with gas outlet 4.X-ray diffraction (XRD) is measured (referring to Fig. 4) and is shown that prepared nano silicon particles is a crystalline state, calculates its average-size through the Scherrer formula and is about 10nm.
Embodiment 2:
As shown in Figure 2, a kind of capacitance coupling plasma prepares the device of four family's nano particles, comprising: external electrode 22 and interior electrode 21.External electrode 22 is the rectangle shell of a hollow, and rectangle shell one end is provided with air inlet 23, is connected with reacting gas, and the other end is provided with gas outlet 24, is connected with the nano particle gathering-device, and external electrode 22 links to each other with earth connection 27, is ground electrode.Interior electrode 21 is the hollow square structure, is fixed on the inside of square shell, and a lead links to each other with radio-frequency power supply 28 with the matching box of outside, is radio-frequency electrode.The center of external electrode 22 and interior electrode 21 overlaps.Cavity between external electrode 22 and the interior electrode 21 is reaction cavity (plasma chamber).
Wherein, the material of external electrode 22 and interior electrode 21 is a copper.Radio-frequency power supply adopts the radio-frequency power supply of 13.56MHz to excite discharge, through adaptation radio-frequency power and reacting gas is complementary, and provocative reaction gas produces plasma.
For the ease of the plasma situation of observing response inside cavity, on square shell external electrode 22, establish an observation window 25.
It is following to adopt device capacitance coupling plasma as shown in Figure 2 to prepare the method for four family's nano particles:
Electrode 21 is of a size of 80 * 100mm in selecting, and external electrode 22 is of a size of 130 * 150mm.The silane gas of 18.8sccm (standard milliliter per minute), the argon gas of 300sccm are mixed the back through in the air inlet 23 entering plasma reaction chambers.Pneumatic pipe cleaner in the plasma chamber is crossed the vavuum pump that gathering-device was connected that is connected with gas outlet 24 and is adjusted to about 300Pa.The effective radio-frequency power that is applied on the plasma is 100W.
Gas is activated into plasma state in the plasma chamber under radio-frequency drive, and generates nano silicon particles continuously, and is collected by the gathering-device that links to each other with gas outlet 24.X-ray diffraction (XRD) is measured (referring to Fig. 5) and is shown that prepared nano silicon particles is a crystalline state.Calculate its average-size through the Scherrer formula and be about 40nm.Comparison diagram 4 can see that the peak width of XRD narrows down along with the increase of particle size.
Embodiment 3:
As shown in Figure 3, a kind of capacitance coupling plasma prepares the device of four family's nano particles, comprising: external electrode 32 and interior electrode 31.External electrode 32 is the triangle shell of a hollow, and triangle shell one end is provided with air inlet 33, is connected with reacting gas, and the other end is provided with gas outlet 34, is connected with the nano particle gathering-device, and external electrode 32 links to each other with earth connection 37, is ground electrode.Interior electrode 31 is the three-pointed hollow star structure, is fixed on the inside of triangle shell, and a lead links to each other with radio-frequency power supply 38 with the matching box of outside, is radio-frequency electrode.The center of external electrode 32 and interior electrode 31 overlaps.Cavity between external electrode 32 and the interior electrode 31 is reaction cavity (plasma chamber).
Wherein, the material of external electrode 32 and interior electrode 31 is a copper.Radio-frequency power supply adopts the radio-frequency power supply of 13.56MHz to excite discharge, through adaptation radio-frequency power and reacting gas is complementary, and provocative reaction gas produces plasma.
For the ease of the plasma situation of observing response inside cavity, on triangle shell external electrode 32, establish an observation window 35.
It is following to adopt device capacitance coupling plasma as shown in Figure 3 preparation to mix the method for nano silicon particles of P:
Electrode 31 is an equilateral triangle in selecting, and size dimension is 80mm; External electrode 32 is an equilateral triangle, and size dimension is 160mm.
The argon gas of the silane gas of 10sccm (standard milliliter per minute), 300sccm and the phosphine source of the gas of 72sccm (containing 0.1% phosphine and 99.9% argon gas) are mixed the back to be got in the plasma reaction chambers through air inlet 33.Pneumatic pipe cleaner in the plasma chamber is crossed the vavuum pump that gathering-device was connected that is connected with gas outlet 34 and is adjusted to about 550Pa.The effective radio-frequency power that is applied on the plasma is 85W.
Gas is activated into plasma state in the plasma chamber under radio-frequency drive, and generates the nano silicon particles of mixing P continuously, and is collected by the gathering-device that links to each other with gas outlet 34.These nano silicon particles sizes of mixing P are about 10nm.Through the doping of P in the inductively coupled plasma Atomic Emission Spectrometer AES measurement nano silicon particles, find that the content of P in the nano silicon particles is about 4% (atomic concentration).
More than be merely several embodiment of the present invention, but the present invention is not limited to this, the some distortion according to inventive concept has been done all should be regarded as protection scope of the present invention.When preparing four family nano particles at device capacitance coupling plasma as shown in Figure 1; Through the external diameter of electrode 1 in changing or the internal diameter of external electrode 2; Or under external electrode 2 permanence conditions, change the interior electrode 1 of different size; The size of adjustment reaction cavity can change the time of staying of reaction particles in cavity, obtains the nano particle of different size.
Claims (10)
1. a capacitance coupling plasma prepares the device of four family's nano particles; It is characterized in that; Comprise: external electrode and interior electrode, described external electrode is made up of the shell of a hollow, and described shell is provided with air inlet and gas outlet; Electrode is fixed on the inside of described shell in described, and described inside and outside electrode shape is identical, the center overlaps; Described external electrode ground connection is ground electrode, and described interior electrode and external radio-frequency drive device are connected to radio-frequency electrode, and the cavity between described interior electrode and the external electrode is a reaction cavity.
2. capacitance coupling plasma as claimed in claim 1 prepares the device of four family's nano particles, it is characterized in that, described inside and outside electrode is the symmetry structure.
3. capacitance coupling plasma as claimed in claim 2 prepares the device of four family's nano particles, it is characterized in that, described symmetry structure is spherical structure, rectangle structure, square structure, triangular structure, ellipsoidal structure or cylindrical structural.
4. capacitance coupling plasma as claimed in claim 1 prepares the device of four family's nano particles, it is characterized in that, the material of described inside and outside electrode is copper or stainless steel.
5. capacitance coupling plasma as claimed in claim 1 prepares the device of four family's nano particles, it is characterized in that, the outer surface of described interior electrode and the inner surface of external electrode are coated with insulating barrier.
6. capacitance coupling plasma as claimed in claim 5 prepares the device of four family's nano particles, it is characterized in that, described insulating barrier is silica, silicon nitride, borosilicate, carborundum or gathers acetate fat-aluminium oxide.
7. capacitance coupling plasma as claimed in claim 1 prepares the device of four family's nano particles, it is characterized in that, the spacing of described interior electrode and external electrode is the 5-50 millimeter.
8. adopt the method for preparing four family's nano particles like the arbitrary described device capacitance coupling plasma of claim 1～7, it is characterized in that comprise: reacting gas enters into described reaction cavity through described air inlet; Under vacuum condition, described reacting gas is excited by rf wave to be plasma state, and generates four family's nano particles continuously; Described four family's nano particles flow out through described gas outlet and are collected;
Described reacting gas comprises reactant gas source and inert gas; Described reactant gas source is the silane, the chlorosilane and the hydrogen that are used to prepare nano silicon particles that are used to prepare nano silicon particles, be used to the chlorine germane and the hydrogen that prepare the germane of germanium nano particle or be used to prepare the germanium nano particle, and described inert gas is helium, neon or argon gas.
9. method as claimed in claim 8 is characterized in that described reacting gas also comprises impurity gas, and described impurity gas is the gas that contains the 3rd major element or the 5th major element.
10. method as claimed in claim 9 is characterized in that, described impurity gas is borine or phosphine.
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| CN108686597A (en) * | 2018-05-16 | 2018-10-23 | 亚洲硅业（青海）有限公司 | A kind of preparation method of gas discharge reactor, gas discharge system and trichlorosilane |
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| CN108686597A (en) * | 2018-05-16 | 2018-10-23 | 亚洲硅业（青海）有限公司 | A kind of preparation method of gas discharge reactor, gas discharge system and trichlorosilane |
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Application publication date: 20120201 |