CN103290392A - Electrode-shearing plasma enhanced chemical vapor deposition device and method - Google Patents
Electrode-shearing plasma enhanced chemical vapor deposition device and method Download PDFInfo
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- CN103290392A CN103290392A CN2012100520280A CN201210052028A CN103290392A CN 103290392 A CN103290392 A CN 103290392A CN 2012100520280 A CN2012100520280 A CN 2012100520280A CN 201210052028 A CN201210052028 A CN 201210052028A CN 103290392 A CN103290392 A CN 103290392A
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Abstract
The invention discloses an electrode-shearing plasma enhanced chemical vapor deposition device and method. The device comprises multiple side plates which are sequentially arranged in a hollow shell and overlapped at the center and respectively serve as a head electrode, multiple middle electrodes and a tail electrode; a cavity is formed among adjacent head electrode, middle electrode and tail electrode; an air inlet and an air outlet are formed in the cavity; the head electrode is connected with an external matching box and a radio-frequency power supply through a wire to serve as a radio-frequency electrode; and the tail electrode is connected with the ground to serve as a ground electrode. The device disclosed by the invention has a simple structure and a larger plasma generation area; and by applying the device disclosed by the invention to the plasma preparation of nano particles, the plasma density and uniformity can be guaranteed, the prepared nano particles have good uniformity, continuous stable production can be realized, and the device is suitable for the popularization of industrial production.
Description
Technical field
The present invention relates to technical field of nano material, relate in particular to a kind of plasma enhanced chemical vapor deposition unit and method of common electrode.
Background technology
In recent years, nano particle is 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, improve the performance of traditional devices; On the other hand, they have greatly promoted the generation of novel process and novel material.For example, will profoundly change the manufacturing process of metal and nonmetal device based on the printing electronics of carbon nano-particle, reduce the cost of various nonmetal devices such as transistor and solar cell greatly.
Aspect the research and application and development of nano particle, the problem that at first relates to is exactly the preparation of nano particle.At present, nano particle, for example carbon nano-particle can prepare by solid phase method, liquid phase method and vapor phase process.
It is current that to prepare the highest method of nano particle productive rate be vapor phase process, for example: utilize laser (as Li etc., plasma method is as a kind of novel preparation of nanoparticles mode, normally place radio-frequency electrode and ground electrode at the silica tube outer wall that is connected with reaction gas, provocative reaction gas produces plasma body between two electrodes, utilize the reactive behavior of plasma height, the synthesis of nano particle.Because it is simple, with low cost that the using plasma legal system is equipped with the nano particle method, and the nanoparticle size that obtains is little, is evenly distributed, and is not prone to the agglomeration traits in the chemical synthesis process, therefore more and more be subjected to people's attention.
But, in the above-mentioned plasma apparatus, thereby the inwall that nano particle can be attached to plasma chamber between radio-frequency electrode and ground electrode forms continuous film, causes the conducting between the electrode, the final stability that influences plasma body makes the preparation of nano particle be difficult to continue carry out.In addition, unsettled plasma body also is difficult to guarantee to obtain high-quality nano particle.Therefore, preparing nano particle about plasma method at present mainly is to be applied to the scientific research aspect, and low output is the main bottleneck that the restriction nano particle is used in wider scope.In the face of the shortcoming of plasma method in preparation of nanoparticles, people attempt to adopt new plasma producing apparatus, solve that nano particle is assembled and the problem that limits continuity production between radio-frequency electrode and ground electrode.
Summary of the invention
The invention provides a kind of plasma enhanced chemical vapor deposition unit and method of common electrode, employing is coupled as electric capacity with radio-frequency electrode and the ground electrode of tropism's structure, between two electrodes, produce plasma body and prepare nano particle, this apparatus structure is simple, can produce sustainedly and stably, be fit to the popularization of suitability for industrialized production.
A kind of plasma enhanced chemical vapor deposition unit of common electrode and method, being included in empty enclosure in arranges successively and establishes and several side plates that the center overlaps, respectively as first electrode, several electrodes and tail electrode, be provided with cavity between described adjacent first electrode, an electrode and the tail electrode, cavity is provided with inlet mouth and air outlet; Described first electrode links to each other with radio-frequency power supply with the match box of outside by lead, as radio-frequency electrode; Described tail electrode links to each other with the earth, as ground electrode.
Described first electrode, an electrode be identical with the tail electrode shape, vary in size, the center overlaps, and all is located in the rectangular enclosure empty in.Cavity between described first electrode and the tail electrode is plasma reaction body cavity body.
Preferably, the spacing between described several electrodes is the 5-50 millimeter, to guarantee to obtain highdensity plasma body.
Preferably, described first electrode, an electrode and tail electrode are the symmetry structure, for example are square structure.Can guarantee the density of plasma body like this, also can guarantee the homogeneity of plasma body, the nano particle of preparation is occurred than big difference.
Preferably, described inlet mouth and air outlet are located at the two ends of respective chamber respectively.
Preferably, the material of described first electrode or tail electrode is copper or stainless steel.
Preferably, the internal surface of the surface of described electrode and first electrode, tail electrode is coated with insulation layer, to prevent the pollution of the nano particle that electrode pair prepares.The material of described insulation layer is silicon nitride, borosilicate, silicon-dioxide, silicon carbide or poly-acetic acid fat-aluminum oxide, preferably adopts silicon nitride, and is relatively low because of its sputtering raste, is optimal insulating material.
The plasma enhanced chemical vapor deposition unit of common electrode of the present invention and method can be used for preparing different nano particles, comprise germanium nano particle, sige alloy nano particle.Simultaneously, by changing reactant gas source, can also in the preparation process of nano particle, realize mixing.For example, in the process of synthetic germanium nano particle, by in reactant gases, adding borine or phosphine, be implemented in the germanium nano particle boron-doping or mix phosphorus.
The plasma enhanced chemical vapor deposition unit of common electrode of the present invention and method, first,, the center of tail electrode overlaps, and constitutes radio-frequency electrode and the ground electrode of concentric structure.First,, the cavity between the tail electrode is reaction cavity (plasma chamber), after radio-frequency power supply work, first,, produce plasma body between the tail electrode.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 nano particle, the nano particle that produces in the reaction cavity may accumulate between the electrode, but the nanometer particle film on the electrode can mutual conduction, thereby can keep continuous stably manufactured; Because first,, the tail electrode is concentric structure, and takes condenser coupling, can guarantee the density of plasma body, also can guarantee the uniformity coefficient of plasma body, the nano particle good evenness of preparation; In addition, owing to be between the total inner surface of the entire exterior surface of an electrode and outer electrode, to produce plasma body, with respect to producing plasma body in the prior art between two internal and external electrodes, the electrode arrangement mode in apparatus of the present invention has bigger plasma body generation area.Therefore, the device that capacitance coupling plasma of the present invention prepares nano particle can guarantee the density of plasma body for a long time, realizes serialization production.
The plasma enhanced chemical vapor deposition unit of common electrode of the present invention and method, can also be by changing the relative size of radio-frequency electrode (first electrode) and ground electrode (tail electrode), perhaps under the ground electrode rigid condition, change the internal radio frequency electrode size, can change the size of reaction cavity easily, thereby can regulate the parameter of cold plasma, thereby the different nano particles that require are satisfied in preparation.Therefore, utilize capacitance coupling plasma of the present invention to prepare the device of nano particle, can prepare the nano particle of different sizes, different degree of crystallizations.
With respect to prior art, the plasma enhanced chemical vapor deposition unit of common electrode of the present invention and method have following beneficial technical effects:
(1) simplifies the structure, reduced cost;
(2) avoided in the preparation process of nano particle nano particle between electrode, to assemble the defective that forms continuous film, steady operation constantly;
(3) have bigger plasma body generation area, can guarantee the density of plasma body for a long time, realize serialization production.
(4) can guarantee the density of plasma body, also can guarantee the uniformity coefficient of plasma body, the nano particle good evenness of preparation.
Utilize plasma enhanced chemical vapor deposition unit and the method for above-mentioned apparatus of the present invention common electrode, comprising: reactant gases enters into described reaction cavity by described inlet mouth; Under vacuum condition, described reactant gases is excited by rf wave to be plasma state, and generates nano particle continuously; Described nano particle flows out by described air outlet and is collected.Described reactant gases comprises reactant gas source and rare gas element, and described reactant gas source is all gases that can be used for preparing nano particle in the prior art, comprises the chlorosilane (SiHCl for the preparation of nano silicon particles
3Or SiCl
4), for the preparation of 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 to be used simultaneously, if there is not hydrogen, the nano particle that makes can contain a large amount of chlorine (C1), this is disadvantageous to nano particle in the application aspect a lot.Described rare gas element can be argon gas (Ar), helium (He), neon gases such as (Ne).
When needs when nano-particle doped, can also in plasma chamber, feed impurity gas.Impurity gas can be the gas that contains the 5th main group element or the 3rd main group element, as phosphine (PH
3).
Compared with prior art, the inventive method has following beneficial technical effects:
1, utilizes method of the present invention can in the preparation process of nano particle, avoid the continuous film forming of nano particle between electrode, make plasma body steady operation constantly.
2, adopt method of the present invention to prepare nano particle, can guarantee the density of plasma body, also can guarantee the uniformity coefficient of plasma body, the nano particle good evenness of preparation.
3, adopt method of the present invention can prepare the nano particle with different characteristics, comprise germanium nano particle, nano silicon particles, sige alloy nano particle, and can carry out the 3rd main group element or the doping of the 5th main group element to them.
Description of drawings
Fig. 1 is the synoptic diagram of a kind of embodiment of the plasma enhanced chemical vapor deposition unit of common electrode of the present invention and method.
Fig. 2 is the XRD figure spectrum of embodiment 1 preparation nano silicon particles.
Number in the figure explanation: 1. first electrode, 2. an electrode, 3. tail electrode, 4. inlet mouth, 5. air outlet, 6. insulation layer, 7. grounding wire.
Embodiment
Describe the present invention in detail 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 plasma enhanced chemical vapor deposition unit of common electrode and method, being included in empty enclosure in arranges successively and establishes and the side plate of several rectangular configuration that the center overlaps, respectively as first electrode 1, several electrodes 2 and tail electrode 3, be provided with plasma reaction chamber between described adjacent first electrode 1, an electrode 2 and the tail electrode 3, one end of cavity is provided with the inlet mouth 4 that is connected with reactant gases, and the other end is provided with the air outlet 5 that is connected with the nano particle collection device; Described first electrode 1 links to each other with radio-frequency power supply with the match box of outside by lead, as radio-frequency electrode; Described tail electrode 3 links to each other with the earth, as ground electrode.
Preferably, described first electrode 1, an electrode 2 and tail electrode 3 are the symmetry structure, for example are square structure.Can guarantee the density of plasma body like this, also can guarantee the homogeneity of plasma body, the nano particle of preparation is occurred than big difference.Preferably, the spacing between described several electrodes 2 is the 5-50 millimeter, to guarantee to obtain highdensity plasma body.
Wherein, the material of first electrode 1 and tail electrode 3 is stainless steel.Internal surface at the outside surface of an electrode 2 and first electrode 1, tail electrode 3 is coated with insulation layer 6.Insulation layer 6 materials are silicon nitride.Radio-frequency power supply adopts the radio-frequency power supply of 13.56MHz to excite discharge, by matching box radio frequency power and reactant gases is complementary, and provocative reaction gas produces plasma body.
For the ease of the plasma body situation of observing response inside cavity, can establish a viewing window at shell.Reactant gases enters into described reaction cavity by described inlet mouth; Under vacuum condition, described reactant gases is excited by rf wave to be plasma state, and generates nano particle continuously; Described nano particle flows out by described air outlet and is collected; Described reactant gases comprises reactant gas source and rare gas element, and described reactant gas source comprises the chlorosilane for the preparation of nano silicon particles, for the preparation of germane or the chlorine germane of germanium nano particle; When using chlorosilane or chlorine germane, hydrogen also needs to be used simultaneously; Described rare gas element comprises argon gas, helium or neon; When needs when nano-particle doped, can also in plasma chamber, feed impurity gas, impurity gas can be the gas that contains the 5th main group element or the 3rd main group element, as phosphine.
Only be several embodiment of the present invention below, but the present invention is not limited to this, the some distortion according to inventive concept has been done all should be considered as protection scope of the present invention.Adjust the size of reaction cavity, can change the residence time of reaction particles in cavity, obtain the nano particle of different size.
Claims (10)
1. the plasma enhanced chemical vapor deposition method of a common electrode and device, it is characterized in that, being included in empty enclosure in arranges successively and establishes and several side plates that the center overlaps, respectively as first electrode (1), several electrodes (2) and tail electrode (3), be provided with cavity between described adjacent first electrode (1), an electrode (2) and the tail electrode (3), cavity is provided with inlet mouth (4) and air outlet (5); Described first electrode (1) links to each other with radio-frequency power supply with the match box of outside by lead, as radio-frequency electrode; Described tail electrode (3) links to each other with the earth, as ground electrode.
2. the plasma enhanced chemical vapor deposition method of common electrode according to claim 1 and device is characterized in that, described first electrode (1), several electrodes (2) and tail electrode (3) all are located in the rectangular enclosure empty in.
3. the plasma enhanced chemical vapor deposition method of common electrode according to claim 1 and device is characterized in that, described first electrode (1), an electrode (2) be identical with tail electrode (3) shape, vary in size, the center overlaps.
4. the plasma enhanced chemical vapor deposition method of common electrode according to claim 1 and device is characterized in that, the spacing between described several electrodes (2) is the 5-50 millimeter.
5. the plasma enhanced chemical vapor deposition method of common electrode according to claim 1 and device is characterized in that, described first electrode (1), an electrode (2) and tail electrode (3) are the symmetry structure.
6. the plasma enhanced chemical vapor deposition method of common electrode according to claim 5 and device is characterized in that, described first electrode (1), an electrode (2) and tail electrode (3) are square structure.
7. the plasma enhanced chemical vapor deposition method of common electrode according to claim 1 and device is characterized in that, described inlet mouth (4) and air outlet (5) are located at the two ends of respective chamber respectively.
8. the plasma enhanced chemical vapor deposition method of common electrode according to claim 1 and device is characterized in that, the material of described first electrode (1) or tail electrode (3) is copper or stainless steel.
9. the plasma enhanced chemical vapor deposition method of common electrode according to claim 1 and device, it is characterized in that, the internal surface of the surface of described electrode (2) and first electrode (1), tail electrode (3) is coated with insulation layer, and the material of described insulation layer is silicon nitride, borosilicate, silicon-dioxide, silicon carbide or poly-acetic acid fat-aluminum oxide.
10. one kind is utilized the plasma enhanced chemical vapor deposition method of the described common electrode of claim 1 and the method that device prepares nano particle, it is characterized in that comprise: reactant gases enters into described reaction cavity by described inlet mouth; Under vacuum condition, described reactant gases is excited by rf wave to be plasma state, and generates nano particle continuously; Described nano particle flows out by described air outlet and is collected; Described reactant gases comprises reactant gas source and rare gas element, and described reactant gas source comprises the chlorosilane for the preparation of nano silicon particles, for the preparation of germane or the chlorine germane of germanium nano particle; When using chlorosilane or chlorine germane, hydrogen also needs to be used simultaneously; Described rare gas element comprises argon gas, helium or neon; When needs when nano-particle doped, can also in plasma chamber, feed impurity gas, impurity gas can be the gas that contains the 5th main group element or the 3rd main group element, as phosphine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617176A (en) * | 2015-02-10 | 2015-05-13 | 陕西师范大学 | Silicon-based thin-film solar cell and preparation method thereof |
| CN108950515A (en) * | 2018-06-19 | 2018-12-07 | 上海治臻新能源装备有限公司 | A kind of fuel battery metal pole plate carbon-base coating preparation facilities based on PECVD |
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| CN1786262A (en) * | 2005-11-07 | 2006-06-14 | 东华大学 | Method of atmospheric pressure plane discharge chemical gaseous phase depositing nano-particular film and its device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104617176A (en) * | 2015-02-10 | 2015-05-13 | 陕西师范大学 | Silicon-based thin-film solar cell and preparation method thereof |
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Application publication date: 20130911 |