CN203339107U - Arc discharge-plasma combined device used for preparing nanometer silicon powder - Google Patents
Arc discharge-plasma combined device used for preparing nanometer silicon powder Download PDFInfo
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- CN203339107U CN203339107U CN2013202857570U CN201320285757U CN203339107U CN 203339107 U CN203339107 U CN 203339107U CN 2013202857570 U CN2013202857570 U CN 2013202857570U CN 201320285757 U CN201320285757 U CN 201320285757U CN 203339107 U CN203339107 U CN 203339107U
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Abstract
The utility model discloses an arc discharge-plasma combined device used for preparing nanometer silicon powder. The arc discharge-plasma combined device used for preparing nanometer silicon powder is characterized by comprising an arc discharge apparatus and a plasma generator, wherein the arc discharge apparatus and the plasma generator are connected through a pipeline and valve. The combined device described in the utility model is characterized in that silicon rods formed by high-purity semiconductors (9N grade crystalline silicon) or solar energy grade (6N grade crystalline silicon) semiconductors through ingot casting operation can be directly adopted; a core-shell-structure silicon nanocomposite material can be obtained by adopting an arc discharge step, a hot plasma gasification step, an activating treatment step, a grafting reaction step and the like; a high finished product conversion rate and high purity are achieved; a simple and easy-to-do preparation method can be realized by using the device, and the arc discharge-plasma combined device is suitable for large scale production.
Description
Technical field
The utility model belongs to the plasma technology field, is specifically related to a kind of arc discharge that is used for preparing nano silica fume-plasma set composite.
Background technology
Existing nano-silicon preparation method can be summed up as two class methods: first kind method is that the little molecule of cracking forms nano-silicon particle (Bottom Up).Usually with silane (SiH
4) energy of using high power laser light or plasma for raw material carries out dehydrogenation, and the Si-H bond fission is generated to Si-Si key, silicon core (Si
x), so that the silicon particle.The common fault of these class methods be dehydrogenation not exclusively, raw material low conversion rate, productive rate be low.Due to incomplete dehydrogenation, product often includes the gas of harmfulness, such as unreacted unstrpped gas (SiH
4), the accessory substance hydrogen (H of reaction intermediate poly silane and dehydrogenation reaction
2).These flammable explosive gas affects safety production.The Equations of The Second Kind method is silico briquette to be carried out to the mechanical crushing ball milling become nano particle (Top Down).The shape of particle of this method output is irregular, size distribution is inhomogeneous.In addition, the long productive rate of time of mechanical ball-milling method production nanometer particle is low.Be not suitable for industrial-scale production.
Existing method is all the silica flours that make Nano grade, and the nano-silicon specific area is large, and the reactions such as oxidation very easily occur, and is difficult for preserving.
Summary of the invention
The purpose of this utility model is to provide a kind of arc discharge that is used for preparing nano silica fume-plasma set composite; can directly adopt the silicon rod of high-purity semiconductor (9N level crystal silicon) or solar level (6N level crystal silicon) ingot casting; adopt the steps such as arc discharge, high-temperature plasma gasification, activation processing, graft reaction to obtain a kind of nucleocapsid structure silicon nano composite material; finished product conversion ratio and purity are higher; use this device preparation method simple, be applicable to large-scale production.
For realizing above-mentioned utility model purpose, the utility model has adopted following technical scheme:
A kind of arc discharge that is used for preparing nano silica fume-plasma set composite is characterized in that comprise arc discharge device and plasma generator, described arc discharge device is connected with valve by pipeline with plasma generator.
Further, described arc discharge device comprises the cavity that holds sparkover, described cavity one end is communicated with the pipeline entered for dielectric material, the cavity other end is communicated with the first collecting chamber, also comprise the first electrode of being placed in cavity, the second electrode and with the pulse power of the first electrode, the second electrode conduction; Described the second electrode is connected with the rotation motor that makes the second electrode rotary, and described the first electrode is connected with the stepper motor that the first electrode is moved forward and backward.
Its generation voltage of the described pulse power puts on the first electrode and the second electrode and makes it to produce sparkover; The described pulse power is any in rotary pulsed power source generator (Rotary Impulse Generator), relaxation power source generator (Relaxation Generator), pulse power generator (Pulse Generator) and hydridization power source generator (Hybird Generator).
Further, described plasma generator comprises the cavity of hollow, and described cavity upper end is provided with the air curtain that the dog-house that enters for the silica flour material and protective atmosphere pass into; Described inside cavity is divided into upper, middle, and lower part, and the first half is combustion chamber, and mid portion is the graft reaction chamber, and the latter half is the precipitation chamber; In described combustion chamber, quartz ampoule is housed, the quartz ampoule periphery is wound with discharge coil, and described discharge coil is circumscribed with power supply; In quartz ampoule, it is plasma arc; Described quartz ampoule upper end connects dog-house and air curtain inlet end; The plasma arc lower end is located in the graft reaction chamber, and the graft reaction cavity wall is provided with the admission line that passes into active gases and graft reaction gas from outside, and the nozzle of described active gases admission line is towards the plasma arc lower end.
Further, the bulk of the nano material that described the first electrode is required preparation, its face of cylinder that is spill near the one side of the second electrode; Described the second electrode is cylinder surface; The spacing of the concave cylindrical face of the cylinder surface of described the second electrode and the first electrode is 0.8 ~ 1.2mm.
Further, described dog-house upper end is connected with pipeline with the outlet of the first collecting chamber, and described pipeline is provided with the first valve.
Further, the chamber outer wall of described plasma generator is provided with cooling device, and described cooling device is the pipeline that cooling water is housed.
Further, the admission line of described graft reaction gas is located at the below of active gases admission line.
Further, the outlet of lower end, described precipitation chamber is connected with the second collecting chamber, is provided with screen cloth in described the second collecting chamber, the nano silica fume prepared for collection.
The utility model advantage:
The arc discharge that is used for preparing nano silica fume described in the utility model-plasma set composite has following advantage:
Can directly adopt the silicon rod of high-purity semiconductor (9N level crystal silicon) or solar level (6N level crystal silicon) ingot casting; adopt the steps such as arc discharge, high-temperature plasma gasification, activation processing, graft reaction to obtain a kind of nucleocapsid structure silicon nano composite material; finished product conversion ratio and purity are higher; use this device preparation method simple, be applicable to large-scale production.
The accompanying drawing explanation
The structural representation that Fig. 1 is the arc discharge that is used for preparing nano silica fume described in the utility model-plasma set composite;
Wherein: 1, stepper motor; 2, protective gas admission line; 3, the first electrode; 4, the second electrode; 5, rotation motor; 6, arc chamber; 7, the pulse power; 8, the first precipitation chamber; 9, the first collecting chamber; 10, the first valve, 11, powder feeding gas admission line, 12, dog-house, 13, the second valve, 14, air curtain, 15, discharge coil, 16, quartz ampoule, 17, plasma arc, 18, combustion chamber, 19, power supply, 20, the activated gas admission line, 21, grafting gas inlet pipe road, 22, activation chamber, 23, the graft reaction chamber, 24, the precipitation chamber, 25, cooling device, the 26, second collecting chamber.
Embodiment
Below in conjunction with accompanying drawing and a preferred embodiment, the technical solution of the utility model is further described.
Embodiment 1:
As shown in Figure 1: a kind of arc discharge that is used for preparing nano silica fume-plasma set composite, it is characterized in that, comprise arc discharge device and plasma generator, described arc discharge device is connected with valve by pipeline with plasma generator.
Described arc discharge device comprises the cavity that holds sparkover, described cavity one end is communicated with the pipeline entered for dielectric material, the cavity other end is communicated with the first collecting chamber 9, also comprise the first electrode 3 of being placed in cavity, the second electrode 4 and with the pulse power 7 of the first electrode 3, the second electrode 4 conductings; Described the second electrode 4 is connected with the rotation motor 5 that makes the second electrode 4 rotations, and described the first electrode 3 is connected with the stepper motor 1 that the first electrode 3 is moved forward and backward.
The described pulse power 7 its generation voltages put on the first electrode and the second electrode and make it to produce sparkover; The described pulse power is any in rotary pulsed power source generator (Rotary Impulse Generator), relaxation power source generator (Relaxation Generator), pulse power generator (Pulse Generator) and hydridization power source generator (Hybird Generator).
Described plasma generator comprises the cavity of hollow, and described cavity upper end is provided with the air curtain 14 that the dog-house 12 that enters for the silica flour material and protective atmosphere pass into; Described inside cavity is divided into upper, middle, and lower part, and the first half is combustion chamber 18, and mid portion is graft reaction chamber 23, and the latter half is precipitation chamber 24; In described combustion chamber 18, quartz ampoule 16 is housed, quartz ampoule 16 peripheries are wound with discharge coil 15, and described discharge coil 15 is circumscribed with power supply 19; In quartz ampoule 16, it is plasma arc 17; Described quartz ampoule 16 upper ends connect dog-house 12 and air curtain 14 inlet ends; Plasma arc 17 lower ends are located in graft reaction chamber 23, and graft reaction chamber 23 inwalls are provided with the admission line 21 that passes into active gases admission line 20 and graft reaction gas from outside, and the nozzle of described active gases admission line 20 is towards plasma arc 17 lower ends.
The bulk of the nano material that described the first electrode 3 is required preparation, its face of cylinder that is spill near the one side of the second electrode 4; Described the second electrode 4 is cylinder surface; The spacing of the concave cylindrical face of the cylinder surface of described the second electrode 4 and the first electrode 3 is 1mm.
Described dog-house 12 upper ends are connected with pipeline with the outlet of the first collecting chamber 9, and described pipeline is provided with the first valve 10.
The chamber outer wall of described plasma generator is provided with cooling device 25, and described cooling device 25 is for being equipped with the pipeline of cooling water.
The admission line 21 of described graft reaction gas is located at the below of active gases admission line 20.
The 24 lower end outlets of described precipitation chamber are connected with the second collecting chamber 26, in described the second collecting chamber 26, are provided with screen cloth, the nano silica fume prepared for collection.
The method that application the present embodiment prepares nano silica fume is as follows:
The electrode used therein material is the doped silicon polycrystalline material, and resistivity is 0.0002 ~ 0.0004 ohmcm, and the diameter of the second electrode 4 silicon rods is 2.54cm, and length is 10.0cm; The first electrode 3 is the rectangle of concave cylindrical face for having one side, and its width is 2.54cm, is highly 5cm, and length is 9cm.The first electrode 2 rotates under connected rotation motor 3 drives, and rotating speed is 30 rev/mins; After sparkover each time, stepper motor 1 moves the first electrode 3, makes it and the second electrode 4 contact short circuits, and mobile the first electrode 3 retreats to the electrode spacing set again afterwards, is made as 1mm, carries out next sparkover.
Introduce argon gas by protective gas admission line 2, argon pressure is 20Psi; Keeping the arc discharge device cavity internal pressure is 100mTorr; Start the Pulse Generator type pulse power 7.Pulse frequency is made as 200Hz, and the interpulse break time, (Reverse Time) was made as 5 microseconds, and power is made as 5kW.Can observe the continuous Spark Discharges of generation between the first electrode 3, the second electrode 4, and have particle to produce, be collected by the first collecting chamber 9.
The plasma generator cavity vacuumizes and in cavity, is filled with argon gas afterwards.After the circulation, in cavity, be ar gas environment several times.Regulate the cavity air pressure between 0.1-0.5MPa.Open plasma power supply 19, and regulation voltage and electric current are respectively 100-200V and 50-200A; After plasma power is stable, the micron order silica flour prepared is sent in dog-house 12, from air curtain 14, the micron order silica flour in dog-house 12 is introduced to combustion chamber 18 by the argon gas stream that contains 5% phosphine.The powder feeding gas rate of flow of fluid is made as 100slpm, and air curtain 14 argon gas flow velocitys are made as 600slpm.In plasma arcs 17, generation phosphorus and hydrogen occur to decompose in phosphine.Micron silicon grain generating gasification.Under the effect of cooling blast, silicon and phosphorus nucleation also grow into particle.Active gases admission line 20 at the afterbody of plasma arcs 17 is introduced ammonias, and concentration is 10%, and hydrogenation treatment is carried out in silicon grain surface.In the graft reaction chamber, introduce grafting gas acetylene, concentration is 10%, flow velocity is 300slpm, introduces graft reaction gas from the admission line 21 of graft reaction gas the silicon particle hydrogenation treatment is carried out to graft reaction, forms shell.Finished product is collected in the second collecting chamber 26.Through check analysis, productive rate reaches 800 Grams Per Hours, and the silicon particle is spherical, and average diameter is 50 nanometers.
It is to be noted; as described above is only in order to explain the preferred embodiment of the utility model; not attempt is done any formal restriction to the utility model according to this; be with; all any modification or changes that the relevant the utility model of doing under identical utility model spirit is arranged, all must be included in the category that the utility model is intended to protection.
Claims (8)
1. the arc discharge that is used for preparing nano silica fume-plasma set composite, is characterized in that, comprise arc discharge device and plasma generator, described arc discharge device is connected with valve by pipeline with plasma generator.
2. the arc discharge that is used for preparing nano silica fume according to claim 1-plasma set composite, it is characterized in that, described arc discharge device comprises the cavity that holds sparkover, described cavity one end is communicated with the pipeline entered for dielectric material, the cavity other end is communicated with the first collecting chamber, also comprise the first electrode of being placed in cavity, the second electrode and with the pulse power of the first electrode, the second electrode conduction; Described the second electrode is connected with the rotation motor that makes the second electrode rotary, and described the first electrode is connected with the stepper motor that the first electrode is moved forward and backward.
3. the arc discharge that is used for preparing nano silica fume according to claim 2-plasma set composite, it is characterized in that, described plasma generator comprises the cavity of hollow, and described cavity upper end is provided with the air curtain that the dog-house that enters for the silica flour material and protective atmosphere pass into; Described inside cavity is divided into upper, middle and lower three parts, and the first half is combustion chamber, and mid portion is the graft reaction chamber, and the latter half is the precipitation chamber; In described combustion chamber, quartz ampoule is housed, the quartz ampoule periphery is wound with discharge coil, and described discharge coil is circumscribed with power supply; In quartz ampoule, it is plasma arc; Described quartz ampoule upper end connects dog-house and air curtain inlet end; The plasma arc lower end is located in the graft reaction chamber, and the graft reaction cavity wall is provided with the admission line that passes into active gases and graft reaction gas from outside, and the nozzle of described active gases admission line is towards the plasma arc lower end.
4. the arc discharge that is used for preparing nano silica fume according to claim 3-plasma set composite, is characterized in that, the bulk of the nano material that described the first electrode is required preparation, its face of cylinder that is spill near the one side of the second electrode; Described the second electrode is cylinder surface; The spacing of the concave cylindrical face of the cylinder surface of described the second electrode and the first electrode is 0.8 ~ 1.2mm.
5. the arc discharge that is used for preparing nano silica fume according to claim 4-plasma set composite, is characterized in that, described dog-house upper end is connected with pipeline with the outlet of the first collecting chamber, and described pipeline is provided with the first valve.
6. the arc discharge that is used for preparing nano silica fume according to claim 5-plasma set composite, is characterized in that, the chamber outer wall of described plasma generator is provided with cooling device, and described cooling device is the pipeline that cooling water is housed.
7. the arc discharge that is used for preparing nano silica fume according to claim 6-plasma set composite, is characterized in that, the admission line of described graft reaction gas is located at the below of active gases admission line.
8. the arc discharge that is used for preparing nano silica fume according to claim 7-plasma set composite, it is characterized in that, the outlet of lower end, described precipitation chamber is connected with the second collecting chamber, is provided with screen cloth in described the second collecting chamber, the nano silica fume prepared for collection.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103730319A (en) * | 2013-12-23 | 2014-04-16 | 苏州市奥普斯等离子体科技有限公司 | Novel powder plasma processing device |
| CN106698437A (en) * | 2017-01-03 | 2017-05-24 | 昆明理工大学 | Method for preparing spherical nanometer silicon by virtue of thermal plasma method |
| CN107186209A (en) * | 2017-06-09 | 2017-09-22 | 中国航天空气动力技术研究院 | High frequency plasma heater for high-temperature metal powder nodularization |
| CN108101060A (en) * | 2018-01-23 | 2018-06-01 | 湖南久泰冶金科技有限公司 | Plasma atomization prepares the device of lithium ion battery with high energy density nano-silicon |
| CN113304848A (en) * | 2021-07-08 | 2021-08-27 | 江苏鑫华半导体材料科技有限公司 | Silicon block crushing device and using method thereof, and silicon block crushing method and application method thereof |
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2013
- 2013-05-23 CN CN2013202857570U patent/CN203339107U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103730319A (en) * | 2013-12-23 | 2014-04-16 | 苏州市奥普斯等离子体科技有限公司 | Novel powder plasma processing device |
| CN106698437A (en) * | 2017-01-03 | 2017-05-24 | 昆明理工大学 | Method for preparing spherical nanometer silicon by virtue of thermal plasma method |
| CN107186209A (en) * | 2017-06-09 | 2017-09-22 | 中国航天空气动力技术研究院 | High frequency plasma heater for high-temperature metal powder nodularization |
| CN107186209B (en) * | 2017-06-09 | 2022-03-22 | 云航时代(重庆)科技有限公司 | High-frequency plasma heater for spheroidizing high-temperature metal powder |
| CN108101060A (en) * | 2018-01-23 | 2018-06-01 | 湖南久泰冶金科技有限公司 | Plasma atomization prepares the device of lithium ion battery with high energy density nano-silicon |
| CN108101060B (en) * | 2018-01-23 | 2023-12-15 | 湖南久泰冶金科技有限公司 | Device for preparing high-energy-density lithium ion battery nano silicon by plasma atomization |
| CN113304848A (en) * | 2021-07-08 | 2021-08-27 | 江苏鑫华半导体材料科技有限公司 | Silicon block crushing device and using method thereof, and silicon block crushing method and application method thereof |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131211 Termination date: 20180523 |