CN103343331A - Chemical vapor deposition reaction device - Google Patents
Chemical vapor deposition reaction device Download PDFInfo
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- CN103343331A CN103343331A CN2013102733125A CN201310273312A CN103343331A CN 103343331 A CN103343331 A CN 103343331A CN 2013102733125 A CN2013102733125 A CN 2013102733125A CN 201310273312 A CN201310273312 A CN 201310273312A CN 103343331 A CN103343331 A CN 103343331A
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- chemical vapour
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 183
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 48
- 239000000758 substrate Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 18
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000007789 sealing Methods 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 238000005234 chemical deposition Methods 0.000 abstract description 2
- 238000000265 homogenisation Methods 0.000 abstract 3
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 18
- 238000000151 deposition Methods 0.000 description 17
- 229910052786 argon Inorganic materials 0.000 description 11
- 239000002245 particle Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005243 fluidization Methods 0.000 description 2
- 238000003331 infrared imaging Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012802 pre-warming Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a chemical vapor deposition reaction device comprising an upper end cover, a reaction tube and a lower end cover, wherein a feed opening and an air outlet are formed in the upper end cover; a micropore distribution plate is arranged in the reaction tube, a plurality of punch holes are formed in the micropore distribution plate, the reaction tube is divided into an upper fluidized bed reaction chamber and a lower fixed bed homogenization chamber by the micropore distribution plate, an electric furnace is sleeved outside the fixed bed homogenization chamber of the reaction tube, metal wires are winded outside the fluidized bed reaction chamber of the reaction tube, and the upper end of the reaction tube is connected with the upper end cover through an upper sealing sleeve; and an air inlet is formed in the lower end cover, and the lower end cover is connected to the lower end of the reaction tube through a lower sealing sleeve. The chemical vapor deposition reaction device disclosed by the invention provides uniform temperature field and concentration field through the fluidized bed reaction chamber at the upper part of the reaction tube and is used for quickly preheating, uniformly mixing and stabilizing the flow of the air through the fixed bed homogenization chamber at the lower part of the reaction tube; according to the chemical vapor deposition reaction device, the homogeneity of chemical reaction and deposition is improved and the quality of a deposited material is also improved.
Description
Technical field
The present invention is relevant for a kind of reaction unit, especially relevant for the device of the chemical vapour deposition reaction in a kind of technical field of chemical.
Background technology
Preparing material by chemical vapour deposition technique has the following advantages: (1) synthetic materials under far below the temperature of material melting point; (2) composition of synthetic materials, structure and microscopic appearance are controlled; (3) do not need sintering aid, can synthesize high-purity, high density material; (4) can realize the material micron level, even nano level control; (5) can prepare gradient composites, gradient cladding etc.At present, chemical vapour deposition technique is widely used in preparing optoelectronic film, corrosion-resistant finishes/film, carbon nanotube and particle surface modification etc.The core of chemical vapour deposition technique is its reaction unit.The structure composition of reaction unit, energy supply mode, reaction conditions observing and controlling situation all can influence the quality, efficient, performance etc. of preparation material.Therefore, chemical vapour deposition reaction Design of device structure is very crucial.
Fluidized-bed-chemical vapour deposition provides the space and uniform temperature field, concentration field of abundant reaction for chemical vapour deposition reaction, can greatly improve deposition quality.The important feature of fluidized-bed reactor is to be easy to realize successive reaction, large-scale production.But the fluidized-bed chemical vapor deposition type of reactor of use is more at present, and textural difference is bigger, and the structure of reactor is comparatively complicated usually, and inconvenience processing, dismounting and cleaning are unfavorable for life-time service.
In addition, at present the chemical vapour deposition reaction device adopts the resistance wire heating that energy source is provided usually, and the temperature of preparation material is all higher relatively, has caused the wasting of resources, cost height, efficient low.During chemical vapour deposition reaction gas handle without the preheating homogenizing usually or do not carry out temperature, the control of concentration homogeneity is handled and has just been participated in reaction directly, makes material be prone to problems such as component segregation, became uneven, has influenced quality and the performance of material.Because the instantaneous rising of temperature when gas enters reactor generation deposition reaction continuously, volume sharply expands, cause reaction compartment atmosphere fluctuating range big, influenced the deposition reaction process, the temperature of gas when especially preparing the large area film material, concentration homogeneity are bigger to the influence of the performance of material and quality.Usually the state of fluidized particles is difficult to real-time grasp in the fluidized-bed under the situation of high temperature successive reaction, is unfavorable for the continuous regulation and control of fluidized, can influence the stability of deposition reaction.
Therefore, be necessary to provide a kind of new reaction unit, to address the above problem.
Summary of the invention
The device that the purpose of this invention is to provide a kind of chemical vapour deposition reaction, it utilizes the fluidized-bed reaction chamber on reaction tubes top that uniform temperature field and concentration field are provided, and the fixed bed levelling chamber that passes through the reaction tubes bottom handles gas rapidly pre-warming, mixing and current stabilization, the device of this chemical vapour deposition reaction has improved the homogeneity of chemical reaction and deposition, has improved the quality of deposition material.
Above-mentioned purpose of the present invention can adopt following technical proposal to realize:
The invention provides a kind of device of chemical vapour deposition reaction, the device of described chemical vapour deposition reaction comprises:
Upper end cover offers opening for feed and air outlet on it;
Reaction tubes, be provided with the micropore grid distributor in it, offer a plurality of perforation on the described micropore grid distributor, described reaction tubes is divided into upper fluid-bed reaction chamber and lower fixed bed levelling chamber by described micropore grid distributor, the outer cover of the fixed bed levelling chamber of described reaction tubes is provided with electric furnace, the fluidized-bed reaction outdoor of described reaction tubes is wound with wire, and the upper end of described reaction tubes links to each other with described upper end cover by upper sleeve gasket;
Lower end cover, it offers inlet mouth, and described lower end cover is connected the lower end of described reaction tubes by lower sleeve gasket.
In preferred embodiment, the diameter of the perforation of offering on the described micropore grid distributor is 10～100 μ m.
In preferred embodiment, be provided with container in the described fixed bed levelling chamber, described container seat is located in the described lower end cover.
In preferred embodiment, described upper end cover is provided with the infrared thermoviewer window.
In preferred embodiment, the outside described wiry that is wrapped in the fluidized-bed reaction outdoor of described reaction tubes is provided with the heat-insulation and heat-preservation body.
In preferred embodiment, the outside surface of described upper end cover and the outside surface of the described lower end cover water jacket that has been sticked respectively.
In preferred embodiment, be provided with thermopair in the described fixed bed levelling chamber, the end that described thermopair passes described lower end cover is connected with temperature sensor and pressure transmitter.
In preferred embodiment, described upper end cover links to each other with a vacuum pump by valve tube respectively with described lower end cover.
In preferred embodiment, the inwall of the fluidized-bed reaction chamber of described reaction tubes is provided with substrate slot and places bank, and substrate slot is placed on the bank and is placed with substrate slot.
In preferred embodiment, the device of described chemical vapour deposition reaction also comprises support, and described lower end cover is fixedly connected on the lower end of described support, and described upper end cover can be connected the upper end of described support axially slidably.
Apparatus features and the advantage of chemical vapour deposition reaction of the present invention are:
One, the device of chemical vapour deposition reaction of the present invention, its reaction tubes is a simple silica tube with micropore grid distributor, it is easy to use, the micropore grid distributor is divided into upper fluid-bed reaction chamber and lower fixed bed levelling chamber with reaction tubes, wherein, utilize efficient heat transfer, the mass transfer function of the fluidized-bed reaction chamber on reaction tubes top, for the chemical vapour deposition reaction space provides uniform temperature field, concentration field, and fixed bed levelling chamber can be used for the preheating mixing of reactant gases, further improve the homogeneity of deposition material composition, improved the performance of preparation material.In addition, the present invention adopts wire that the gas in the fluidized-bed reaction chamber is carried out ionization, with the plasma body that the produced energy source as reaction, has significantly reduced the temperature of deposition reaction, has improved the efficient of deposition reaction greatly.
Two, the device of chemical vapour deposition reaction of the present invention, the infrared thermoviewer window of offering on the upper end cover, by the macroscopical temperature of outside infrared thermoviewer from infrared thermoviewer windows detecting reaction tubes ionic medium zone, and carry out the fluidized particles infrared imaging and observe, deposition reaction is carried out the fluidized state of temperature detection and regulation and control fluidized-bed reaction indoor particle, guarantee the stability of deposition reaction, and then improve the quality of deposition material.
Three, the device of chemical vapour deposition reaction of the present invention is sticked respectively at the water jacket of the outside surface of the outside surface of upper end cover and lower end cover, can play cooling effect, prevents that thermal radiation is big and influences the upper sleeve gasket of reaction tubes and lower sleeve gasket to the sealing of reaction tubes; Simultaneously, this water jacket also can carry out cooling process to the tail gas from upper end cover and lower end cover discharge.
Description of drawings
In order to be illustrated more clearly in the technical scheme in the embodiment of the invention, the accompanying drawing of required use is done to introduce simply in will describing embodiment below, apparently, accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the front view of the device of chemical vapour deposition reaction of the present invention.
Fig. 2 is the stereographic map of substrate slot of the device of chemical vapour deposition reaction of the present invention.
Fig. 3 is the front view of support of the device of chemical vapour deposition reaction of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
As shown in Figure 1, the invention provides a kind of device of chemical vapour deposition reaction, it comprises upper end cover 1, reaction tubes 2 and lower end cover 3.Wherein: offer opening for feed 11 and air outlet 12 on the upper end cover 1; Be provided with micropore grid distributor 21 in the reaction tubes 2, offer a plurality of perforation (not shown)s on the described micropore grid distributor 21, described reaction tubes 2 is divided into upper fluid-bed reaction chamber 22 and lower fixed bed levelling chamber 23 by described micropore grid distributor 21, the outer cover of the fixed bed levelling chamber 23 of described reaction tubes 2 is provided with electric furnace 4,22 outsides, fluidized-bed reaction chamber of described reaction tubes 2 are wound with wire 5, and the upper end of described reaction tubes 2 links to each other with described upper end cover 1 by upper sleeve gasket 24; Lower end cover 3 offers inlet mouth 31, and described lower end cover 3 is connected the lower end of described reaction tubes 2 by lower sleeve gasket 25.
Specifically be, upper end cover 1 is cone shape substantially, offers opening for feed 11 and air outlet 12 on it, and upper end cover 1 is sealedly connected on the upper end of reaction tubes 2 by upper sleeve gasket 24, the intracavity inter-connection of its opening for feed 11, air outlet 12 and reaction tubes 2.
In one embodiment of this invention, it is as follows to prepare the process of carbon nanotube with the device of this chemical vapour deposition reaction:
At first, container 231 is placed in the lower end cover 3, fills an amount of inertia macrobead in container 231, the oarse-grained median size of those inertia is 2～5mm; Afterwards, with the Ni/MgO granules of catalyst of a certain amount of 10%wt, its particle diameter is 100～300 μ m, is placed in the fluidized-bed reaction chamber 22 of reaction tubes 2; Upper end cover 1 and lower end cover 3 are sealed in the upper end of reaction tubes 2 and the lower end of reaction tubes 2.
After the device assembling for the treatment of chemical vapour deposition reaction finishes, open vacuum pump 7 and valve 321, vacuumized 2 minutes from the lower end of reaction tubes 2, then, open valve 131 again, vacuumized 5 minutes from the upper end of reaction tubes 2, with the air in the quick eliminating reaction tubes 2; Afterwards, begin to feed argon gas (Ar) from the inlet mouth 31 of lower end cover 3, argon gas flows in the reaction tubess 2 through lower end cover 3, through the fixed bed levelling chamber 23 of reaction tubes 2, on the micropore grid distributor 21 a plurality of perforation and flow in the fluidized-bed reaction chamber 22 of reaction tubes 2; At this moment, increasing tolerance gradually fully contacts the Ni/MgO granules of catalyst in argon gas and the fluidized-bed reaction chamber 22; Then, electric preheating furnace 4 makes electric furnace 4 be warmed up to 450 ℃, at this moment, opens the external radio frequency producer, and by wire 5 heated fluidized bed reaction chambers 22, ionization of gas also produces plasma body, so that the temperature in the fluidized-bed reaction chamber 22 rises to 450～500 ℃; Afterwards, the inlet mouth 31 from lower end cover 3 feeds hydrogen (H
2), the granules of catalyst after the fluidisations is fully contacted and carry out reduction reaction, so that the transiting metal oxidation particle is reduced to the elemental metals nano particle.In this embodiment, the volume ratio of argon gas and hydrogen is 7:3, and the time that the catalyzer after the fluidisation carries out reduction reaction is 30～60 minutes.
At last, feed carbon source gas (methane CH for example from the inlet mouth 31 of lower end cover 3
4), wherein, Ar, H
2, CH
4Volume ratio be 10:1:1, react after 40～60 minutes, close external radio frequency producer and electric furnace 4, at this moment, only feed argon shield and be cooled to room temperature; At last, carrier granule is carried out cleanup acid treatment and just can obtain high-quality carbon nanotube.
In another embodiment of the present invention, convex with substrate slot on the inwall of the fluidized-bed reaction chamber 22 of described reaction tubes 2 and place bank 221, substrate slot is placed on the bank 221 and is placed with substrate slot 26, sees also shown in Figure 2.When the device by this chemical vapour deposition reaction prepares diamond like carbon film:
At first, container 231 is placed in the lower end cover 3, fills an amount of inertia macrobead in container 231, the oarse-grained median size of those inertia is 2～5mm; Afterwards, put into the inertia small-particle in the fluidized-bed reaction chamber 22 of reaction tubes 2, its particle diameter is 100～300 μ m; Silicon substrate 261 is cleaned, vertically is placed in the substrate slot 26 after the processing such as oven dry, tighten the retaining screw 262 of substrate slot 26 sidewalls, the substrate slot that then substrate slot 26 is placed on reaction tubes 2 is placed on the bank 221; At last, the reaction tubes 2 of getting substrate ready is positioned over upper end cover 1 and 3 good seals of lower end cover.
After the device assembling for the treatment of chemical vapour deposition reaction finishes, adjust the position of reaction tubes 2 external metallization silks 5, its zone of action is concentrated on around the substrate slot 26; At this moment, open vacuum pump 7 and valve 321, vacuumized 2 minutes from the lower end of reaction tubes 2, then, open valve 131 again, vacuumized 5 minutes from the upper end of reaction tubes 2, with the air in the quick eliminating reaction tubes 2; Afterwards, feed argon gas (Ar) from the inlet mouth 31 of lower end cover 3, argon gas flows in the reaction tubes 2 through lower end cover 3, through the fixed bed levelling chamber 23 of reaction tubes 2, on the micropore grid distributor 21 a plurality of perforation and flow in the fluidized-bed reaction chamber 22 of reaction tubes 2, at this moment, increase tolerance gradually the gas-solid in the fluidized-bed reaction chamber 22 is fully contacted mutually, present fluidized state; Then, electric preheating furnace 4 makes electric furnace 4 be warmed up to 450 ℃, at this moment, opens the external radio frequency producer, and by wire 5 heated fluidized bed reaction chambers 22, ionization of gas also produces plasma body, so that the temperature in the fluidized-bed reaction chamber 22 rises to 450～500 ℃; Inlet mouth 31 from lower end cover 3 feeds argon gas (Ar), hydrogen (H respectively then
2) and carbon source gas (CH
4), wherein, Ar, H
2, CH
4Volume ratio be 2:1:1, react after 30 minutes, close external radio frequency producer and electric furnace 4, at this moment, only feed argon shield and be cooled to room temperature; At last, on the substrate slot 26 of substrate slot placement bank 221, can obtain diamond like carbon film.
The device of chemical vapour deposition reaction of the present invention, reaction tubes 2 is a simple silica tube with micropore grid distributor 21, it is easy to use, micropore grid distributor 21 is divided into upper fluid-bed reaction chamber 22 and lower fixed bed levelling chamber 23 with reaction tubes 2, wherein, utilize the efficient heat transfer of the fluidized-bed reaction chamber 22 on reaction tubes 2 tops, mass transfer function, for the chemical vapour deposition reaction space provides uniform temperature field, concentration field, and fixed bed levelling chamber 23 is used for the preheating mixing of reactant gases, further improve the homogeneity of deposition material composition, improved the performance of preparation material.In addition, the present invention adopts the gases in 5 pairs of fluidized-bed reaction chambers of wire 22 to carry out ionization, and with the plasma body that the produced energy source as reaction, the high reactive force of energy of plasma is strong, significantly reduce the temperature of deposition reaction, improved the efficient of deposition reaction greatly.
According to an embodiment of the invention, described upper end cover 1 is provided with infrared thermoviewer window 14.Adopt infrared thermoviewer from the infrared thermoviewer window 14 detection reaction pipes 2 ionic medium zones of upper end cover 1 (also to be, fluidized-bed reaction chamber 22) macroscopical temperature, and carry out the fluidized particles infrared imaging and observe, temperature detection and regulation and control fluidized-bed reaction chamber 22 endocorpuscular fluidized states are carried out in deposition reaction, guarantee the stability of deposition reaction, and then improve the quality of deposition material.
According to an embodiment of the invention, the outside surface of the outside surface of described upper end cover 1 and described lower end cover 3 water jacket that has been sticked respectively.This water jacket is attached to the outside surface of upper end cover 1 and the outside surface of lower end cover 3 plays cooling effect, prevents that thermal radiation from influencing the sealing of upper sleeve gasket 24 and 25 pairs of reaction tubess 2 of lower sleeve gasket of reaction tubes 2 greatly; Simultaneously, this water jacket also can carry out cooling process to the tail gas from upper end cover 1 and lower end cover 3 discharges.
According to an embodiment of the invention, be provided with thermopair 232 in the described fixed bed levelling chamber 23, the end that described thermopair 232 passes described lower end cover 3 is connected with temperature sensor 233 and pressure transmitter 234.Temperature sensor 233 and pressure transmitter 234 are by being located in the temperature and pressure in the thermopair 232 sensing fixed bed levelling chamber 23 in the fixed bed levelling chamber 23.In addition, also be connected with pressure transmitter 241 on upper sleeve gasket 24, it is used for the pressure in the fluidized-bed reaction chamber 22 of reaction tubes 2 is carried out sensing.
According to an embodiment of the invention, as shown in Figure 3, the device of described chemical vapour deposition reaction also comprises support 8, and described lower end cover 3 is fixedly connected on the lower end of described support 8, and described upper end cover 1 can be connected the upper end of described support 8 axially slidably.
Specifically be, support 8 has upper connecting rod 81 and lower connecting rod 82, and upper end cover 1 is connected on the upper connecting rod 81, and lower end cover 3 is connected on the lower connecting rod 82.Upper connecting rod 81 for example can be connected on the different heights position of support 8 by slide rail, thereby can adjust the upper level position of upper connecting rod 81 according to actual needs, so that the upper end cover 1 of dismounting reaction tubes makes things convenient for the taking-up of product and cleans repeated use.
The above only is several embodiments of the present invention, and those skilled in the art can carry out various changes or modification to the embodiment of the invention according to the disclosed content of application documents and not break away from the spirit and scope of the present invention.
Claims (10)
1. the device of a chemical vapour deposition reaction is characterized in that, the device of described chemical vapour deposition reaction comprises:
Upper end cover offers opening for feed and air outlet on it;
Reaction tubes, be provided with the micropore grid distributor in it, offer a plurality of perforation on the described micropore grid distributor, described reaction tubes is divided into upper fluid-bed reaction chamber and lower fixed bed levelling chamber by described micropore grid distributor, the outer cover of the fixed bed levelling chamber of described reaction tubes is provided with electric furnace, the fluidized-bed reaction outdoor of described reaction tubes is wound with wire, and the upper end of described reaction tubes links to each other with described upper end cover by upper sleeve gasket;
Lower end cover, it offers inlet mouth, and described lower end cover is connected the lower end of described reaction tubes by lower sleeve gasket.
2. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, the diameter of the perforation of offering on the described micropore grid distributor is 10～100 μ m.
3. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, is provided with container in the described fixed bed levelling chamber, and described container seat is located in the described lower end cover.
4. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, described upper end cover is provided with the infrared thermoviewer window.
5. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, the outside described wiry that is wrapped in the fluidized-bed reaction outdoor of described reaction tubes is provided with the heat-insulation and heat-preservation body.
6. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, the outside surface of described upper end cover and the outside surface of the described lower end cover water jacket that has been sticked respectively.
7. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, is provided with thermopair in the described fixed bed levelling chamber, and the end that described thermopair passes described lower end cover is connected with temperature sensor and pressure transmitter.
8. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, described upper end cover links to each other with a vacuum pump by valve tube respectively with described lower end cover.
9. the device of chemical vapour deposition reaction as claimed in claim 1 is characterized in that, the inwall of the fluidized-bed reaction chamber of described reaction tubes is provided with substrate slot and places bank, and substrate slot is placed on the bank and is placed with substrate slot.
10. the device of chemical vapour deposition reaction as claimed in claim 1, it is characterized in that, the device of described chemical vapour deposition reaction also comprises support, and described lower end cover is fixedly connected on the lower end of described support, and described upper end cover can be connected the upper end of described support axially slidably.
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| CN201310273312.5A CN103343331B (en) | 2013-07-02 | 2013-07-02 | Chemical vapor deposition reaction device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710684A (en) * | 2013-12-31 | 2014-04-09 | 中国航空工业集团公司北京航空制造工程研究所 | Integrated online detection system for chemical vapor deposition reaction |
| CN107377968A (en) * | 2017-09-08 | 2017-11-24 | 安徽工业大学 | A kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation |
| CN108330470A (en) * | 2018-04-16 | 2018-07-27 | 福建闽烯科技有限公司 | The chemical vapor depsotition equipment of single heating system multi-reaction chamber |
| CN110777360A (en) * | 2019-11-01 | 2020-02-11 | 西北工业大学 | A kind of feeding device of powder precursor under negative pressure of chemical vapor deposition |
| CN113005427A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Full-size SiC composite material cladding tube chemical vapor deposition device |
| CN113124683A (en) * | 2020-01-15 | 2021-07-16 | 株洲弗拉德科技有限公司 | Vacuum vapor deposition furnace with feeder |
| CN113564561A (en) * | 2020-04-29 | 2021-10-29 | 清华大学 | Powder particle coating equipment based on fluidized bed and chemical vapor deposition technology |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009112738A1 (en) * | 2008-03-11 | 2009-09-17 | Arkema France | Method and system for depositing a metal or metalloid on carbon nanotubes |
| CN201351156Y (en) * | 2008-12-23 | 2009-11-25 | 煤炭科学研究总院 | Coupling gasification device of fixed bed and fluidized bed |
| CN101817716A (en) * | 2009-02-27 | 2010-09-01 | 中国科学院过程工程研究所 | Method and device for catalyzing methanation of synthesis gas |
| CN102597294A (en) * | 2009-02-16 | 2012-07-18 | 拜耳国际有限公司 | A connection means, a method of manufacturing the same and a material connection |
-
2013
- 2013-07-02 CN CN201310273312.5A patent/CN103343331B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009112738A1 (en) * | 2008-03-11 | 2009-09-17 | Arkema France | Method and system for depositing a metal or metalloid on carbon nanotubes |
| CN201351156Y (en) * | 2008-12-23 | 2009-11-25 | 煤炭科学研究总院 | Coupling gasification device of fixed bed and fluidized bed |
| CN102597294A (en) * | 2009-02-16 | 2012-07-18 | 拜耳国际有限公司 | A connection means, a method of manufacturing the same and a material connection |
| CN101817716A (en) * | 2009-02-27 | 2010-09-01 | 中国科学院过程工程研究所 | Method and device for catalyzing methanation of synthesis gas |
Non-Patent Citations (1)
| Title |
|---|
| 恽松 等: "流化床与固定床耦合反应器中的颗粒磨损", 《过程工程学报》, vol. 10, no. 1, 28 February 2010 (2010-02-28), pages 17 - 22 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710684A (en) * | 2013-12-31 | 2014-04-09 | 中国航空工业集团公司北京航空制造工程研究所 | Integrated online detection system for chemical vapor deposition reaction |
| CN103710684B (en) * | 2013-12-31 | 2015-12-09 | 中国航空工业集团公司北京航空制造工程研究所 | A kind of integrated on-line detecting system for chemical vapour deposition reaction |
| CN107377968A (en) * | 2017-09-08 | 2017-11-24 | 安徽工业大学 | A kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation |
| CN108330470A (en) * | 2018-04-16 | 2018-07-27 | 福建闽烯科技有限公司 | The chemical vapor depsotition equipment of single heating system multi-reaction chamber |
| CN110777360A (en) * | 2019-11-01 | 2020-02-11 | 西北工业大学 | A kind of feeding device of powder precursor under negative pressure of chemical vapor deposition |
| CN113005427A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Full-size SiC composite material cladding tube chemical vapor deposition device |
| CN113124683A (en) * | 2020-01-15 | 2021-07-16 | 株洲弗拉德科技有限公司 | Vacuum vapor deposition furnace with feeder |
| CN113564561A (en) * | 2020-04-29 | 2021-10-29 | 清华大学 | Powder particle coating equipment based on fluidized bed and chemical vapor deposition technology |
| CN113564561B (en) * | 2020-04-29 | 2022-05-06 | 清华大学 | Powder particle coating equipment based on fluidized bed and chemical vapor deposition technology |
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