CN102515139A - Two-chamber vertical vacuum controllable atmosphere furnace for continuously preparing nano materials through gas-phase method - Google Patents
Two-chamber vertical vacuum controllable atmosphere furnace for continuously preparing nano materials through gas-phase method Download PDFInfo
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to the technical field of nano material synthesis equipment, and discloses a vacuum controllable atmosphere furnace capable of continuously preparing nano materials through a gas-phase method. A furnace body is designed into a two-chamber structure; the upper part of the furnace body is a reaction chamber, the lower part of the furnace body is a material taking chamber, so that a vertical structure is formed, a heat insulation sealing door is arranged between the two chambers, and the material taking and a production process of the reaction chamber can be carried out synchronously. An induction heating device is adopted to realize the high-efficiency heating to gas raw materials; an automatic material taking device is adopted to automatically take a product; the material taking process does not interrupt the production process of the reaction chamber, so that the purpose of continuously and efficiently preparing the nano materials is achieved. Compared with a traditional single-chamber furnace, the two-chamber vertical vacuum controllable atmosphere furnace for continuously preparing nano materials through the gas-phase method has the advantages of high heating efficiency and production efficiency, and energy saving.
Description
Affiliated technical field
The present invention relates generally to nano material vapor phase process synthesis device technical field; But relate to efficient, the energy-conservation controlled atmosphere generator of the vertical quantity-produced in a kind of two Room of vapor phase process continuous production nano material, this equipment can be used for the preparation and the production of carbon nanotube, one dimension carbide nanometer material etc.
Background technology
At present, nano material demonstrates wide application prospect at aspects such as magneticsubstance, electronic material, optical material, high compactedness material sintering, catalysis, sensing, ceramic toughenings, and the market of nano material enlarges year by year, and has produced huge economic benefit.The sales volume that Lux research company predicts global nanotechnology in 2015 and product will reach 2.5 trillion dollars.The BCC company that is engaged in market survey predicts from 2008 to 2014, and the nanotechnology market scale annual growth that is applied to environmental area will be 61.8%, and sales volume also will increase to 21,800,000,000 dollars in 2014 from 1,100,000,000 dollars in 2008.In January, 2010, pointed out by " the 2010-2015 China's nano material industry investment analysis and the prospect prediction address " of middle throwing consultant issue: by 2011, the demand of global nano material will reach 4,200,000,000 dollars, by 2025, will be increased to 1,000 hundred million dollars.By 2025, nano material will be well beyond original range of application, like the lapping liquid of semiconductor fabrication, the transparent superhard plastics synthetic products of sunscreen product, high-performance, other personal-care supplies, self-cleaning glass, high-grade sports equipment etc.In following 10-20, some are novel nano materials relatively, like nanotube etc., with occupying the bigger market share.Nano material market is shooting up, and also bonded is tightr for nano material and daily daily life, and its Application Areas will constantly be opened up.
Vapor phase process is present synthesizing one-dimensional, a kind of domestic method of quasi-one-dimensional nanometer material.Because the vapor phase process preparation is mostly carried out in the container of sealing; Prepared nano material is compared with the nano material of other method preparation; Has higher purity; The space of material nucleation and growth increases in gas phase, and prepared appearance of nano material homogeneous, size are little, the size range narrowly distributing, have good monodispersity.Therefore vapor phase process is one of optimized method for production of industrialized mass production one dimension, quasi-one-dimensional nanometer material.In addition, through changing reactant gases, can prepare the nano material of the various materials such as various metal nitrides, carbide, boride and carbon nanotube that liquid phase method is difficult to prepare.
The equipment that uses vapor phase process to prepare nano material at present mainly is vacuum controlled atmosphere furnace; With solid phase and gas phase is reaction raw materials; And utilize gas phase to be mostly single cell structure for the atmosphere furnace that reaction raw materials prepares nano material; Be mainly tubular oven, need blowing out get material after each preparation feedback is accomplished, prepare many walls nanotube at laboratory using single chamber horizontal pipe stove like the Li Shutang of City University of Hong Kong etc.; The patent No. adopts the single-chamber vacuum tube furnace to prepare the single or multiple lift Graphene for " CN201110153485.4 " name is called " method that a kind of chemical vapour deposition prepares individual layer and multi-layer graphene ".Tradition single chamber atmosphere furnace receives structural limitations, and each preparation all needs heating and cooling repeatedly, the waste mass energy; Be called " forvacuum special atmosphere oven " like the patent No. for " 200520096581.X " name; The patent No. is called " intermittent type atmosphere stone " for " 200610008219.1 " name, and the patent No. is called " heating quenching vacuum atmosphere oven automatically " for " 200820078861.1 " name, and the each shove charge of these atmosphere furnace all needs to heat up again; Can not be used for continuous production, cause the mass energy waste.In addition, all need manually to place substrate before the each preparation feedback of traditional one-way fired furnace, reaction finishes also to need manually to take out substrate after the blowing out, and mainly adopts the radiation heating mode, and heat is wasted on furnace wall and the substrate in a large number, and heating efficiency is low.The problems referred to above have hindered the suitability for industrialized production paces that vapor phase process prepares nano material to a certain extent.This shows that the nano material production industry presses for a kind of novel controlled atmosphere generator, this atmosphere furnace should possess characteristics such as continuous production, heating efficiency and production efficiency height.
The objective of the invention is to overcome traditional single chamber atmosphere furnace and can not be used for the continuous production nano material; Shortcomings such as and production efficiency is low, and energy utilization rate is low realize continuous production through improving structure design; Thereby enhance productivity; Change type of heating to improve heating efficiency, solve the limitation that present preparation nano material exists, promote the Industrialization Progress of nano material preparation.
Summary of the invention
The present invention has overcome the deficiency of existing nano material preparation equipment; A kind of controlled atmosphere generator that vapor phase process prepares nano material continuously that can be used for is provided; This atmosphere furnace is made up of reaction chamber and material extracting chamber's two portions, between two Room, is provided with the thermal-insulating sealing door, and body of heater adopts vertical structure can realize that automatic material taking process and reaction chamber production process carry out synchronously; This equipment adopts induction heating mode that inlet pipe is heated simultaneously; And then realize that to reactant gases and the efficient heating that has the catalyzer carrier gas deficiency such as overcoming traditional single chamber atmosphere furnace can not continuous production, production efficiency is low and heating efficiency is low promotes the industriallization progress of nano material preparation.
Technical scheme of the present invention is achieved in that Proper Design is two cell structures, and top is reaction chamber, and the bottom is a material extracting chamber, thereby constitutes vertical structure, all can realize sealing between two Room reach separately.Reaction chamber is provided with Stage microscope and scraper, between two Room, is provided with the thermal-insulating sealing door, but insulation between realization response chamber and the material extracting chamber and sealing.During production, reactant gases gets into reaction chamber through two inlet pipe of upper of furnace body respectively with the carrier gas that has catalyzer, meets and reacts; The gained solid product at first is deposited on the Stage microscope; Subsequently, scraper is transferred to product on the transport unit of material extracting chamber, and final product is discharged by the sealing door of material extracting chamber bottom through transport unit automatically; Production process with get the material process and can carry out synchronously, thereby realized the continuous production of nano material.
Heating system among the present invention is made up of induction electrode (7), graphite sleeve calorifier (19) and load coil (20); During heating; " surface action " rapid heating graphite sleeve calorifier (19) that utilizes load coil (20) to produce on graphite sleeve calorifier (19) surface; And then inlet pipe I and the inlet pipe II that stretches into reaction chamber from the body of heater top and pass graphite sleeve calorifier (19) heated, thereby the carrier gas that has catalyzer among reactant gases among the inlet pipe I and the inlet pipe II is heated.Inlet pipe I adopts the inclination that becomes 15 ° of angles with vertical direction to place design with inlet pipe II; Can realize that the two pipe mouths of pipe are adjacent; Two inlet pipe end is 50mm with Stage microscope upper surface distance; Thereby heated reactant gases and the carrier gas that has catalyzer can be reacted by thorough mixing when discharging, and the solid product that reaction obtains is deposited on the Stage microscope.
Material extracting chamber among the present invention is provided with automatic fetching device, can realize automatic material taking.Automatic fetching device is made up of material scraper, Stage microscope and travelling belt, when the thermal-insulating sealing door between reaction chamber and the material extracting chamber is opened, scrapes the material cylinder and stretches out, resets; The traction material scraper is scraped the product of getting on the Stage microscope, and product falls under gravity on material extracting chamber's travelling belt, scrapes material and finishes; The thermal-insulating sealing door is closed, and production process continues, and feeds rare gas element to a normal atmosphere to material extracting chamber; Open material extracting chamber's sealing door, start material extracting chamber's transport unit, product flows out from the material extracting chamber bottom automatically.
Be provided with the thermal-insulating sealing door between reaction chamber among the present invention and the material extracting chamber, to realize insulation and the sealing between two Room.The thermal-insulating sealing door is provided with four guide deflection sheaves, and guide deflection sheave can reciprocatingly slide in track, through the keying that the thermal-insulating sealing door cylinder stretches out, homing action is realized the thermal-insulating sealing door.
Reaction chamber among the present invention and material extracting chamber are equipped with vacuum-pumping tube and inert protective gas ventpipe.Vacuum-pumping tube is connected with the vacuum unit, realizes vacuumizing reaction chamber and material extracting chamber; The inert protective gas ventpipe is connected with inertia protection gas bottle, for body of heater feeds inert protective atmosphere.
Reaction chamber is provided with vapor pipe among the present invention, and vapor pipe is connected with emission-control equipment, realizes the safe handling to waste gas.Vapor pipe is in reactor top, is beneficial to the discharge of waste gas.High-temp waste gas gets into water cooling heat exchanger through vacuum breaker and obtains cooling, and the inflow exhaust gas treatment soln is discharged through after the reaction treatment, and the production that exhaust process is not interrupted nano material in the reaction chamber prepares process.
Stable and reliable structure of the present invention, heating efficiency is high, can practice thrift mass energy, has improved the efficient that vapor phase process prepares nano material effectively, has promoted the industriallization progress of nano material preparation.
Description of drawings
Fig. 1 is a body of heater one-piece construction synoptic diagram;
1-connects bearing pin; The 2-holding screw; 3-thermal-insulating sealing door cylinder; 4-scrapes the material cylinder; The 5-material scraper; 6-changes the brush bell; The 7-induction electrode; 8,9,10-holding bolt; The 11-furnace wall; The hard felt plate of 12-graphite; The 13-graphite carbon felt; 14-inlet pipe I; The 15-holding bolt; 16-thermopair anchor clamps; 17-inlet pipe II; The 18-vapor pipe; 19-graphite sleeve calorifier; The 20-load coil; The 21-thermopair; 22-reaction chamber vacuum-pumping tube; The 23-Stage microscope; 24-Stage microscope height adjuster; The 25-baffle plate; The 26-guide rail; 27-rare gas element ventpipe I; The 28-sealring; 29-thermal-insulating sealing door; 30-rare gas element ventpipe II; 31-material extracting chamber sealing door; The 32-travelling belt; 33-material extracting chamber vacuum-pumping tube; The 34-roller bearing.
Fig. 2 is the objective table device synoptic diagram;
The 1-Stage microscope; The 2-bolt; 3-altitude mixture control support; The 4-fixed support.
Fig. 3 is the scraper synoptic diagram;
The 1-push rod; The 2-deep floor; The high temperature resistant steel wire of 3-is scraped the material brush; 4-rigidity scraper.
Fig. 4 is a thermal-insulating sealing door synoptic diagram;
The 1-water outlet; 2-thermal-insulating sealing door shell; The 3-water-in; The 4-guide deflection sheave; The 5-web plate; 6-graphite fibre thermal insulation layer; 7-cooling trough cover plate.
Fig. 5 is the emission-control equipment synoptic diagram;
The 1-tensimeter; The 2-vacuum breaker; The 3-water cooling heat exchanger; 4-off gas treatment solution; The 5-Glass Containers.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is elaborated: the vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that in this embodiment, design, its furnace binding synoptic diagram is seen Figure of description 1, mainly by connecting bearing pin 1; Holding screw 2; Thermal-insulating sealing door cylinder 3; Scrape material cylinder 4; Material scraper 5; Change brush bell 6; Induction electrode 7; Holding bolt 8,9,10; Furnace wall 11; The hard felt plate 12 of graphite; Graphite carbon felt 13; Inlet pipe I 14; Holding bolt 15; Thermopair anchor clamps 16; Inlet pipe II 17; Vapor pipe 18; Graphite sleeve calorifier 19; Load coil 20; Thermopair 21; Reaction chamber vacuum-pumping tube 22; Stage microscope 23; Stage microscope height adjuster 24; Baffle plate 25; Guide rail 26; Rare gas element ventpipe I 27; Sealring 28; Thermal-insulating sealing door 29; Rare gas element ventpipe II 30; Material extracting chamber's sealing door 31; Travelling belt 32; Material extracting chamber's vacuum-pumping tube 33 is formed with roller bearing 34, and the body of heater reaction chamber adopts double-deck water-cooled, and is too high to prevent furnace body temperature.
In this embodiment, equipment size all is of a size of benchmark design with Stage microscope, and Stage microscope is of a size of 180 * 160 * 5mm; The size that obtains reaction chamber and material extracting chamber's burner hearth according to this size is respectively Φ 430 * 260mm and Φ 1000 * 550mm, and insulation layer thickness is 35mm, body of heater whole height 1000mm; Heating power is 40kw; Maximum operation (service) temperature is 1200 ℃, and the body of heater wall thickness is 10mm, and it is that hard felt plate of graphite and the thickness of 20mm is the graphite carbon felt of 15mm that the thermal insulation layer material is selected thickness respectively for use; Body of heater material selection Q235B, inlet pipe I, II select alundum tube.
The vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that in this embodiment, design; Being provided with objective table device (seeing Figure of description 2) Stage microscope and being reaction product provides and adheres to the place; Wherein fixed support 4 is welded on the body of heater, and altitude mixture control support 3 is taked one-piece construction with Stage microscope 1, and altitude mixture control support 3 is connected through bolt 2 with fixed support 4; To regulate the height of Stage microscope 1, Stage microscope 1 adopts Al
2O
3Structural ceramics, the reaction chamber reaction product is deposited on the Stage microscope.
The vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that in this embodiment, design; Be provided with scraper (seeing Figure of description 3) to scrape the reaction product of getting on the Stage microscope; Wherein push rod 1 is connected with cylinder; Realization is stretched out, homing action, and material scraper adopts high temperature resistant steel wire to scrape material brush 3 and rigidity scraper 4 unitized constructions, deep floor 2 assurance device requirement of strength.Scrape the material brush because of high temperature resistant steel wire and be the rapid wear article, scrape the material brush for the ease of installing, changing, body of heater is provided with and changes the brush bell.
The vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that in this embodiment, design are provided with sealing door in material extracting chamber, and it is positioned at the material extracting chamber bottom.Under material extracting chamber's sealing door opened condition, start transport unit, product is discharged by the material extracting chamber bottom automatically.
The vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that in this embodiment, design; Adopt insulation and sealing between thermal-insulating sealing door (seeing Figure of description 4) realization response chamber and the material extracting chamber, wherein: graphite fibre thermal insulation layer 6 is realized heat insulating; Cylinder is connected by web plate 5 with the thermal-insulating sealing door, and guide deflection sheave 4 cooperates with track, stretching out, resetting and realize the keying of thermal-insulating sealing door through cylinder; The thermal-insulating sealing door is provided with water cooling plant, is made up of water outlet 1, water-in 3 and cooling trough cover plate 7, prevents that thermal-insulating sealing Men Wendu is too high.
The vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that in this embodiment, design; Emission-control equipment (seeing Figure of description 5) is connected with the vapor pipe at body of heater top; The reaction chamber high-temp waste gas is discharged from vapor pipe; Flow into water cooling heat exchanger 3 through vacuum breaker 2,, be discharged in the atmosphere at last through feeding after the water-cooled in the off gas treatment solution 4 in the Glass Containers 5.
The vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that in this embodiment, design; Its continuous production mode implementation step: (see Figure of description 1) during production; At first close thermal-insulating sealing door 29 and material extracting chamber's sealing door 31; Start water-cooling system, guarantee that the double-deck water-cooled in reaction chamber furnace wall is normal.Start pumped vacuum systems, reaction chamber and material extracting chamber are vacuumized respectively, reach set(ting)value 1pa.Vacuumize after the completion; In stove, feed rare gas element through rare gas element ventpipe I 27 and rare gas element ventpipe II30; Two constant pressures all reach 1 normal atmosphere by force, through heating system inlet pipe I 14 and inlet pipe II 17 are heated, through thermopair 21 thermometrics; When temperature reaches set(ting)value, feed reactant gasess through inlet pipe I 14, inlet pipe II 17 respectively and have the carrier gas of catalyzer, the reaction beginning.The reaction product deposition reaches a certain amount of on Stage microscope 23, opens thermal-insulating sealing door 29 through 3 tractions of thermal-insulating sealing door cylinder, treats after thermal-insulating sealing door 29 complete openings; Scrape and expect that cylinder 4 slowly stretches out 5 completion of traction material scraper Stage microscope 23 is scraped material; Reaction product falls under gravity on material extracting chamber's travelling belt 32, scrape the material finish scrape the material cylinder 4 reset, close thermal-insulating sealing door 29; Continue to feed reactant gases and the carrier gas that has catalyzer, reaction is proceeded.Product reaches q.s on the travelling belt of material back when repeatedly scraping, and material extracting chamber is fed rare gas element reach 1 normal atmosphere, unlatching material extracting chamber sealing door 31; Start transport unit, product is discharged by the material extracting chamber bottom automatically, closes material extracting chamber's sealing door 31; After material extracting chamber is evacuated down to 1pa, stop to vacuumize, feed rare gas element and reaction chamber air pressure balance; Wait for the material process of next time getting, so the loop cycle automatic material taking is got the material process and can independently be carried out; Do not interrupt the production process of reaction chamber, realize preparation nano material continuously.
The design of the vapor phase process continuous production nano material two Room vertical vacuum controlled atmosphere generators that this embodiment relates to has realized that automatic material taking process and production process carry out synchronously; And to the efficient heating of reaction chamber; Solved traditional single chamber atmosphere furnace, the tube furnace heating efficiency is low; And deficiencies such as can not preparing continuously of must blowing out getting that material causes have improved the production efficiency that vapor phase process prepares nano material greatly.
Claims (5)
1. vertical continuous production vacuum controlled atmosphere furnace; This atmosphere furnace be a kind of be raw material with gas; Be used for the equipment that vapor phase process prepares nano material continuously; Shown in Figure of description 1; Its structure comprises: connect bearing pin (1), holding screw (2), thermal-insulating sealing door cylinder (3), scrape material cylinder (4), material scraper (5), change brush bell (6), induction electrode (7), holding bolt (8,9,10), furnace wall (11), the hard felt plate of graphite (12), graphite carbon felt (13), inlet pipe I (14), holding bolt (15), thermopair anchor clamps (16), inlet pipe II (17), vapor pipe (18), graphite sleeve calorifier (19), load coil (20), thermopair (21), reaction chamber vacuum-pumping tube (22), Stage microscope (23), Stage microscope height adjuster (24), baffle plate (25), guide rail (26), rare gas element ventpipe I (27), sealring (28), thermal-insulating sealing door (29), rare gas element ventpipe II (30), material extracting chamber's sealing door (31), travelling belt (32), material extracting chamber's vacuum-pumping tube (33) and roller bearing (34); It is characterized in that: the reaction chamber of body of heater is on top; Material extracting chamber is in the bottom; Thereby the formation vertical structure is provided with thermal-insulating sealing door (29) between reaction chamber and the material extracting chamber, but insulation between realization response chamber and the material extracting chamber and sealing; Reaction chamber is double-deck water-cooling structure; Too high to prevent furnace body temperature, during heating, " surface action " rapid heating graphite sleeve calorifier (19) that utilizes load coil (20) to produce on graphite sleeve calorifier (19) surface; And then inlet pipe I (14) and the inlet pipe II (17) that stretches into reaction chamber from the body of heater top and pass graphite sleeve calorifier (19) heated; Thereby the carrier gas that has catalyzer among reactant gases among the inlet pipe I (14) and the inlet pipe II (17) is heated, and the high-temperature reacting gas that two inlet pipe are discharged meets and reacts with the carrier gas that has catalyzer, generates solid product and is deposited on the Stage microscope (23); Scraper can be scraped the product of getting on the Stage microscope (23); Product is transferred on the travelling belt (32) in the material extracting chamber, starts transport unit, and product is finally discharged by material extracting chamber's sealing door (31) of material extracting chamber bottom automatically.
2. vertical continuous production vacuum controlled atmosphere furnace according to claim 1; Adopt induction heating mode to heat; Induction heating device mainly is made up of induction electrode (7), graphite sleeve calorifier (19) and load coil (20); It is characterized in that: induction heating device is in the top of reaction chamber; Realize heating by load coil (20) to graphite sleeve calorifier (19), thereby directly to inlet pipe I (14), inlet pipe II (17) heating, and then realize reactant gases and the carrier gas heating that has catalyzer.
3. vertical continuous production vacuum controlled atmosphere furnace according to claim 1; Be provided with the breather of being made up of inlet pipe I (14) and inlet pipe II (17), it is characterized in that: inlet pipe I (14) and inlet pipe II (17) adopt alundum tube, and two pipes stretch into reaction chamber from the body of heater top; Pass graphite sleeve calorifier (19); The terminal distance with Stage microscope (23) upper surface of two pipes is 50mm, and two pipes adopt the inclination that becomes 15 ° of angles with vertical direction to place design, can realize that the mouth of pipe is adjacent; The high-temperature gas that the two pipe mouths of pipe are discharged meets and reacts, and solid product is deposited on Stage microscope (23) upper surface.
4. a vertical continuous production vacuum controlled atmosphere furnace according to claim 1 is provided with automatic fetching device, is made up of material scraper (5), Stage microscope (23) and travelling belt (32); Wherein material scraper (5) is shown in Figure of description 3, scrapes material brush (3) by push rod (1), deep floor (2), high temperature resistant steel wire and forms with rigidity scraper (4), it is characterized in that: under the situation of thermal-insulating sealing door (29) unlatching; Scrape material cylinder (4) and stretch out, traction material scraper (5) is scraped the product of getting on the Stage microscope (23), and product is transferred on material extracting chamber's travelling belt (32); After scraping material and finishing, thermal-insulating sealing door (29) is closed, and produce to continue; Feed rare gas element to a normal atmosphere to material extracting chamber; Open material extracting chamber's sealing door (31), start material extracting chamber's transport unit, product is discharged by the material extracting chamber bottom automatically.
5. vertical continuous production vacuum controlled atmosphere furnace according to claim 1, its working method is continous way production, it is characterized by: during production; At first two Room are vacuumized, feed inert protective gas through rare gas element ventpipe I (27) and rare gas element ventpipe II (30) to reaction chamber and material extracting chamber respectively then, reactant gases feeds reaction chamber through inlet pipe I (14) and inlet pipe II (17) respectively with the carrier gas that has catalyzer; Heating system realizes reactant gases and the carrier gas heating that has catalyzer inlet pipe I (14) and inlet pipe II (17) heating indirectly, and high-temperature reacting gas and the carrier gas that has catalyzer are met at the end of two inlet pipe and reacted; Generate solid product and be deposited on the Stage microscope (23), when satisfying the condition of material collection, open thermal-insulating sealing door (29); Scrape material cylinder (4) and stretch out, traction material scraper (5) is scraped the product of getting on the Stage microscope (23), and product falls under gravity on the travelling belt (32) of material extracting chamber; Scrape to scrape after material finishes and expect that cylinder (4) resets, close thermal-insulating sealing door (29), reaction is proceeded; When going up product and reach a certain amount of, feed rare gas element to a normal atmosphere to material extracting chamber, open material extracting chamber's sealing door (31) through rare gas element ventpipe II (30) through repeatedly scraping material back travelling belt (32); Start transport unit, product is discharged in the material extracting chamber bottom automatically, gets material and finishes; Close material extracting chamber's sealing door (31), then material extracting chamber is evacuated to set(ting)value after, feed rare gas element and reaction chamber air pressure balance; Wait for next time and get the material process, so the loop cycle automatic material taking is got the material process and is independently carried out; Do not interrupt the production process of reaction chamber, realize vapor phase process continuous production nano material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011103692551A CN102515139B (en) | 2011-11-10 | 2011-11-10 | Two-chamber vertical vacuum controllable atmosphere furnace for continuously preparing nano materials through gas-phase method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174242A (en) * | 2015-03-23 | 2015-12-23 | 南昌大学 | Vertical reaction furnace for continuous production of carbon nanotubes with preset catalyst |
| CN106115662A (en) * | 2016-07-05 | 2016-11-16 | 上海峻岗环保科技有限公司 | A kind of continuous growth apparatus of technical grade overlength carbon nano pipe array |
| CN107381540A (en) * | 2017-07-21 | 2017-11-24 | 南昌大学 | A kind of horizontal kiln for reinforcing body catalyst continuous production CNT |
| CN111039256A (en) * | 2019-12-12 | 2020-04-21 | 江苏大学 | Mold and method for preparing nano-layered composite material |
| CN112933648A (en) * | 2021-01-29 | 2021-06-11 | 杨立娟 | Preparation device for material with water-based nano coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11281259A (en) * | 1998-03-27 | 1999-10-15 | Tokai Konetsu Kogyo Co Ltd | Continuous atmospheric furnace |
| CN201212049Y (en) * | 2008-01-31 | 2009-03-25 | 秦文隆 | Automatic heating quenching vacuum atmosphere oven |
| CN101893373A (en) * | 2010-07-23 | 2010-11-24 | 青岛科技大学 | Vertical and horizontal efficient energy-saving vacuum controlled atmosphere furnace for continuous production |
-
2011
- 2011-11-10 CN CN2011103692551A patent/CN102515139B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11281259A (en) * | 1998-03-27 | 1999-10-15 | Tokai Konetsu Kogyo Co Ltd | Continuous atmospheric furnace |
| CN201212049Y (en) * | 2008-01-31 | 2009-03-25 | 秦文隆 | Automatic heating quenching vacuum atmosphere oven |
| CN101893373A (en) * | 2010-07-23 | 2010-11-24 | 青岛科技大学 | Vertical and horizontal efficient energy-saving vacuum controlled atmosphere furnace for continuous production |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174242A (en) * | 2015-03-23 | 2015-12-23 | 南昌大学 | Vertical reaction furnace for continuous production of carbon nanotubes with preset catalyst |
| CN105174242B (en) * | 2015-03-23 | 2017-07-11 | 南昌大学 | A kind of reacting furnace of the preset Catalyst Production CNT of vertical continuous |
| CN106115662A (en) * | 2016-07-05 | 2016-11-16 | 上海峻岗环保科技有限公司 | A kind of continuous growth apparatus of technical grade overlength carbon nano pipe array |
| CN106115662B (en) * | 2016-07-05 | 2018-03-09 | 上海峻岗环保科技有限公司 | A kind of array continuous growth apparatus of technical grade overlength carbon nano pipe |
| CN107381540A (en) * | 2017-07-21 | 2017-11-24 | 南昌大学 | A kind of horizontal kiln for reinforcing body catalyst continuous production CNT |
| CN111039256A (en) * | 2019-12-12 | 2020-04-21 | 江苏大学 | Mold and method for preparing nano-layered composite material |
| CN111039256B (en) * | 2019-12-12 | 2022-07-22 | 江苏大学 | Mold and method for preparing nano-layered composite material |
| CN112933648A (en) * | 2021-01-29 | 2021-06-11 | 杨立娟 | Preparation device for material with water-based nano coating |
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