CN104627980B - Controllable flame burner and method for synthesizing carbon nano tubes - Google Patents
Controllable flame burner and method for synthesizing carbon nano tubes Download PDFInfo
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Abstract
The invention discloses a controllable flame burner and a method for synthesizing carbon nano tubes. The controllable flame burner comprises vertically penetrated double layers of straight round tubes embedded with one another, wherein an area encircled by the inner layer straight round tube refers to a central reactive synthesis area; an area encircled between the inner layer straight round tube and the outer layer straight round tube is segmented into a high-temperature heat source area and a low-temperature cooling area; a carbon nano tube sampling area is formed at the upper outlet of the double-layer straight round tube; the lower opening of the central reactive synthesis area refers to an inlet of reactant mixed gas, inert gases and nano catalyst particles; the lower opening of the high-temperature heat source area refers to an inlet of combustible premixed gas; and the lower opening of the low-temperature cooling area refers to an inlet of cooling gas. The large-scale controllable and continuous synthesis of the carbon nano tubes can be realized at low cost, and the yield of the carbon nano tubes can be improved.
Description
Technical field
The present invention relates to a kind of CNT synthetic technology, more particularly to a kind of controllable flame burner and its synthesis carbon are received
The method of mitron.
Background technology
CNT (Carbon Nanotubes, CNTs) is the isomer of carbon, is by layer structure graphene film
The hollow pipe of the nano-scale being rolled into, with very high draw ratio, while with fabulous mechanics, electrically and thermally performance.
Japanese Electronic Speculum expert's Sumio Iijima (Sumio Iijima) is found that first depositing for CNT using ultramicroscope within 1991
.At present, the synthetic method of CNT mainly has four kinds：Arc discharge method (arc discharge), laser evaporization method
(laser vaporization), chemical vapour deposition technique (chemical vapor deposition, CVD) and flame synthesize
Method (flame synthesis).Wherein, flame synthesis (utilizing combustion flame synthesizing carbon nanotubes) are a brand-new technologies
And research field.
First three prior synthesizing method (arc discharge method, laser evaporization method, chemical vapour deposition technique) equipment is complicated, cost
It is higher, yield poorly, it is impossible to operate continuously, and flame synthesis can be carried out under normal atmosphere, and equipment is simple, low cost
Honest and clean, generated time is short, the possibility with commercial synthesis.
Before 2000, the research of Flame Synthesis of Carbon Nanotubes is less, and representative is 1994 Belgian
Ivanov et al. is in document " Ivanov V, Nagy J B et, al.The Study of Carbon nanotubes
Produced by Catalytic Method.Chem Phys Lett.1994,223:With acetylene by pyrolysis in 329-335 "
The CNT of tens nanometers of diameter is grown on the catalyst particle such as cobalt and ferrum.The same year, Massachusetts Institute Technology
Howard et al. is in document " Howard JB, Das Chowdhury K, Vander Sande JB.Carbon shells in
flames.Nature,1994,370(6491):603 " burning acetylene, benzene in the low pressure vessel of oxygenation and diluent is found in
Or ethylene etc. can obtain CNT.
After 2000, the research work of Flame Synthesis of Carbon Nanotubes is just gradually carried out both at home and abroad.
NASA Vander wal in 2000 et al. are in document " Vander wal RL, Ticich TM, Curtis
VE.Diffusion Flame Synthesis of Single-walled Carbon Nanotubes.Chem Phys
Lett.2000,354(1-2):CNT has been obtained using " cracking flame " in 20-4 ".NASA in 2002
Vander wal et al. are in document " Vander wal RL, Fe-Catalyzed.Single-walled Carbon
Nanotubes Synthesis within a Flame Environment.Combustion and Flame.2002,130:
Fuel gas is adopted in 37-47 " for carbon source, a small amount of single wall carbon has been obtained using Mckenna's burner (McKenna burner) and has been received
Mitron.
Massachusetts Institute Technology Height and Howard in 2004 et al. document " Height MT, Howard JB,
Tester JW et al.Flame Synthesis of Single-walled Carbon
Nanotubes.Carbon.2004,42:With oxygenation and the burning acetylene premixed gas of diluent in 2295-2307 ", in burning
SWCN is have collected behind the laminar flow flat flame of device outlet at differing heights.
Japan NaKazawa in 2005 et al. is in document " NaKazawa S, YoKomori T, Mizomoto M.Flame
Synthesis of Carbon Nanotubes in a Wall Stagnation Flow.Chemical Physics
Letter.2005,403:The premix gas jet impulse of the acetylene/air in 158-162 " using fuel-rich scribbles Raney nickel layer
Ceramics stay and allocate plate, form horn-like flame, and generating multi-walled carbon nano-tubes in allocating narrow annular band region on plate.
Sang Kil Woo of Korea in 2008 et al. are in document " Sang Kil Woo, Young Taek Hong, Oh
Chae Kwon.Flame synthesis of carbon-nanotubes using a double-faced wall
stagnation flow burner.Carbon,2009,47(3):Obtained using double-walled standing current burner in 912-916 "
CNT.
From the point of view of summarizing, flame synthetic method of the prior art has advantage, but there is also deficiency.First thermal source temperature
Degree poor controllability, relies primarily on the combustion intensity (combustion oxygen ratio) of adjustment flame to regulate and control reaction temperature, causes product to have one
Fixed impurity, is difficult to obtain SWCN and with the CNT compared with long structure；Two is the conjunction due to CNT
It is bad into condition (mainly temperature and catalyst) controllability so that the yield of CNT still awaits improving.
Commercial Application and the scientific research of CNT it is desirable that a large amount of quality preferably, grow controllable, purity it is higher and
Lower-cost CNT, the flame method of synthesizing carbon nanotubes is difficult to overcome traditional flame synthetic method in prior art
Drawback.
The content of the invention
It is an object of the invention to provide it is a kind of can realize controllable, continuous, extensive, inexpensive synthesizing carbon nanotubes can
The method of control flame burner and its synthesizing carbon nanotubes.
The purpose of the present invention is achieved through the following technical solutions：
The controllable flame burner of the synthesizing carbon nanotubes of the present invention, including the straight circle of bilayer of mutually nested up/down perforation
Pipe, is synthesized area, the region surrounded between the straight pipe of internal layer and the straight pipe of outer layer centered on the region that the straight pipe of internal layer is surrounded
Be divided into high temperature heat source area and sub-cooled area, the upper outlet of the double-deck straight pipe is CNT sampling area, it is described in
The heart is synthesized the entrance of the lower mouth for reactant gaseous mixture, noble gases and nano-catalyst particles in area, the high temperature heat source
The lower mouth in area is the entrance of flammable premixed gas, and the lower mouth in the sub-cooled area is the entrance of cooling gas.
The method of the above-mentioned controllable flame burner synthesizing carbon nanotubes of utilization of the invention, including step：
After by fuel gas and air or oxygen premix, the high temperature heat source area is passed into, Jing after ignition, it is right to produce
The stable flame for claiming, provides CNT synthesis necessary stable high temperature heat source, while producing to the central reaction synthesis zone
First portion CNT；
Meanwhile, it is passed through cooling gas to the sub-cooled area to control the temperature in the central reaction synthesis zone；
Meanwhile, the reaction mixture gas body after premix, noble gases and nanometer are passed through in the central reaction synthesis zone and are urged
Catalyst particles, there is provided the necessary stable carbon-source gas of CNT synthesis and nano-catalyst particles, split at high temperature
Solution reaction, produces the active atoms of carbon of free state, under the protection of noble gases, is combined rapidly with nano-catalyst particles, into
Growth core for CNT and constantly grow, ultimately form CNT.
As seen from the above technical solution provided by the invention, controllable flame burner provided in an embodiment of the present invention and
The method of its synthesizing carbon nanotubes, due to the straight pipe of bilayer including mutually nested up/down perforation, the straight pipe of internal layer is surrounded
Area is synthesized centered on region, the region segmentation surrounded between the straight pipe of internal layer and the straight pipe of outer layer is high temperature heat source area and low
Warm cooling zone, the upper outlet of the double-deck straight pipe is CNT sampling area, and the lower mouth of the central reaction synthesis zone is
The entrance of reactant gaseous mixture, noble gases and nano-catalyst particles, the lower mouth in the high temperature heat source area is flammable premix gas
The entrance of body, the lower mouth in the sub-cooled area is the entrance of cooling gas.Controllable, continuous, extensive, low cost can be realized
Synthesizing carbon nanotubes, synthesizing carbon nanotubes process and combustion process is completely isolated, while increased CNT building-up process
The sub-cooled stage, can reduce burning produce a large amount of impurity, realize CNT synthesis temperature it is relatively accurate, can
Control and regulation, regulate and control reaction temperature, it is ensured that carbon nanometer without being completely dependent on the combustion intensity (combustion oxygen ratio) of adjustment flame
Pipe synthesizes under the conditions of Optimal Temperature, is more beneficial for SWCN and the generation with the CNT compared with long structure.
In addition, CNT is mainly obtained in central canal outlet in the present invention, while in the upper outlet in Liang Ge high temperature heat sources area
Part CNT can be obtained, according to spherical-surface substrate sampling, effective collection area of CNT can be expanded, these all will
Further increase the yield of CNT.
Description of the drawings
Fig. 1 is the dimensional structure diagram of controllable flame burner provided in an embodiment of the present invention.
Fig. 2 is the cross-sectional structure schematic diagram of controllable flame burner provided in an embodiment of the present invention.
In figure：
1 represents central reaction synthesis zone, and in its bottom reactant gaseous mixture, noble gases and nanocatalyst are passed through
Grain；2 and 4 represent high temperature heat source area, and in its bottom flammable premixed gas is passed through, and provide high by the way that area is synthesized centered on burning
Temperature-heat-source；3 and 5 represent sub-cooled area, be passed through noble gases or nitrogen in its bottom or air comes control centre and is synthesized
Synthesis reaction temperature in area 1；6 represent CNT sampling area.
Specific embodiment
The embodiment of the present invention will be described in further detail below.
The controllable flame burner of the synthesizing carbon nanotubes of the present invention, its preferably specific embodiment is：
Including the straight pipe of bilayer of mutually nested up/down perforation, it is synthesized centered on the region that the straight pipe of internal layer is surrounded
Area, the region segmentation surrounded between the straight pipe of internal layer and the straight pipe of outer layer is high temperature heat source area and sub-cooled area, the bilayer
The upper outlet of straight pipe is CNT sampling area, and the lower mouth of the central reaction synthesis zone is reactant gaseous mixture, inertia
The entrance of gas and nano-catalyst particles, the lower mouth in the high temperature heat source area is the entrance of flammable premixed gas, the low temperature
The lower mouth of cooling zone is the entrance of cooling gas.
The high temperature heat source area and sub-cooled area have respectively 2, and 2 high temperature heat source areas are arranged symmetrically, 2 sub-cooled
Area is arranged symmetrically.
The outlet of the straight pipe of the internal layer is concordant with the outlet of the straight pipe of the outer layer；
The cooling gas are noble gases or air, and the CNT sampling area is used to collect the carbon nanometer of synthesis
Tube material.
The method of the above-mentioned controllable flame burner synthesizing carbon nanotubes of utilization of the present invention, its preferably specific embodiment party
Formula is：
Including step：
After by fuel gas and air or oxygen premix, the high temperature heat source area is passed into, Jing after ignition, it is right to produce
The stable flame for claiming, provides CNT synthesis necessary stable high temperature heat source, while producing to the central reaction synthesis zone
First portion CNT；
Meanwhile, it is passed through cooling gas to the sub-cooled area to control the temperature in the central reaction synthesis zone；
Meanwhile, the reaction mixture gas body after premix, noble gases and nanometer are passed through in the central reaction synthesis zone and are urged
Catalyst particles, there is provided the necessary stable carbon-source gas of CNT synthesis and nano-catalyst particles, split at high temperature
Solution reaction, produces the active atoms of carbon of free state, under the protection of noble gases, is combined rapidly with nano-catalyst particles, into
Growth core for CNT and constantly grow, ultimately form CNT.
The fuel gas is carbonaceous gas, including methane, ethylene, acetylene and/or liquefied petroleum gas；
The noble gases are argon or helium；
The nano-catalyst particles are transition-metal catalyst granule, and the transition-metal catalyst granule is nickeliferous, ferrum
Or cobalt element；
The reaction mixture gas body is carbonaceous gas, including ethylene, acetylene, ethane, carbon monoxide and/or hydrogen.
The sampling instrument of the CNT is metal probe, metal flat substrate, metallic spheric surface substrate and/or tinsel
Net.
The ignition temperature in the high temperature heat source area is between 550 DEG C～1250 DEG C.
The controllable flame burner of the present invention and its method for synthesizing carbon nanotubes, can realize controllable, continuous, big rule
Mould, inexpensive synthesizing carbon nanotubes, synthesizing carbon nanotubes process and combustion process is completely isolated, while increased CNT
In the sub-cooled stage of building-up process, a large amount of impurity that burning is produced can be reduced, realize the relative of CNT synthesis temperature
Accurately, controllable adjustable, without being completely dependent on the combustion intensity (combustion oxygen ratio) of adjustment flame reaction temperature is regulated and controled, and is protected
Card CNT synthesizes under the conditions of Optimal Temperature, is more beneficial for SWCN and with the CNT compared with long structure
Generation.In addition, CNT is mainly obtained in central canal outlet in the present invention, while on the top in Liang Ge high temperature heat sources area
Outlet can also obtain part CNT, according to spherical-surface substrate sampling, can expand effective collection area of CNT, this
A little yield that CNT all will be further increased.
Specific embodiment：
The present invention is illustrated by taking the concrete grammar of controllable flame burner synthesizing carbon nanotubes as an example.
As shown in Figure 1 and Figure 2, by central reaction synthesis zone 1, high temperature heat source area (combustor) 2 and 4, the and of sub-cooled area 3
5th, CNT sampling area 6 is constituted.
The bottom of area's (central canal) 1 is synthesized from center and is passed through reactant gaseous mixture, noble gases and nanocatalyst
Grain, from the bottom of high temperature heat source area 2 and 4 flammable premixed gas is passed through, and high temperature heat source can be provided by premixed combustion, from low temperature
The bottom of cooling zone 3 and 5 be passed through noble gases either nitrogen or air adjusting the synthesis reaction temperature in central canal.Inside and outside
The CNT sampling area 6 of layer pipe upper outlet, collects the carbon nano-tube material of synthesis.CNT is mainly in central canal
1 outlet is obtained, while the upper outlet in Liang Ge high temperature heat sources area 2 and 4 can also obtain part CNT.
Specific implementation step using controllable flame synthesizing carbon nanotubes is as follows：
By methane (or ethylene, acetylene, liquefied petroleum gas) and the premixed gas of air (or oxygen) be passed into two it is relative
High temperature heat source area (combustor) 2 and 4, Jing ignition, combustion, produce symmetrical stable flame, carry to central reaction synthesis zone 1
For the necessary stable high temperature heat source of CNT synthesis.Flammable premixed gas can produce part CNT in burning, can
Upper outlet in high temperature heat source area 2 and 4 is collected and obtained.
The reaction mixture gas body after premix, noble gases and nano-catalyst particles are passed through to central reaction synthesis zone 1, are carried
For the necessary stable carbon-source gas of CNT synthesis and nano-catalyst particles.Reactant in central reaction synthesis zone 1
Gaseous mixture can be carbonaceous gas ethylene (or carbon monoxide, acetylene, ethane), hydrogen and noble gases (such as argon, helium), and hydrogen can be with
Ensure the satisfactory texture and form of CNT.Noble gases are used as protective gas, while the activity of catalyst can be kept.
Nano-catalyst particles are typically chosen transition-metal catalyst granule (nickeliferous, ferrum or cobalt element), are received using the catalyst of iron content
Effect is preferable during rice grain synthesizing carbon nanotubes.
Due to three fundamentals for possessing CNT synthesis：Thermal source, carbon source and catalyst, therefore carbon can be synthesized
Nanotube.
Carbon-source gas in central reaction synthesis zone 1, can occur at high temperature cracking reaction, produce the activated carbon of free state
Atom, under the protection of noble gases, is combined rapidly with nano-catalyst particles, becomes the growth core and not of CNT
Medium well is long, ultimately forms CNT.
Deposition (or the CNT nucleation) process of carbon atom needs certain cool condition excessively, utilizes to two in this method
It is warm controllably suitably to reduce central reaction synthesis zone 1 that relative sub-cooled area 3 and 5 is passed through noble gases or nitrogen or air
Degree, promotes CNT fast nucleation, and promotes it to grow.
Generally, keep methane relative with the volume flow ratio of air stable, make flame temperature 550 DEG C～1250
Between DEG C, it is ensured that flame front is stable；The method for being passed through noble gases (or nitrogen, air) using the bottom of sub-cooled area 3 and 5
To adjust the synthesis reaction temperature in central canal, with the top carbon atom deposition and carbon nanometer that ensure that area is synthesized in central canal
The nucleation of pipe.In this method, main regulation is passed through the noble gases in sub-cooled area (or nitrogen, air) flow come in adjusting
The heart is synthesized the wall surface temperature in area 1, is formed " controllable flame ", expands the range of accommodation of CNT synthesis temperature, it is ensured that
CNT synthesizes under optimum temperature conditionss.
The method of controllable flame burner synthesizing carbon nanotubes in the present embodiment, by synthesizing carbon nanotubes process and burned
Journey is completely isolated, and being completely independent each process is carried out, while the sub-cooled stage of CNT building-up process is increased, can
A large amount of impurity that burning is produced are reduced, while being capable of achieving the accurately controllable adjustable relatively of heat source temperature, it is ensured that CNT
Synthesize under optimum temperature conditionss, it is not necessary to depend only on the combustion intensity (combustion oxygen ratio) of adjustment flame to adjust temperature, can
Easily to realize the controllable synthesis of CNT, it is more beneficial for SWCN and receives with the carbon compared with long structure
The generation of mitron.In addition, CNT is mainly obtained in central canal outlet in the present invention, while in Liang Ge high temperature heat sources area
Upper outlet can also obtain part CNT, and this will be further increased the yield of CNT.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
All should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (7)
1. the controllable flame burner of a kind of synthesizing carbon nanotubes, it is characterised in that including the double of mutually nested up/down perforation
The straight pipe of layer, centered on the region that the straight pipe of internal layer is surrounded area is synthesized, and is surrounded between the straight pipe of internal layer and the straight pipe of outer layer
Region segmentation be high temperature heat source area and sub-cooled area, the upper outlet of the double-deck straight pipe is CNT sampling area,
The lower mouth of the central reaction synthesis zone for reactant gaseous mixture, noble gases and nano-catalyst particles entrance, the height
The lower mouth of warm source region is the entrance of flammable premixed gas, and the lower mouth in the sub-cooled area is the entrance of cooling gas.
2. the controllable flame burner of synthesizing carbon nanotubes according to claim 1, it is characterised in that the high temperature heat source
Area and sub-cooled area have respectively 2, and 2 high temperature heat source areas are arranged symmetrically, and 2 sub-cooled areas are arranged symmetrically.
3. the controllable flame burner of synthesizing carbon nanotubes according to claim 2, it is characterised in that the internal layer is directly justified
The outlet of pipe is concordant with the outlet of the straight pipe of the outer layer；
The cooling gas are noble gases or air, and the CNT sampling area is used to collect the CNT material of synthesis
Material.
4. the method for the controllable flame burner synthesizing carbon nanotubes described in a kind of utilization claim 1,2 or 3, its feature exists
In, including step：
After by fuel gas and air or oxygen premix, the high temperature heat source area is passed into, Jing after ignition, is produced symmetrical
Stable flame, provides CNT synthesis necessary stable high temperature heat source, while generating unit to the central reaction synthesis zone
Divide CNT；
Meanwhile, it is passed through cooling gas to the sub-cooled area to control the temperature in the central reaction synthesis zone；
Meanwhile, the reaction mixture gas body after premix, noble gases and nanocatalyst are passed through in the central reaction synthesis zone
, there is cracking at high temperature anti-in granule, there is provided the necessary stable carbon-source gas of CNT synthesis and nano-catalyst particles
Should, the active atoms of carbon of free state is produced, under the protection of noble gases, combined rapidly with nano-catalyst particles, become carbon
The growth core of nanotube and constantly grow, ultimately form CNT.
5. the method for synthesizing carbon nanotubes according to claim 4, it is characterised in that the fuel gas is carbon containing gas
Body, including methane, ethylene, acetylene and/or liquefied petroleum gas；
The noble gases are argon or helium；
The nano-catalyst particles are transition-metal catalyst granule, and the transition-metal catalyst granule is nickeliferous, ferrum or cobalt
Element；
The reaction mixture gas body is carbonaceous gas and hydrogen, and the carbonaceous gas includes ethylene, acetylene, ethane, carbon monoxide.
6. the method for synthesizing carbon nanotubes according to claim 5, it is characterised in that the sampling instrument of the CNT
For metal probe, metal flat substrate, metallic spheric surface substrate and/or metal gauze.
7. the method for synthesizing carbon nanotubes according to claim 6, it is characterised in that the burning temperature in the high temperature heat source area
Degree is between 550 DEG C～1250 DEG C.
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| CN107619036A (en) * | 2017-11-02 | 2018-01-23 | 北京化工大学 | The method that burning is oriented to quick preparation structure ordered carbon nanotube array |
| CN107782480B (en) * | 2017-11-17 | 2023-08-29 | 北京石油化工学院 | Method and device for testing minimum ignition energy of combustible dust/combustible gas mixture |
| CN112473554A (en) * | 2020-12-03 | 2021-03-12 | 华中科技大学 | Prevent sedimentary nanometer particle of wall surface granule and generate device |
| CN113422045B (en) * | 2021-05-31 | 2022-09-16 | 河南城建学院 | Device and method for preparing carbon-based nano composite electrode material through sectional combustion |
| CN114162806B (en) * | 2022-01-07 | 2023-05-16 | 北京石油化工学院 | Burner with controllable flame and symmetrical distribution and method for synthesizing carbon nano tube by burner |
| CN115285974A (en) * | 2022-08-18 | 2022-11-04 | 安徽建马防护用品科技有限公司 | Method and device for manufacturing alkene carbon material |
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