CN110483101A - The preparation method of carbon nano-fiber film without metallic catalyst - Google Patents
The preparation method of carbon nano-fiber film without metallic catalyst Download PDFInfo
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- CN110483101A CN110483101A CN201910748423.4A CN201910748423A CN110483101A CN 110483101 A CN110483101 A CN 110483101A CN 201910748423 A CN201910748423 A CN 201910748423A CN 110483101 A CN110483101 A CN 110483101A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5001—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with carbon or carbonisable materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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- Nanotechnology (AREA)
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- Inorganic Fibers (AREA)
Abstract
The invention discloses a kind of preparation methods of carbon nano-fiber film without metallic catalyst.After it first immerses aluminium flake in copper nitrate aqueous solution, it takes out, is dry, the aluminium flake of obtained area load copper nitrate is placed in ceramic vessel again, and ceramic fragment is covered thereon, later, the ceramic vessel of aluminium flake and ceramic fragment that obtained bottom is successively covered with area load copper nitrate is placed in 20-40h in the mixed atmosphere of the acetylene at 420-460 DEG C and argon gas, product is made in the surface of ceramic vessel and ceramic fragment.The carbon nano-fiber film without metallic catalyst has not only been made in it, also there is the characteristics of at low cost, yield is big, is easy to industrial-scale production, can more realize the recycling to various ceramics and building waste, to mitigate the pollution to environment；Product obtained has the characteristics that light-weight, hydrophobic and good mechanical property, be extremely easy to widely commercial applications in various oils leak cleaning field.
Description
Technical field
The present invention relates to a kind of preparation method of carbon nano-fiber film, especially a kind of carbon without metallic catalyst is received
The preparation method of rice fiber membrane.
Background technique
Have many advantages, such as that light-weight, large specific surface area, conductivity are high, chemical and strong mechanical stability carbon nano-fiber is thin
Film has extensive in fields such as high capacity oils absorbent, electrochemical catalysis agent carrier, supercapacitor and lithium ion batteries
Application.Currently, the preparation method of carbon nano-fiber film mainly includes electrostatic spinning, hydro-thermal, the carbonization of biological material, electricity
Solution and chemical vapor deposition, wherein chemical vapour deposition technique compared with other methods, have easy to operate, controllability it is strong, at
This low advantage.Such as in " Large-scale synthesis, annealing, purification, and magnetic
properties of crystalline helical carbon nanotubes with symmetrical
(" symmetrical structure crystallizes spiral carbon nanotubes by structures ", Adv.Funct.Mater.17,1542-1550 (2007)
Extensive synthesis, annealing, purifying and magnetic properties ", the 1542-1550 page of volume 17 of " advanced function material " 2007) it is one literary
Described in, catalyst is made using transition metal nanoparticles in chemical vapor deposition processes, carbon Nanowire is easily implemented
Tie up the controllable growth of film.But the shortcoming of this method is, the transition-metal catalyst particle inside carbon nano-fiber
Even if being all difficult to thoroughly remove using the strong acid of highly corrosive, to limit the application model of this carbon nano-fiber film
It encloses.To solve this problem, people are made that unremitting effort, such as entitled " Metal-free chemical vapor
deposition growth of graphitic tubular structures on engineered perovskite
Oxide substrates ", Carbon 99,591-598 (2016) (" utilize the change without metal in perovskite oxide substrate
Learn the graphited tubular structure of vapor deposition growth ", the 591-598 pages of volume 99 of " carbon " 2016) the utilization that refers to of article
The growth of carbon nano-fiber film is realized in the catalytic action of strontium titanate ceramics rough surface in chemical vapor deposition processes.It is this
Though method obtains the carbon nano-fiber film without any metallic catalyst, since the rough surface of strontium titanate ceramics needs
Expensive argon ion etching equipment processing can just obtain, and be difficult to realize the carbon without metallic catalyst so as to cause such method and receive
The low cost and large-scale production of rice fiber membrane.
Summary of the invention
The technical problem to be solved in the present invention in order to overcome the shortcomings in the prior art place, provide it is a kind of low cost, scale
Metaplasia produces the preparation method of the carbon nano-fiber film without metallic catalyst.
To solve technical problem of the invention, used technical solution is the carbon nano-fiber without metallic catalyst
The preparation method of film uses chemical vapour deposition technique, especially completion, and steps are as follows:
Step 1, aluminium flake is immersed to taking-up, drying in the copper nitrate aqueous solution of 0.08-0.12mol/L after at least 20min,
Obtain the aluminium flake of area load copper nitrate；
Step 2, the aluminium flake of area load copper nitrate is placed in ceramic vessel, and covers ceramic fragment thereon,
It obtains bottom and is successively covered with the aluminium flake of area load copper nitrate and the ceramic vessel of ceramic fragment；
Step 3, the ceramic vessel of aluminium flake and ceramic fragment that bottom is successively covered with to area load copper nitrate is placed in
Acetylene at 420-460 DEG C and 20-40h in the mixed atmosphere of argon gas are made in the surface of ceramic vessel and ceramic fragment
Carbon nano-fiber film without metallic catalyst.
The further improvement of preparation method as the carbon nano-fiber film without metallic catalyst:
Preferably, the time that aluminium flake immerses in copper nitrate aqueous solution is 20-40min.
Preferably, ceramic vessel is ceramic boat or ceramic bowl or ceramic disk or pottery pot.
Preferably, ceramic fragment is that ceramic bowl fragment or ceramic insulator fragment or ceramic tile fragment or common brick are broken
Block or cement concrete fragment.
Preferably, before being warming up to 420-460 DEG C, bottom is first successively covered with to the aluminium flake and ceramics of area load copper nitrate
The ceramic vessel of pieces, which is placed in argon atmospher, to heat up.
Preferably, the acetylene and 0.008-0.012L/min that the mixed atmosphere of acetylene and argon gas is 0.08-0.12L/min
The mixed gas of argon gas.
Beneficial effect compared with the existing technology is:
First, product made from surface for ceramic vessel and ceramic fragment uses scanning electron microscope, transmission respectively
Electronic Speculum and the subsidiary power spectrum tester of scanning electron microscope are characterized, as a result, it can be seen that, product is three-dimensional porous by carbon nanometer
The film of fiber composition；Wherein, carbon nano-fiber is polycrystalline structure, and it is free of any metallic catalyst.It is this by carbon nanometer
The product that fiber is assembled into, not only due to the speciality of carbon nano-fiber, but also because carbon nano-fiber is polycrystalline structure, due also to carbon nanometer
Fiber is free of any metallic catalyst, is more accumulated because of film by a large amount of carbon nano-fiber, and has greatly expanded product
Application range.
Second, the carbon nano-fiber film without metallic catalyst has not only been made in preparation method, also there is at low cost, production
The characteristics of amount is big, is easy to industrial-scale production can more realize the recycling to various ceramics and building waste, to mitigate
Pollution to environment；Product obtained has the characteristics that light-weight, hydrophobic and good mechanical property, is extremely easy to widely business
Change and is applied to various oils leakage cleaning field.
Detailed description of the invention
Fig. 1 be respectively to ceramic vessel, ceramic fragment and product obtained using camera, scanning electron microscope (SEM), thoroughly
One of the result that radio mirror (TEM) and subsidiary power spectrum (EDS) tester of scanning electron microscope are characterized.A figure in Fig. 1 is chemistry
Before vapor deposition, the optical photograph of ceramic fragment --- ceramic bowl fragment is placed in ceramic vessel --- in ceramic boat,
In, ceramic boat bottom is placed with the aluminium flake of load copper nitrate；B figure is the SEM image of ceramic bowl scrap section shown in a schemes；C figure is b
The high magnification SEM image of boxed area, can be seen that by it in figure, and the section of ceramic bowl fragment is also very coarse；D figure is chemistry
After vapor deposition, the optical photograph of ceramic bowl fragment and ceramic boat, what the arrow 1 in figure indicated is raw in ceramic bowl fragment surface
Long carbon nano-fiber film, what arrow 2 indicated is the carbon nano-fiber film in the growth of ceramic boat surface, what arrow 3 indicated
It is the carbon nano-fiber in aluminum flake surface by copper catalytic growth；E figure be ceramic bowl fragment surface growth carbon nano-fiber it is thin
The SEM image of film can be seen that film is as made of the accumulation of a large amount of carbon nano-fiber by the figure；F figure is e Tu Zhong box area
The high magnification SEM image in domain；G figure is the TEM image in the carbon nano-fiber of ceramic bowl fragment surface growth, and the illustration in figure is
The high magnification TEM image of carbon nano-fiber in boxed area illustrates that the carbon nano-fiber grown in ceramic bowl fragment surface is more
Crystal structure；H figure is the EDS spectrogram in the carbon nano-fiber film of ceramic bowl fragment surface growth, it was demonstrated that carbon nano-fiber is thin
Film contains only carbon, is free of any metallic catalyst element.
Fig. 2 is to be characterized respectively using product made from preparation method using camera to ceramic fragment and thereon
One of result.A, b, c, d figure in Fig. 2 is respectively ceramic insulator fragment, ceramic tile fragment, common brick fragment, cement concrete
The optical photograph of fragment；E figure is the optical photograph of the ceramic insulator fragment after chemical vapor deposition；F figure is processization
The optical photograph of ceramic tile fragment after learning vapor deposition；G figure is the optical photograph of the common brick fragment after chemical vapor deposition；
H figure is the optical photograph of the cement concrete fragment after chemical vapor deposition.
Specific embodiment
Preferred embodiment of the invention is described in further detail with reference to the accompanying drawing.
It buys from market or is voluntarily made first:
Copper nitrate aqueous solution；
As the ceramic boat of ceramic vessel, ceramic bowl, ceramic disk and pottery pot；
It is mixed as the ceramic bowl fragment of ceramic fragment, ceramic insulator fragment, ceramic tile fragment, common brick fragment and cement
Solidifying soil fragment；
Acetylene；
Argon gas.
Then:
Embodiment 1
The specific steps of preparation are as follows:
Step 1, aluminium flake is immersed in the copper nitrate aqueous solution of 0.08mol/L after 40min, it is negative to obtain surface for taking-up, drying
Carry the aluminium flake of copper nitrate.
Step 2, the aluminium flake of area load copper nitrate is placed in ceramic vessel, and covers ceramic fragment thereon；
Wherein, ceramic vessel is ceramic boat, and ceramic fragment is ceramic bowl fragment, obtains bottom and is successively covered with area load copper nitrate
Aluminium flake and ceramic fragment ceramic vessel.
Step 3, the ceramic vessel of aluminium flake and ceramic fragment that bottom is first successively covered with to area load copper nitrate is set
It is warming up to 420 DEG C in argon atmospher, then places it in 40h in the mixed atmosphere of the acetylene at identical temperature and argon gas；Wherein, second
The mixed atmosphere of alkynes and argon gas is the mixed gas of the acetylene of 0.08L/min and the argon gas of 0.012L/min, in ceramic vessel and
The surface of ceramic fragment, which is made, to be similar to shown in Fig. 1, and the carbon without metallic catalyst as shown by the curve in figure 1
Nano-fiber film.
Embodiment 2
The specific steps of preparation are as follows:
Step 1, aluminium flake is immersed in the copper nitrate aqueous solution of 0.09mol/L after 35min, it is negative to obtain surface for taking-up, drying
Carry the aluminium flake of copper nitrate.
Step 2, the aluminium flake of area load copper nitrate is placed in ceramic vessel, and covers ceramic fragment thereon；
Wherein, ceramic vessel is ceramic boat, and ceramic fragment is ceramic bowl fragment, obtains bottom and is successively covered with area load copper nitrate
Aluminium flake and ceramic fragment ceramic vessel.
Step 3, the ceramic vessel of aluminium flake and ceramic fragment that bottom is first successively covered with to area load copper nitrate is set
It is warming up to 430 DEG C in argon atmospher, then places it in 35h in the mixed atmosphere of the acetylene at identical temperature and argon gas；Wherein, second
The mixed atmosphere of alkynes and argon gas is the mixed gas of the acetylene of 0.09L/min and the argon gas of 0.011L/min, in ceramic vessel and
The surface of ceramic fragment, which is made, to be similar to shown in Fig. 1, and the carbon without metallic catalyst as shown by the curve in figure 1
Nano-fiber film.
Embodiment 3
The specific steps of preparation are as follows:
Step 1, aluminium flake is immersed in the copper nitrate aqueous solution of 0.1mol/L after 30min, it is negative to obtain surface for taking-up, drying
Carry the aluminium flake of copper nitrate.
Step 2, the aluminium flake of area load copper nitrate is placed in ceramic vessel, and covers ceramic fragment thereon；
Wherein, ceramic vessel is ceramic boat, and ceramic fragment is ceramic bowl fragment, obtains bottom and is successively covered with area load copper nitrate
Aluminium flake and ceramic fragment ceramic vessel.
Step 3, the ceramic vessel of aluminium flake and ceramic fragment that bottom is first successively covered with to area load copper nitrate is set
It is warming up to 440 DEG C in argon atmospher, then places it in 30h in the mixed atmosphere of the acetylene at identical temperature and argon gas；Wherein, second
The mixed atmosphere of alkynes and argon gas is the mixed gas of the acetylene of 0.1L/min and the argon gas of 0.01L/min, in ceramic vessel and pottery
The surface of ceramic products fragment is made as shown in Figure 1, and the carbon Nanowire without metallic catalyst as shown by the curve in figure 1
Tie up film.
Embodiment 4
The specific steps of preparation are as follows:
Step 1, aluminium flake is immersed in the copper nitrate aqueous solution of 0.11mol/L after 25min, it is negative to obtain surface for taking-up, drying
Carry the aluminium flake of copper nitrate.
Step 2, the aluminium flake of area load copper nitrate is placed in ceramic vessel, and covers ceramic fragment thereon；
Wherein, ceramic vessel is ceramic boat, and ceramic fragment is ceramic bowl fragment, obtains bottom and is successively covered with area load copper nitrate
Aluminium flake and ceramic fragment ceramic vessel.
Step 3, the ceramic vessel of aluminium flake and ceramic fragment that bottom is first successively covered with to area load copper nitrate is set
It is warming up to 450 DEG C in argon atmospher, then places it in 25h in the mixed atmosphere of the acetylene at identical temperature and argon gas；Wherein, second
The mixed atmosphere of alkynes and argon gas is the mixed gas of the acetylene of 0.11L/min and the argon gas of 0.009L/min, in ceramic vessel and
The surface of ceramic fragment, which is made, to be similar to shown in Fig. 1, and the carbon without metallic catalyst as shown by the curve in figure 1
Nano-fiber film.
Embodiment 5
The specific steps of preparation are as follows:
Step 1, aluminium flake is immersed in the copper nitrate aqueous solution of 0.12mol/L after 20min, it is negative to obtain surface for taking-up, drying
Carry the aluminium flake of copper nitrate.
Step 2, the aluminium flake of area load copper nitrate is placed in ceramic vessel, and covers ceramic fragment thereon；
Wherein, ceramic vessel is ceramic boat, and ceramic fragment is ceramic bowl fragment, obtains bottom and is successively covered with area load copper nitrate
Aluminium flake and ceramic fragment ceramic vessel.
Step 3, the ceramic vessel of aluminium flake and ceramic fragment that bottom is first successively covered with to area load copper nitrate is set
It is warming up to 460 DEG C in argon atmospher, then places it in 20h in the mixed atmosphere of the acetylene at identical temperature and argon gas；Wherein, second
The mixed atmosphere of alkynes and argon gas is the mixed gas of the acetylene of 0.12L/min and the argon gas of 0.008L/min, in ceramic vessel and
The surface of ceramic fragment, which is made, to be similar to shown in Fig. 1, and the carbon without metallic catalyst as shown by the curve in figure 1
Nano-fiber film.
Select the ceramic boat or ceramic bowl or ceramic disk or pottery pot as ceramic vessel respectively again, it is broken as ceramic
The ceramic bowl fragment or ceramic insulator fragment or ceramic tile fragment or common brick fragment or cement concrete fragment of block repeat above-mentioned reality
Apply a 1-5, be equally made as or be similar to shown in Fig. 1 or Fig. 2, and as shown by the curve in figure 1 be free of metal catalytic
The carbon nano-fiber film of agent.
Obviously, those skilled in the art can be to the system of the carbon nano-fiber film without metallic catalyst of the invention
Preparation Method carries out various modification and variations without departing from the spirit and scope of the present invention.If in this way, being repaired to of the invention these
Change with modification within the scope of the claims of the present invention and its equivalent technology, then the present invention be also intended to encompass these change and
Including modification.
Claims (6)
1. a kind of preparation method of the carbon nano-fiber film without metallic catalyst, using chemical vapour deposition technique, feature
It is that steps are as follows for completion:
Step 1, aluminium flake is immersed in the copper nitrate aqueous solution of 0.08-0.12mol/L after at least 20min, taking-up, drying obtain
The aluminium flake of area load copper nitrate；
Step 2, the aluminium flake of area load copper nitrate is placed in ceramic vessel, and covers ceramic fragment thereon, obtained
Bottom is successively covered with the aluminium flake of area load copper nitrate and the ceramic vessel of ceramic fragment；
Step 3, the ceramic vessel of aluminium flake and ceramic fragment that bottom is successively covered with to area load copper nitrate is placed in 420-
Acetylene at 460 DEG C and 20-40h in the mixed atmosphere of argon gas are made in the surface of ceramic vessel and ceramic fragment and are free of
The carbon nano-fiber film of metallic catalyst.
2. the preparation method of the carbon nano-fiber film according to claim 1 without metallic catalyst, it is characterized in that aluminium
The time that piece immerses in copper nitrate aqueous solution is 20-40min.
3. the preparation method of the carbon nano-fiber film according to claim 1 without metallic catalyst, it is characterized in that pottery
Porcelain container is ceramic boat or ceramic bowl or ceramic disk or pottery pot.
4. the preparation method of the carbon nano-fiber film according to claim 1 without metallic catalyst, it is characterized in that pottery
Ceramic products fragment is that ceramic bowl fragment or ceramic insulator fragment or ceramic tile fragment or common brick fragment or cement concrete are broken
Block.
5. the preparation method of the carbon nano-fiber film according to claim 1 without metallic catalyst, it is characterized in that in
Before being warming up to 420-460 DEG C, the ceramics of aluminium flake and ceramic fragment that bottom is first successively covered with to area load copper nitrate hold
Device is placed in argon atmospher and heats up.
6. the preparation method of the carbon nano-fiber film according to claim 1 without metallic catalyst, it is characterized in that second
The mixed atmosphere of alkynes and argon gas is the mixed gas of the acetylene of 0.08-0.12L/min and the argon gas of 0.008-0.012L/min.
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Cited By (2)
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| CN111604032A (en) * | 2020-06-02 | 2020-09-01 | 山东建筑大学 | Janus nitrogen-doped carbon nanofiber film and preparation method and application thereof |
| CN111943169A (en) * | 2020-08-04 | 2020-11-17 | 山东建筑大学 | Method for preparing metal-free carbon nano fiber by stripping method |
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