CN107986247A - A kind of preparation method of graphite phase carbon nitride nanotube - Google Patents
A kind of preparation method of graphite phase carbon nitride nanotube Download PDFInfo
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- CN107986247A CN107986247A CN201711443095.4A CN201711443095A CN107986247A CN 107986247 A CN107986247 A CN 107986247A CN 201711443095 A CN201711443095 A CN 201711443095A CN 107986247 A CN107986247 A CN 107986247A
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- presoma
- carbon nitride
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Abstract
The invention discloses a kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：1) presoma is placed in ceramic crucible, then by alumina formwork of the aperture in the range of 10~200nm, Open Side Down is placed directly within above presoma, sealed crucible is placed in Muffle furnace or tube furnace, presoma is set to be deposited in the duct of alumina formwork under cryogenic conditions, continue to heat up, the presoma for making to be deposited in alumina formwork duct is pyrolyzed；2) with concentration be 0.1~3mol/L dilute acid soln remove alumina formwork, after centrifuged or suction filtration processing, drying, obtain finished product.The method of the present invention step is simple, non-environmental-pollution, and without complicated equipment, prepared graphite phase carbon nitride tube diameters controllability is strong, and better crystallinity degree, nanometer tube wall, pattern are uniform, so as to greatly improve the photocatalysis performance of the azotized carbon nano pipe finished product.
Description
Technical field
The present invention relates to field of inorganic nano material, more particularly to a kind of preparation method of inorganic nano-tube.
Background technology
With becoming increasingly conspicuous for global environment, the energy and safety problem, solar energy is cleaned as one kind, regenerative resource,
The extensive concern of all circles is obtained.To achieve the purpose that to the Efficient Conversion of solar energy with utilizing, the exploitation of high efficiency photocatalyst
Have become the research hotspot of academia with performance study.At present, photochemical catalyst mainly have metal oxide, metal sulfide,
The materials such as noble metal.2009, it is visible that Wang Xinchen et al. has found that non-metal semiconductive graphite phase carbon nitride (gC3N4) has first
Light hydrogen production potential.Graphite phase carbon nitride material is made of the carbon of rich content, nitrogen on the earth, and band gap is moderate (2.7eV), tool
There is certain visible light-responded property, and it has unique electronic structure, chemical stability, corrosion resistance, compared to traditional
Metal, semi-conducting material, relative inexpensiveness, discharges in catalytic reaction process without noxious material, environmental-friendly.It is all these
Advantage so that graphite phase carbon nitride receives much concern.
Graphite phase carbon nitride imparts its excellent optics and electrochemical properties because of its unique electronic structure so that its
Photocatalysis field account for one seat.However, simple graphite phase carbon nitride still suffers from light induced electron combined efficiency height, quantum effect
The low problem of rate, limits its practical application.Research of the scholars to graphite phase carbon nitride at present is focused primarily upon to graphite-phase
Carbonitride is modified, and answering for its band structure, regulation and control microstructure, reduction photo-generated carrier and electron hole is modified to reach
The purpose of closing probability.Specific modified method mainly has doping, design heterojunction composite, utilizes nanometer technology, soft template
Change the microstructure sizes of graphite phase carbon nitride.Wherein, photo-generated carrier can effectively be weakened by preparing one-dimensional nano structure
Recombination probability, improve photocatalysis efficiency.
A kind of patent of invention " preparation method of graphite type carbon nitride nanotube " (application number：201310613352.X), its
There is no template or extra organic substance to add, azotized carbon nano pipe is prepared simply by control heating schedule；Patent of invention " one
The preparation method of kind azotized carbon nano pipe " (application number：201510655423.1), it is template using silica spheres, is passed through
The pyrolysis cladding of melamine prepares azotized carbon nano pipe；Patent of invention " a kind of azotized carbon nano pipe and preparation method thereof " (Shen
Please number：201610219084.7), it is dialysed by bag filter using sodium acid carbonate and the pyrolysis of urea, is prepared nitridation
Carbon nanotubes；Patent of invention " a kind of synthetic method that the azotized carbon nano pipe with electrochemical capacitance performance is constructed based on ZIF-67 "
(application number：201610596681.1), it prepares azotized carbon nano pipe by the carbonization of ZIF-67；A patent of invention " species pipe
Shape boron doped graphite phase carbon nitride " (application number：201710040539.3), its tubulose carbonitride pattern being prepared is nanometer
Piece, is that incomplete curling interlocks；Patent of invention " a kind of graphite type carbon nitride nanotube array photoelectrode, its preparation method and use
(application number on the way "：201710220962.1), it in the duct of alumina formwork by pouring into cyanamide solution, then high temperature pyrolysis
Prepare azotized carbon nano pipe.
Preparation method disclosed above, more complicated, the pattern of the prepared azotized carbon nano pipe obtained is difficult to effectively control
System, so as to influence its photocatalysis performance.
The content of the invention
It is an object of the invention in view of the above shortcomings of the prior art, there is provided a kind of system of graphite phase carbon nitride nanotube
Preparation Method, its preparation process is simple, and the obtained tubular looks controllability of azotized carbon nano is strong.
The technical solution used in the present invention is：A kind of preparation method of graphite phase carbon nitride nanotube, it includes as follows
Processing step：
1) presoma is placed in ceramic crucible, then the alumina formwork opening by aperture in the range of 10~200nm
It is placed directly within downwards above presoma, sealed crucible is placed in Muffle furnace or tube furnace, and presoma is made under cryogenic conditions in oxygen
Change and deposited in the duct of aluminum alloy pattern plate, continue to heat up, the presoma for making to be deposited in alumina formwork duct is pyrolyzed；
2) with concentration be 0.1~3mol/L dilute acid soln remove alumina formwork, after centrifuged or suction filtration processing, dry
It is dry, obtain finished product.
Further as such scheme is improved, the presoma described in step 1) be selected from urea, thiocarbamide, double focusing cyanamide,
At least one of melamine.Specifically, research has shown that, its gained graphite phase carbon nitride is received when using single presoma
The controllability of mitron pattern is stronger, therefore present invention preferably uses single presoma.
Further as such scheme is improved, and the temperature of low temperature depositing described in step 1) is 100~200 DEG C, insulation 1
~10h.Specifically, the present invention directly obtains presoma deposit by low temperature depositing, when it is to low temperature depositing temperature and insulation
Long restriction can make presoma deposition more abundant.
Further as such scheme is improved, and the temperature being pyrolyzed described in step 1) is 550~650 DEG C, pyrolysis time
For 0.5~5h.Specifically, the restriction of pyrolysis temperature and pyrolysis time of the present invention can effectively improve presoma in alumina formwork
Crystallinity.
Further as such scheme is improved, and dilute acid soln described in step 2) is selected from phosphoric acid solution, hydrochloric acid solution, sulphur
One of which in acid solution.Specifically, further limit of dilute acid soln can more efficiently remove alumina formwork.
The beneficial effects of the invention are as follows：The method of the present invention step is simple, non-environmental-pollution, made without complicated equipment
Strong for the graphite phase carbon nitride tube diameters controllability obtained, good crystallinity, nanometer tube wall, pattern are uniform, so as to carry significantly
The photocatalysis performance of the high azotized carbon nano pipe finished product.
Brief description of the drawings
Fig. 1 of the present invention is the stereoscan photograph (amplification factor for the graphite phase carbon nitride nanotube that embodiment 1 is prepared into：
20.0k)。
Embodiment
The present invention is specifically described with reference to embodiment, in order to technical field personnel to the present invention
Understand.It is necessary that herein the present invention will be further described it is emphasized that embodiment is only intended to, it is impossible to be interpreted as to this
The limitation of invention protection domain, fields person skilled in the art, the non-intrinsically safe made according to foregoing invention content to the present invention
The modifications and adaptations of property, should still fall within protection scope of the present invention.Mentioned raw materials following at the same time are unspecified, are
Commercial product；The processing step or preparation method not referred in detail be processing step known to a person skilled in the art or
Preparation method.
Embodiment 1
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g urea is placed in ceramic crucible, then by alumina formwork of the aperture in the range of 40nm, that Open Side Down is straight
Connect and be placed in above urea, sealed crucible is placed in Muffle furnace, is warming up to 130 DEG C and keeps the temperature 10h, proceeds to 600 DEG C and keep the temperature
2h, the presoma for making to be deposited in alumina formwork duct are pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample, the phosphoric acid solution for being 0.5mol/L with concentration are taken out
Alumina formwork is removed, is handled by suction filtration, dries, obtains graphite phase carbon nitride nanotube dust material.
The stereoscan photograph of 1 gained graphite phase carbon nitride nanotube dust material of embodiment as shown in Figure 1, is swept by this
Retouch electromicroscopic photograph to understand, the pattern of gained graphite phase carbon nitride nanotube has a good uniformity, its good crystallinity, and tube wall is equal
Evenness is high.
Embodiment 2
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g thiocarbamides are placed in ceramic crucible, then by alumina formwork of the aperture in the range of 200nm, Open Side Down
It is placed directly within above urea, sealed crucible is placed in Muffle furnace, is warming up to 150 DEG C and keeps the temperature 6h, proceeds to 550 DEG C and keep the temperature
5h, the presoma for making to be deposited in alumina formwork duct are pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample, the phosphoric acid solution for being 0.5mol/L with concentration are taken out
Alumina formwork is removed, is handled by suction filtration, dries, obtains graphite phase carbon nitride nanotube dust material.
Embodiment 3
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g double focusing cyanamides are placed in ceramic crucible, then by alumina formwork opening of the aperture in the range of 20nm to
Under be placed directly within above urea, sealed crucible is placed in Muffle furnace, is warming up to 100 DEG C and keeps the temperature 10h, proceeds to 580 DEG C simultaneously
1.5h is kept the temperature, the presoma for making to be deposited in alumina formwork duct is pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample, the hydrochloric acid solution for being 0.5mol/L with concentration are taken out
Alumina formwork is removed, is handled by suction filtration, dries, obtains graphite phase carbon nitride nanotube dust material.
Embodiment 4
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g melamines are placed in ceramic crucible, then by alumina formwork opening of the aperture in the range of 40nm to
Under be placed directly within above urea, sealed crucible is placed in Muffle furnace, is warming up to 200 DEG C and keeps the temperature 1h, proceeds to 650 DEG C and protect
Warm 0.5h, the presoma for making to be deposited in alumina formwork duct are pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample, the phosphoric acid solution for being 0.1mol/L with concentration are taken out
Alumina formwork is removed, is handled by suction filtration, dries, obtains graphite phase carbon nitride nanotube dust material.
Embodiment 5
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g double focusing cyanamides are placed in ceramic crucible, then by alumina formwork opening of the aperture in the range of 40nm to
Under be placed directly within above urea, sealed crucible is placed in Muffle furnace, is warming up to 180 DEG C and keeps the temperature 4h, proceeds to 620 DEG C and protect
Warm 2h, the presoma for making to be deposited in alumina formwork duct are pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample, the sulfuric acid solution for being 0.5mol/L with concentration are taken out
Alumina formwork is removed, is handled by suction filtration, dries, obtains graphite phase carbon nitride nanotube dust material.
Embodiment 6
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g thiocarbamides are placed in ceramic crucible, then by alumina formwork of the aperture in the range of 10nm, that Open Side Down is straight
Connect and be placed in above urea, sealed crucible is placed in Muffle furnace, is warming up to 150 DEG C and keeps the temperature 6h, proceeds to 590 DEG C and keep the temperature
2h, the presoma for making to be deposited in alumina formwork duct are pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample, the phosphoric acid solution for being 0.5mol/L with concentration are taken out
Alumina formwork is removed, is handled by suction filtration, dries, obtains graphite phase carbon nitride nanotube dust material.
Embodiment 7
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g urea is placed in ceramic crucible, then by alumina formwork of the aperture in the range of 40nm, that Open Side Down is straight
Connect and be placed in above urea, sealed crucible is placed in Muffle furnace, is warming up to 130 DEG C and keeps the temperature 7h, proceeds to 650 DEG C and keep the temperature
0.5h, the presoma for making to be deposited in alumina formwork duct are pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample is taken out, the hydrochloric acid solution for being 3mol/L with concentration is gone
Alumina template, is handled by suction filtration, and drying, obtains graphite phase carbon nitride nanotube dust material.
Embodiment 8
A kind of preparation method of graphite phase carbon nitride nanotube, it is comprised the technical steps that：
1) 5g urea is placed in ceramic crucible, then by alumina formwork of the aperture in the range of 40nm, that Open Side Down is straight
Connect and be placed in above urea, sealed crucible is placed in tube furnace, is warming up to 130 DEG C and keeps the temperature 7h, proceeds to 600 DEG C and keep the temperature
2h, the presoma for making to be deposited in alumina formwork duct are pyrolyzed；
2) when step 1) ceramic crucible temperature is down to room temperature, sample, the phosphoric acid solution for being 0.5mol/L with concentration are taken out
Alumina formwork is removed, is handled by suction filtration, dries, obtains graphite phase carbon nitride nanotube dust material.
Above-described embodiment is the preferred embodiment of the present invention, all with similar technique of the invention and the equivalence changes made,
The protection category of the present invention should all be belonged to.
Claims (5)
1. a kind of preparation method of graphite phase carbon nitride nanotube, it is characterised in that comprise the technical steps that：
1) presoma is placed in ceramic crucible, then by alumina formwork of the aperture in the range of 10~200nm, Open Side Down
It is placed directly within above presoma, sealed crucible is placed in Muffle furnace or tube furnace, and presoma is made under cryogenic conditions in aluminium oxide
Deposited in the duct of template, continue to heat up, the presoma for making to be deposited in alumina formwork duct is pyrolyzed；
2) with concentration be 0.1~3mol/L dilute acid soln remove alumina formwork, after centrifuged or suction filtration processing, drying,
Obtain finished product.
A kind of 2. preparation method of graphite phase carbon nitride nanotube according to claim 1, it is characterised in that：In step 1)
The presoma is selected from least one of urea, thiocarbamide, double focusing cyanamide, melamine.
A kind of 3. preparation method of graphite phase carbon nitride nanotube according to claim 1, it is characterised in that：In step 1)
The temperature of the low temperature depositing is 100~200 DEG C, and soaking time is 1~10h.
A kind of 4. preparation method of graphite phase carbon nitride nanotube according to claim 1, it is characterised in that：In step 1)
The temperature of the pyrolysis is 550~650 DEG C, and pyrolysis time is 0.5~5h.
A kind of 5. preparation method of graphite phase carbon nitride nanotube according to claim 1, it is characterised in that：In step 2)
The dilute acid soln is selected from least one of phosphoric acid solution, hydrochloric acid solution, sulfuric acid solution.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108821249A (en) * | 2018-06-12 | 2018-11-16 | 桑德集团有限公司 | Carbon-nitrogen material and preparation method thereof and lithium sulfur battery anode material and lithium-sulfur cell comprising it |
| CN109012727A (en) * | 2018-08-08 | 2018-12-18 | 南京晓庄学院 | A kind of Half-metallic C4N3Nano-plates and its preparation method and application |
| CN109603880A (en) * | 2018-12-26 | 2019-04-12 | 湖南大学 | Hollow tubular carbon nitride photocatalyst and its preparation method and application |
| CN110124719A (en) * | 2019-05-21 | 2019-08-16 | 电子科技大学 | A kind of preparation method and application of highly crystalline carbonitride catalysis material |
| CN112820921A (en) * | 2019-11-15 | 2021-05-18 | 中国科学院大连化学物理研究所 | Nafion/g-C3N4Composite membrane and preparation method and application thereof |
| CN113247869A (en) * | 2021-05-19 | 2021-08-13 | 东南大学 | Preparation method of carbon nitride material, carbon nitride material prepared by preparation method and application of carbon nitride material |
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