CN106744745A - A kind of graphite phase carbon nitride nanotube of carbon doping and preparation method thereof - Google Patents
A kind of graphite phase carbon nitride nanotube of carbon doping and preparation method thereof Download PDFInfo
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- 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
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Abstract
Graphite phase carbon nitride nanotube the invention discloses a kind of carbon doping and preparation method thereof, its preparation process is:Melamine is dispersed in the ethanol solution of TSL 8330 first, centrifugal drying obtains solid powder after hydro-thermal reaction;Will(3 mercaptopropyis)Trimethyl oxosilane and tetraethyl orthosilicate mixing and stirring, add the mixed solution of second alcohol and water to be again stirring for, the SiO of centrifugation MPS modifications2Solution.The solid powder of the melamine that will be pre-processed adds the SiO of MPS modifications2In solution, it is centrifuged after stirring, dried, calcine to obtain product, product is performed etching by HF solution is obtained final product.Preparation process of the present invention is novel, convenient, controllability is strong, the nanotube of gained has size more uniform, the advantages of tube wall is relatively thin, electric conductivity is preferable, photocatalysis property is excellent, can be used to build various heterojunction structures, have good application potential at aspects such as photocatalysis degradation organic contaminant, photodissociation aquatic products hydrogen.
Description
Technical field
Graphite phase carbon nitride nanotube the present invention relates to a kind of carbon doping and preparation method thereof, belongs to semi-conducting material
Doping vario-property preparing technical field.
Background technology
Single similar graphitization carbonitride (g-C3N4) as a kind of organic polymer semiconductor, due to its good physics and chemistry
Property, easily prepare, stable existence, energy gap, for 2.7eV such as can be excited at the advantage in visible-range, make it in air
As the new organic photochemical catalyst of one kind, can be used for photodissociation aquatic products hydrogen and produce the aspects such as oxygen, degradable organic pollutant, hydrogen storage, thus
Can be widely used in many fields such as environment, the energy, biology.
However, due to the body phase g-C of simple high temperature polymerization preparation3N4Layer it is poor with interlayer electric conductivity, make its light induced electron and
Hole-recombination rate is higher, and photocatalytic activity is poor.People are frequently with method optimizings such as doping, nano modification, structure heterojunction structures
Its performance.By numerous studies, ion doping g-C3N4Nano material also has made great progress.But, the g-C after doping3N4
Be still present the difficult regulation and control of pattern, it is difficult prepare, the deficiency such as pattern is single, by the method for the regulation and control carbonitride pattern that adulterates report compared with
It is few.
The content of the invention
The present invention is directed to g-C3N4A kind of single weak point of pattern of doping vario-property, there is provided carbon doping graphite-phase nitridation
The preparation method of CNT, the method process is simple, the carbonitride pattern after the doping of gained is special, is nanotube, tube wall
Relatively thin, crystallinity is good, surface defect is less.
Concrete technical scheme of the present invention is as follows:
The invention provides a kind of graphite phase carbon nitride nanotube of carbon doping, the graphite phase carbon nitride pattern of the carbon doping is
Hollow nanotube, nanotube is formed by nanometer sheet curling, and thickness of pipe wall is 10nm-15nm, and nanotube length is less than 1 μm, directly
Footpath size is 95-200 nm.
Present invention also offers a kind of preparation method of the graphite phase carbon nitride nanotube of carbon doping, comprise the following steps:
(1)Melamine is scattered in the ethanol solution of TSL 8330 in a kettle., high temperature hydro-thermal is anti-
Ying Hou, centrifugation is dried to obtain solid powder;
(2)To be added in tetraethyl orthosilicate(3- mercaptopropyis)Trimethyl oxosilane, stirring, obtains homogeneous solution A;
(3)Ethanol, water are mixed and stirred for, solution B is obtained;
(4)By in solution A addition solution B, after stirring certain hour, precipitation is centrifugally separating to obtain;
(5)The precipitation that step (4) is obtained is dispersed in water again, the solid powder that step (1) is obtained is subsequently added, stirring is equal
After even, dried after centrifugation, washing, obtain white solid powder, white solid powder is placed in quartz boat in inert gas
The lower calcining of protection, obtains product;
(6)The product obtained after being calcined with the HF solution etches of high concentration, through centrifuge washing, drying, obtains the nitridation of carbon doping
CNT.
Further, step(1)In, the melamine is dense in the ethanol solution of TSL 8330
It is 0.015~0.019g/mL to spend;The volume ratio of the TSL 8330 and ethanol is 0.1 × 10-4~2.5 ×
10-4。
Further, in step (1), above-mentioned hydro-thermal reaction is to react 24h under the conditions of 200-220 DEG C of temperature.
Further, in step (2), the tetraethyl orthosilicate with(3- mercaptopropyis)The volume ratio of trimethyl oxosilane is
100~250:1, the mixing time is 2h.
Further, in step (3), the ratio of the ethanol and water is 10:1 ~ 2, the time of the stirring is 30min.
Further, in step (4), the solution A is 1 with the volume ratio of solution B:108 ~ 118, the ratio of optimization is 1:
113 ~ 115, the time of the stirring is 6-8h.
Further, in step (5), the step(1)The solid powder for obtaining is 1.2 with the mass ratio of tetraethyl orthosilicate
~ 3.3, the time of the stirring is 24h.
Further, in step (5), the calcining is under the protection of nitrogen, 2 to be reacted after being warming up to 560 °C -600 °C
Hour.
Further, in step (6), the mass fraction of the hydrofluoric acid solution is 20 % ~ 40 %, and etch period is 24-
48h。
The present invention is using the method for auto-dope in numerous g-C3N4Be also in doping it is very meaningful, it avoid impurity from
The introducing of son, directly using the method for carbon atom doping, the substitution of C makes the carbon atom of doping and g-C3N4Shape between heterocycle in structure
Into delocalized pi-bond, the ratio of carbon and nitrogen-atoms is improved, so as to improve electric conductivity, promote the migration of light induced electron.
Appearance of nano material of the invention is the azotized carbon nano pipe of carbon doping, and tube wall is relatively thin, and preparation process is to presoma
Pre-processed, recycle the silica of sulfydryl modification to make matrix template, first obtained presoma/SiO2Material, then use hydrogen
Fluoric acid etches template, and removal silica is the azotized carbon nano pipe that can obtain carbon doping, is enriching graphitization carbonitride
Carbon doping is also carried out while pattern to it to be modified, meaning is larger in terms of material modification and topography optimization.The present invention is better than
The single product of the pattern of other element doping carbonitrides, new technology is simple, and cost is relatively low, and its method can be used to prepare other
The doping vario-property of material, with preferable application prospect.
Brief description of the drawings
The C-g-C of the synthesis of Fig. 1 embodiment of the present invention 13N4X-ray diffraction (XRD) collection of illustrative plates of nanotube.
The C-g-C of the synthesis of Fig. 2 embodiment of the present invention 13N4ESEM (SEM) photo of nanotube.
The C-g-C of the synthesis of Fig. 3 embodiment of the present invention 13N4The curve of photocatalytic degradation RhB under nanotube visible ray.
Fig. 4 embodiment of the present invention it is 2-in-1 into C-g-C3N4ESEM (SEM) photo of nanotube.
The C-g-C of the synthesis of Fig. 5 embodiment of the present invention 33N4ESEM (SEM) photo of nanotube.
The g-C of Fig. 6 synthesis of comparative example 1 of the present invention3N4ESEM (SEM) photo.
Fig. 7 comparative examples of the present invention it is 2-in-1 into C-g-C3N4ESEM (SEM) photo of nano material.
Fig. 8 comparative examples of the present invention it is 2-in-1 into C-g-C3N4The curve of photocatalytic degradation RhB under nano material visible ray.
Specific embodiment
Below by embodiment, the present invention will be further elaborated, it should be appreciated that, the description below merely to
The present invention is explained, its content is not defined.
Embodiment 1
1.1 be with volume 100mL reactor in 0.75g melamines are dispersed in containing 8 μ L TSL 8330s
(APS) in 80ml ethanol solutions, at 200 DEG C after hydro-thermal 24h, centrifugation is dried to obtain solid powder;
1.2 add 2 μ L in 0.5mL tetraethyl orthosilicates (TEOS)(3- mercaptopropyis)Trimethyl oxosilane (MPS) solution,
Stir, obtain homogeneous solution A;
1.3 are mixed and stirred for 50mL ethanol, 5mL water uniformly, to obtain solution B;
1.4 solution As for obtaining step 1.2 are added in the solution B that step 1.3 is obtained, and after stirring 6h, it is heavy to be centrifugally separating to obtain
Form sediment;
1.5 are dispersed again in 30mL water the precipitation that step 1.4 is obtained, and are subsequently added and are repeated several times what 1.1 steps were obtained
The solid powder of the melamine after 1.2g treatment, after stirring, dries after centrifugation, washing, obtains white solid powder,
Powder is placed in quartz boat 580 DEG C of calcining 2h in nitrogen, heating rate is 5 DEG C/min, obtains product;
1.6 with the product obtained after calcining in HF solution etches step (5) that mass fraction is 40%, and etch period is 24h, warp
Centrifuge washing, drying, obtain the azotized carbon nano pipe of carbon doping.
Fig. 1 is the carbonitride of carbon doping and the g-C of undoped p carbon3N4The X ray diffracting spectrum of sample, can from figure
Go out, products obtained therefrom is graphite type carbon nitride, and (002) characteristic peak is compared to pure g-C3N4Offset to the right.Fig. 2 is the sample after being etched
The stereoscan photograph of product, as can be seen from the figure nanotube carbonitride length dimension is 1 μm, and nanotube is hollow-core construction, by
Nanometer sheet curling is formed, a diameter of 95 nm ~ 200 nm, and thickness of pipe wall is 10-15nm.Fig. 3 is that the graphite phase carbon nitride of carbon doping exists
The curve of photocatalytic degradation RhB under visible ray.
Embodiment 2
2.1 be with volume 100mL reactor in 1.2g melamines are dispersed in the 80ml ethanol solutions containing 20 μ L APS,
At 220 DEG C after hydro-thermal 24h, centrifugation is dried to obtain solid powder;
2.2 add 5 μ L in 0.5mL tetraethyl orthosilicates (TEOS)(3- mercaptopropyis)Trimethyl oxosilane (MPS) solution,
Stir, obtain homogeneous solution A;
2.3 are mixed and stirred for 50mL ethanol, 10mL water uniformly, to obtain solution B;
2.4 solution As for obtaining step 1.2 are added in the solution B that step 1.3 is obtained, and after stirring 6h, it is heavy to be centrifugally separating to obtain
Form sediment;
2.5 are dispersed again in 30mL water the precipitation that step 1.4 is obtained, and are subsequently added and are repeated several times what 2.1 steps were obtained
The solid powder of the melamine after 1.5g treatment, after stirring, dries after centrifugation, washing, obtains white solid powder,
Powder is placed in quartz boat 600 DEG C of calcining 2h in nitrogen, heating rate is 5 DEG C/min, obtains product;
2.6 are washed for 36 with the product obtained after HF solution etches step 3.5 burning that mass fraction is 40%, etch period through centrifugation
Wash, dry, obtain the azotized carbon nano pipe of carbon doping.
Fig. 4 is the stereoscan photograph of the sample after being etched, as can be seen from the figure nanotube carbonitride length dimension
It is 1 μm, nanotube is hollow-core construction, is formed by nanometer sheet curling, a diameter of 100 nm ~ 200 nm, thickness of pipe wall is 10-15 nm.
Embodiment 3
3.1 be with volume 100mL reactor in 1.5g melamines are dispersed in the 80ml ethanol solutions containing 10 μ L APS,
At 200 DEG C after hydro-thermal 24h, centrifugation is dried to obtain solid powder;
3.2 add 10 μ L in 1mL tetraethyl orthosilicates (TEOS)(3- mercaptopropyis)Trimethyl oxosilane (MPS) solution,
Stir, obtain homogeneous solution A;
3.3 are mixed and stirred for 100mL ethanol, 12mL water uniformly, to obtain solution B;
3.4 solution As for obtaining step 1.2 are added in the solution B that step 1.3 is obtained, and after stirring 6h, it is heavy to be centrifugally separating to obtain
Form sediment;
3.5 are dispersed again in 50mL water the precipitation that step 1.4 is obtained, and are subsequently added and are repeated several times what 2.1 steps were obtained
The solid powder of the melamine after 1.4g treatment, after stirring, dries after centrifugation, washing, obtains white solid powder,
Powder is placed in quartz boat 560 DEG C of calcining 2h in nitrogen, heating rate is 5 DEG C/min, obtains product;
3.6 burnt with HF solution etches step 3.5 that mass fraction is 20% after the product that obtains, etch period is 48h, through centrifugation
Wash, dry, obtain the azotized carbon nano pipe of carbon doping.
Fig. 5 is the stereoscan photograph of the sample after being etched, as can be seen from the figure the azotized carbon nano pipe of carbon doping
Length dimension is 1 μm, and nanotube is hollow-core construction, is formed by nanometer sheet curling, a diameter of 95 nm ~ 200 nm, and thickness of pipe wall is
10-15 nm。
Embodiment 4
Preparation method with embodiment 1, unlike:MPS additions be 5 μ L, the tubular looks of azotized carbon nano of gained carbon doping with
Embodiment 1 is identical, and nanotube length size is 1 μm, and nanotube is hollow-core construction, is formed by nanometer sheet curling, a diameter of 95 nm
~ 200 nm, thickness of pipe wall is 10-15 nm.
Embodiment 5
Preparation method with embodiment 2, unlike:It it is 210 DEG C in melamine pretreatment hydrothermal temperature;Etching concentration is 20 %
Hydrofluoric acid solution, etch period is 30h, and product morphology is same as Example 2, and the azotized carbon nano length of tube size of carbon doping is
1 μm, nanotube is hollow-core construction, is formed by nanometer sheet curling, a diameter of 95 nm ~ 200 nm, and thickness of pipe wall is 10-15 nm.
Embodiment 6
Preparation method is with unlike embodiment 3:Calcining heat is 600 DEG C;HF etch periods are 40h, and products therefrom pattern is same
Embodiment 3 is identical, and nanotube is hollow-core construction, is formed by nanometer sheet curling, and the azotized carbon nano length of tube size of carbon doping is 1
μm, a diameter of 95 nm ~ 200 nm, thickness of pipe wall is 10-15 nm.
Comparative example 1
1.1 add 2 μ L in 0.5mL tetraethyl orthosilicates (TEOS)(3- mercaptopropyis)Trimethyl oxosilane (MPS) solution,
Stir, obtain homogeneous solution A;
1.2 are mixed and stirred for 50mL ethanol, 5mL water uniformly, to obtain solution B;
1.3 solution As for obtaining step 1.1 are added in the solution B that step 1.2 is obtained, and after stirring 6h, it is heavy to be centrifugally separating to obtain
Form sediment;
1.4 are dispersed again in 30mL water the precipitation that step 1.4 is obtained, and are subsequently added 1.2g melamines, after stirring,
Dried after centrifugation, washing, obtain white solid powder, powder is placed in quartz boat 580 DEG C of calcining 2h in nitrogen, heated up
Speed is 5 DEG C/min, obtains product;
1.5 with the product obtained after calcining in HF solution etches step (5) that mass fraction is 40%, and etch period is 24h, warp
Centrifuge washing, drying;
Gained sample topography is loose porous layer structure, and it is the pure graphite-phase of undoped p not obtain nanotube, and product
Carbonitride, as shown in Figure 6.
Comparative example 2
9.1 be with volume 100mL reactor in 1.2g melamines are dispersed in 80ml ethanol, hydro-thermal 24h at 200 DEG C
Afterwards, centrifugation is dried to obtain solid powder;
9.2 add 2 μ L in 0.5mL tetraethyl orthosilicates (TEOS)(3- mercaptopropyis)Trimethyl oxosilane (MPS) solution,
Stir, obtain homogeneous solution A;
9.3 are mixed and stirred for 50mL ethanol, 20mL water uniformly, to obtain solution B;
9.4 solution As for obtaining step 1.2 are added in the solution B that step (3) is obtained, and after stirring 6h, it is heavy to be centrifugally separating to obtain
Form sediment;
9.5 are dispersed again in 50mL water the precipitation that step 1.4 is obtained, and are subsequently added and are repeated several times what 9.1 steps were obtained
Melamine after 1.5g treatment, after stirring, is dried after centrifugation, washing, obtains white solid powder, and powder is placed in
In quartz boat in nitrogen 500 DEG C calcining 2h, heating rate be 5 DEG C/min, obtain product;
9..6 the product obtained after being burnt with the HF solution etches step 3.5 that mass fraction is 20%, etch period is 24h, through centrifugation
Wash, dry, obtain the carbonitride of carbon doping.
Fig. 7 is the stereoscan photograph of product, is random pattern, and Fig. 8 is the song of product Photocatalytic Activity for Degradation RhB
Line.As can be seen from the figure the carbonitride of carbon doping does not form the pattern of nanotube, and its photocatalytic activity also compares carbon doping
Azotized carbon nano pipe poor activity.
Claims (10)
1. a kind of graphite phase carbon nitride nanotube of carbon doping, it is characterised in that the graphite phase carbon nitride pattern of the carbon doping
It is hollow nanotube, nanotube is formed by nanometer sheet curling, and thickness of pipe wall is 10nm-15nm, and nanotube length is less than 1 μm,
Diameter dimension is 95-200 nm.
2. a kind of preparation method of the graphite phase carbon nitride nanotube of carbon doping as claimed in claim 1, it is characterised in that bag
Include following steps:
(1) melamine is scattered in the ethanol solution of TSL 8330 in a kettle., high temperature hydro-thermal is anti-
Ying Hou, centrifugation is dried to obtain solid powder;
(2) will be added in tetraethyl orthosilicate(3- mercaptopropyis)Trimethyl oxosilane, stirring, obtains homogeneous solution A;
(3) ethanol, water are mixed and stirred for, obtain solution B;
(4) by solution A addition solution B, after stirring certain hour, it is centrifugally separating to obtain precipitation;
(5) precipitation that step (4) is obtained is dispersed in water again, is subsequently added the solid powder that step (1) is obtained, stirring is equal
After even, dried after centrifugation, washing, obtain white solid powder, white solid powder is placed in quartz boat in inert gas
The lower calcining of protection, obtains product;
(6) product obtained after being calcined with the HF solution etches of high concentration, through centrifuge washing, drying, obtains the nitridation of carbon doping
CNT.
3. preparation method according to claim 2, it is characterised in that step(1)In, the melamine is in aminopropyl
Concentration in the ethanol solution of trimethoxy silane is 0.015~0.019g/mL;The TSL 8330 and second
The volume ratio of alcohol is 0.1 × 10-4~2.5 × 10-4。
4. preparation method according to claim 3, it is characterised in that in step (1), the hydro-thermal reaction is in temperature
24h is reacted under the conditions of 200-220 DEG C.
5. preparation method according to claim 2, it is characterised in that in step (2), the tetraethyl orthosilicate with(3- mercaptos
Base propyl group)The volume ratio of trimethyl oxosilane is 100~250:1, the mixing time is 2h.
6. preparation method according to claim 2, it is characterised in that in step (3), the ratio of the ethanol and water is
10:1 ~ 2, the time of the stirring is 30min.
7. preparation method according to claim 2, it is characterised in that in step (4), the volume of the solution A and solution B
Than being 1:108 ~ 118, the ratio of optimization is 1:113 ~ 115, the time of the stirring is 6-8h.
8. preparation method according to claim 2, it is characterised in that in step (5), the step(1)The solid for obtaining
Powder is 1.2 ~ 3.3 with the mass ratio of tetraethyl orthosilicate, and the time of the stirring is 24h.
9. preparation method according to claim 2, it is characterised in that in step (5), the calcining is the protection in nitrogen
Under, reacted 2 hours after being warming up to 560 °C -600 °C.
10. preparation method according to claim 2, it is characterised in that in step (6), the quality of the hydrofluoric acid solution
Fraction is 20 % ~ 40 %, and etch period is 24-48h.
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CN107389755A (en) * | 2017-09-14 | 2017-11-24 | 湖南大学 | Electrochemical sensor for detecting mercury and its preparation method and application |
CN108686691A (en) * | 2018-03-26 | 2018-10-23 | 南昌航空大学 | A kind of preparation method of Gd2 O3 class graphite phase carbon nitride catalysis material |
CN108940347A (en) * | 2018-08-03 | 2018-12-07 | 鲁东大学 | A kind of carbon graphite phase carbon nitride composite material and preparation method and application |
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CN109248706A (en) * | 2018-10-25 | 2019-01-22 | 天津工业大学 | Carbon nanotube nitrogenizes carbon composite and synthetic method |
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