CN104986742A - Bead-chain-like graphitized carbon nitride nano material and preparation method thereof - Google Patents
Bead-chain-like graphitized carbon nitride nano material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a bead-chain-like graphitized carbon nitride nano material and a preparation method thereof and belongs to the technical field of semi-conductor material preparation. The bead-chain-like graphitized carbon nitride nano material adopts a bead-chain-like structure formed by arranging raised bead-like objects on the surfaces of graphitized carbon nitride nano-rods, wherein the diameter of the bead-like objects is 200-800 nm; the space between the bead-like objects is 200-800 nm; the nano-rods connected with the bead-like objects are 80-500 nm in diameter, and 5-13.6 [mu]m in chain length. The preparation method comprises the following steps: dissolving melamine into an alcohol solution to obtain an initial solution; then adding a nitric acid solution, stirring and precipitating to produce carbon nitride precursor solid powder; after that, forging to obtain the bead-chain-like graphitized carbon nitride nano material. The preparation process is simple, and the obtained product has the advantages of smooth surface, uniform size, relatively good dispersity and the like, and can serve as a template for preparing other materials or as carriers of noble metal nano-particles.
Description
Technical field
The invention belongs to technical field of semiconductor material preparation, relate to kind bead chain shape greying azotized carbon nano material and preparation method thereof.
Background technology
Class graphitic nitralloy carbon is the semiconductor material of one comparatively low energy gap (energy gap is 2.7eV), and has higher Carrier recombination speed.Class graphitic nitralloy carbon has the advantage such as Heat stability is good, stable chemical nature, and not containing metal, the feature such as nontoxic, visible light-responded, it is made to become a kind of novel photocatalyst, extensive concern is subject in catalyst field, particularly its photoelectric property, photodegradation organic dye, catalyse organic reaction, photodissociation aquatic products hydrogen, makes it be widely used in a lot of field such as electronics, optics, biology.
At present, the method preparing nano-graphite carbonitride is a lot, can be divided into generally: high temperature and high pressure synthesis, physical chemistry vapor phase deposition method, chemical deposition, high-temperature polymerization, template etc.Although template can obtain the sample of different-shape, the method complex process, morphology controllable are poor, and synthesis difficulty is higher.Wherein high-temperature polymerization refers to the one directly and easily method preparing greying carbonitride polymkeric substance by presoma self polycondensation under hot conditions, but the pattern of the sample that the method obtains is mostly bulk comparatively thick-layer shape, is difficult to the sample obtaining other pattern.In order to can different-shape be prepared and the higher pure phase greying azotized carbon nano material of crystallinity, need to update high-temperature polymerization and innovate.
Summary of the invention
The present invention is directed to the weak point that high-temperature polymerization prepares graphitization nano carbonitride, provide a kind bead chain shape greying azotized carbon nano material, greying carbonitride pattern of the present invention is special, is class bead chain shape, good crystallinity, few surface defects.Can be used as the template preparing other material, or as the carrier of noble metal nano particles, have broad application prospects in photocatalysis to degrade organic matter, other Application Areass such as nano particle load and Photocatalyzed Hydrogen Production, also can be widely used in bio-pharmaceutical load etc.
Meanwhile, additionally provide the preparation method of above-mentioned class bead chain shape greying azotized carbon nano material, this preparation method has the simple advantage of technique.
The concrete technical scheme of the present invention is as follows:
One kind bead chain shape greying azotized carbon nano material, it is characterized in that: be the class bead chain shape structure convexed to form by greying azotized carbon nano rod surface alignment class pearl, the diameter dimension of class pearl is 200 ~ 800nm, class pearl spacing 200 ~ 800nm, the nanorod diameter connecting class pearl is 80 ~ 500nm, and chain length is 5 ~ 13.6 μm.
Its preparation method is: by melamine goes in alcohol liquid, obtain initial soln; Then add salpeter solution, stir and separate out precipitation, obtained carbon nitride precursor pressed powder, then under protection of inert gas, obtain class bead chain shape greying azotized carbon nano material by calcining.
The preparation method of above-mentioned class bead chain shape greying azotized carbon nano material, comprises the following steps:
(1) trimeric cyanamide is added in alcohol liquid, stir and obtain uniform initial soln;
(2) in the initial soln of step (1), dropwise add salpeter solution, stir, separate out precipitation;
(3) precipitation step (2) obtained, through centrifugation, washing, drying, obtains presoma pressed powder;
(4) presoma pressed powder step (3) obtained, under protection of inert gas, is heated to 380 ~ 450 DEG C, is fired to trimeric cyanamide and decomposes completely, be cooled to room temperature, obtains class bead chain shape greying azotized carbon nano material.
In step (1), the concentration that described trimeric cyanamide is dissolved in alcohol liquid is 0.16 ~ 0.40mol/L, preferred 0.16mol/L.
In step (1), described alcohol liquid is the mixed solution of ethylene glycol or ethylene glycol and glycerol, and in described mixed solution, ethylene glycol and glycerol volume ratio are 1 ~ 2:1.
In step (2), described salpeter solution is nitre aqueous acid, and concentration is 0.1 ~ 0.5mol/L;
In step (2), the volume ratio of described salpeter solution and alcohol liquid is 1 ~ 3.6:1.
In step (2), the Keep agitation time is 10 ~ 60 min.
In step (3), described washing, washing composition is followed successively by water and ethanol.
In step (4), described rare gas element is nitrogen.
In step (4), described calcining, temperature rise rate is 10 DEG C/min, and calcination time is 1 ~ 5h.
Reaction mechanism of the present invention is: by nitrate radical in salpeter solution and hydrogen ion self-assembly, makes trimeric cyanamide protonated simultaneously, obtains protonated presoma pressed powder, is then polymerized through high-temperature calcination under protection of inert gas and then obtains product.The amino of trimeric cyanamide is active reactive group, after adding nitric acid, easily carries out trimeric cyanamide protonation process, reduces the solubleness of trimeric cyanamide in alcohol liquid.Calcination process, protonated trimeric cyanamide becomes layered polymer along the polymerization of white precipitate nanofiber direction, continuation zone of heating shaped polymer reaches certain thickness and is curled into rod, because layered polymer is in uneven thickness, therefore the nanorod surfaces after curling forms class bead chain shape pattern, and in calcination temperature range, temperature of reaction is higher, curling more closely knit of polymkeric substance, crystallinity is better.
Class bead chain shape greying azotized carbon nano material of the present invention: pattern is class bead chain shape, degree of crystallinity is high, there is less surface imperfection, preparation process does not use template, only carry out presoma process with nitric acid, class bead chain shape greying carbonitride can be synthesized by high temperature polymerization, enrich the pattern of greying carbonitride, had wide application prospects in the novel material energy.The present invention is better than the product of other template synthesis, and technique is simple, and cost is lower, and pattern is special, can be used for the template preparing other material, has good application prospect.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the class bead chain shape greying carbonitride that the embodiment of the present invention 1 is synthesized;
Fig. 2 is scanning electron microscope (SEM) photo of the class bead chain shape greying carbonitride that the embodiment of the present invention 1 is synthesized;
Fig. 3 is scanning electron microscope (SEM) photo of the class bead chain shape greying carbonitride of the 2-in-1 one-tenth of the embodiment of the present invention;
Fig. 4 is scanning electron microscope (SEM) photo of the class bead chain shape greying carbonitride that the embodiment of the present invention 3 is synthesized;
Fig. 5 is scanning electron microscope (SEM) photo of the class bead chain shape greying carbonitride that the embodiment of the present invention 9 is synthesized;
Fig. 6 is scanning electron microscope (SEM) photo of the class bead chain shape greying carbonitride that the embodiment of the present invention 10 is synthesized;
Fig. 7 is scanning electron microscope (SEM) photo of the greying carbonitride of comparative example 1 of the present invention synthesis;
Fig. 8 is scanning electron microscope (SEM) photo of the greying carbonitride of the 2-in-1 one-tenth of comparative example of the present invention;
Fig. 9 is scanning electron microscope (SEM) photo of the greying carbonitride of comparative example 5 of the present invention synthesis.
Embodiment
Below by embodiment, the present invention will be further elaborated, it is to be understood that following explanation is only to explain the present invention, do not limit its content.
embodiment 1
1.1 take 1.0g(0.0079mol) trimeric cyanamide joins in 50mL ethylene glycol, stirs 30min, to obtaining uniform initial soln;
1.2 get 20 mL initial solns, are that the aqueous nitric acid 24mL of 0.3mol/L dropwise adds in initial soln by the concentration prepared, Keep agitation 30min, until precipitation is separated out completely;
1.3 above-mentioned precipitation is carried out centrifugation after wash 2 times with water after, then use ethanol centrifuge washing 2 times, dry, obtain presoma white solid powder;
Presoma pressed powder obtained above is placed in tube furnace by 1.4; under nitrogen atmosphere protection, be warming up to 380 DEG C according to 10 DEG C/min temperature rise rate, insulation 2h calcines; naturally cool to room temperature, namely obtain class bead chain shape greying carbonitride sample (as shown in Figure 2).
The constitutional features of gained class bead chain shape is: the diameter dimension of class pearl is 320 ~ 780nm.
Fig. 1 is the X ray diffracting spectrum of sample, and as can be seen from the figure, gained class bead chain shape carbonitride is graphite type carbon nitride.Fig. 2 is the stereoscan photograph of sample, and can find out in figure that class bead chain shape carbonitride diameter dimension is 320 ~ 780nm scope, class bead chain shape thing spacing is 200 ~ 800nm; The nanorod diameter connecting class pearl is 80 ~ 300nm; Chain length is 5 ~ 13.6 μm.
embodiment 2
Preparation method with embodiment 1, unlike: after instillation concentration is the aqueous nitric acid of 0.5mol/L 14.4mL, churning time is 10min; 400 DEG C of calcining 1h.As shown in Figure 3, the constitutional features of gained class bead chain shape is gained class bead chain shape greying carbonitride pattern: the diameter dimension of class pearl is 300 ~ 500nm, class pearl spacing 200 ~ 500nm; The nanorod diameter connecting class pearl is 80 ~ 250nm; Chain length is 5 ~ 12.5nm.
embodiment 3
Preparation method with embodiment 1, unlike: after instillation concentration is the aqueous nitric acid 14.4mL of 0.5mol/L, churning time is 30min, 450 DEG C of calcining 1h.As shown in Figure 4, the constitutional features of gained class bead chain shape is gained class bead chain shape greying carbonitride pattern: the diameter dimension of class pearl is 300 ~ 500nm, class pearl spacing 200 ~ 500nm; The nanorod diameter connecting class pearl is 80 ~ 250nm; Chain length is 5 ~ 12.5nm.
embodiment 4
Preparation method with embodiment 1, unlike: instillation 0.3mol/L aqueous nitric acid 24mL after, churning time is 60min.Gained class bead chain shape greying carbonitride pattern: the diameter dimension of class pearl is 320 ~ 780nm, class pearl spacing 200 ~ 800nm; The nanorod diameter connecting class pearl is 80 ~ 300nm.
embodiment 5
Preparation method with embodiment 1, unlike: get 1.0g trimeric cyanamide and be directly dissolved in 20mL ethylene glycol and stir, obtain even initial soln.Gained class bead chain shape greying carbonitride pattern: the diameter dimension of class pearl is 320 ~ 780nm, class pearl spacing 200 ~ 800nm; The nanorod diameter connecting class pearl is 80 ~ 300nm.
embodiment 6
Preparation method with embodiment 1, unlike: 450 DEG C calcining 3h.Gained class bead chain shape greying carbonitride pattern gained class bead chain shape greying carbonitride pattern: the diameter dimension of class pearl is 400 ~ 800nm, class pearl spacing 500 ~ 800nm; The nanorod diameter connecting class pearl is 100 ~ 300nm.
embodiment 7
Preparation method with embodiment 1, unlike: 0.5g trimeric cyanamide is joined in 20mL ethylene glycol.Gained class bead chain shape greying carbonitride pattern: the diameter dimension of class pearl is 300 ~ 800nm, class pearl spacing 200 ~ 800nm; The nanorod diameter connecting class pearl is 80 ~ 300nm.
embodiment 8
Preparation method with embodiment 1, unlike: 380 DEG C calcining 5h.Gained class bead chain shape greying carbonitride pattern: the diameter dimension of class pearl is 300 ~ 800nm, class pearl spacing 500 ~ 800nm; The nanorod diameter connecting class pearl is 80 ~ 300nm.
embodiment 9
Preparation method is with embodiment 1, unlike: trimeric cyanamide is dissolved in the ethylene glycol and glycerol alcohol mixture liquid that volume ratio is 1:1, class bead chain shape greying carbonitride is obtained after calcining, pattern is as shown in Figure 5: the diameter dimension of class pearl is 400 ~ 800nm, class pearl spacing 500 ~ 800nm; The nanorod diameter connecting teardrop shape thing is 80 ~ 500nm.
embodiment 10
Preparation method is with embodiment 1, unlike: trimeric cyanamide is dissolved in the ethylene glycol and glycerol alcohol mixture liquid that volume ratio is 2:1, class bead chain shape greying carbonitride is obtained after calcining, pattern is as shown in Figure 6: the diameter dimension of class pearl is 400 ~ 800nm, class pearl spacing 500 ~ 800nm; The nanorod diameter connecting teardrop shape thing is 80 ~ 500nm.
embodiment 11
Preparation method is with embodiment 1, unlike: trimeric cyanamide is dissolved in the ethylene glycol and glycerol alcohol mixture liquid that volume ratio is 1.5:1, class bead chain shape greying carbonitride is obtained: the diameter dimension of class pearl is 300 ~ 800nm, class pearl spacing 500 ~ 800nm after calcining; The nanorod diameter connecting class pearl is 80 ~ 500nm.
comparative example 1
12.1 take 1.0g trimeric cyanamide joins in 20mL ethylene glycol, stirs 30min to homogeneous solution;
The 0.3M sulphuric acid soln prepared dropwise adds in above-mentioned solution by 12.2, Keep agitation 30min, until precipitation is separated out completely;
Above-mentioned precipitation to be carried out with after water centrifuge washing 2 times after centrifugation by 13.3, then use ethanol centrifuge washing 2 times, dry, obtain presoma pressed powder;
Presoma obtained above is placed in tube furnace by 13.4, is warming up to 380 DEG C under nitrogen atmosphere protection according to 10 DEG C/min temperature rise rate, and insulation 2h calcines, and naturally cool to room temperature, do not generate bead chain shape greying carbonitride sample, pattern is as Fig. 7.
comparative example 2
Preparation method with embodiment 1, unlike: 500 DEG C calcining 2h, do not generate bead chain shape greying carbonitride sample, pattern is as Fig. 8.
comparative example 3
Preparation method with embodiment 1, unlike: 365 DEG C calcining 2h, do not generate bead chain shape greying carbonitride sample.
comparative example 4
Preparation method with embodiment 1, unlike: heat-up rate is 5 DEG C/min, does not generate bead chain shape greying carbonitride sample.
comparative example 5
Preparation method with embodiment 1, unlike: alcohol liquid is ethylene glycol and glycerol, and its volume ratio is 1:2, and do not generate bead chain shape greying carbonitride sample, pattern is as Fig. 9.
comparative example 6
Preparation method with embodiment 1, unlike: sample calcines 2h in atmosphere, does not obtain class bead chain shape greying carbonitride sample.
Claims (10)
1. a kind bead chain shape greying azotized carbon nano material, it is characterized in that: be the class bead chain shape structure convexed to form by greying azotized carbon nano rod surface alignment class pearl, the diameter dimension of class pearl is 200 ~ 800nm, class pearl spacing 200 ~ 800nm, the nanorod diameter connecting class pearl is 80 ~ 500nm, and chain length is 5 ~ 13.6 μm.
2. a preparation method for class bead chain shape greying azotized carbon nano material described in claim 1, is characterized in that: by melamine goes in alcohol liquid, obtain initial soln; Then add salpeter solution, stir and separate out precipitation, obtained carbon nitride precursor pressed powder, then under protection of inert gas, obtain class bead chain shape greying azotized carbon nano material by calcining.
3. preparation method according to claim 2, is characterized in that, comprises the following steps:
(1) trimeric cyanamide is added in alcohol liquid, stir and obtain uniform initial soln;
(2) in the initial soln of step (1), dropwise add salpeter solution, stir, separate out precipitation;
(3) precipitation step (2) obtained, through centrifugation, washing, drying, obtains presoma pressed powder;
(4) presoma pressed powder step (3) obtained, under protection of inert gas, is heated to 380 ~ 450 DEG C, is fired to trimeric cyanamide and decomposes completely, be cooled to room temperature, obtains class bead chain shape greying azotized carbon nano material.
4. preparation method according to claim 3, is characterized in that: in step (1), and the concentration that described trimeric cyanamide is dissolved in alcohol is 0.16 ~ 0.40mol/L.
5. preparation method according to claim 3, is characterized in that: in step (1), and described alcohol liquid is the mixed solution of ethylene glycol or ethylene glycol and glycerol, and in described mixed solution, ethylene glycol and glycerol volume ratio are 1 ~ 2:1.
6. preparation method according to claim 3, is characterized in that: in step (2), and described salpeter solution is nitre aqueous acid, and concentration is 0.1 ~ 0.5mol/L; The volume ratio of described salpeter solution and alcohol liquid is 1 ~ 3.6:1.
7. preparation method according to claim 3, is characterized in that: in step (2), and the Keep agitation time is 10 ~ 60 min.
8. preparation method according to claim 3, is characterized in that: in step (3), and described washing, washing composition is followed successively by water and ethanol.
9. preparation method according to claim 3, is characterized in that: in step (4), and described rare gas element is nitrogen.
10. preparation method according to claim 3, is characterized in that: in step (4), described calcining, and temperature rise rate is 10 DEG C/min, and calcination time is 1 ~ 5h.
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