CN105692572A - Method for synthesizing g-C3N4 nanomaterials with various shapes - Google Patents

Method for synthesizing g-C3N4 nanomaterials with various shapes Download PDF

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CN105692572A
CN105692572A CN201610139398.6A CN201610139398A CN105692572A CN 105692572 A CN105692572 A CN 105692572A CN 201610139398 A CN201610139398 A CN 201610139398A CN 105692572 A CN105692572 A CN 105692572A
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nano material
nanomaterials
reaction temperature
synthesizing
response time
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赵慧敏
甘小荣
全燮
张耀斌
陈硕
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Dalian University of Technology
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Dalian University of Technology
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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
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • 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
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • 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
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C01P2004/36—Spheres fragmented
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a method for synthesizing g-C3N4 nanomaterials with various shapes and belongs to the field of material synthesis. On the basis of a solvent thermal synthesis method, under the condition that the temperature is not lower than 170 DEG C, formamide molecules polymerize to form the g-C3N4 nanomaterials. Through regulation and control on the reaction time which is not shorter than 0.5 h or the reaction temperature, the synthesized g-C3N4 nanomaterials can be in shapes of nanosheets, nanowires and nanofibers. According to the method for synthesizing the g-C3N4 nanomaterials, the shapes, sizes and thicknesses of the g-C3N4 nanomaterials are controllable, the synthesis technology is simple, and complex aftertreatment steps are omitted. With the adoption of the method, the problem that different synthesizing methods are required for the g-C3N4 nanomaterials with different shapes or dimensionality is solved.

Description

A kind of g-C for synthesizing different morphologies3N4The method of nano material
Technical field
The invention belongs to materials synthesis field, relate to a kind of g-C for synthesizing different morphologies3N4The method of nano material。
Background technology
Class graphite C3N4(g-C3N4) be a kind of can the C of stable existence3N4Allotrope。G-C3N4The a series of scientist of nano material energy catalysis " reaction of dream ", for instance photochemical reaction decomposition water, selective oxidation reaction, superactivity produce H-H reaction, have therefore attracted the extensive concern of researcher。Particularly, the g-C of different-shape and dimension (size)3N4There are, due to quantum confined effect, the physicochemical properties showing many uniquenesses in nano material, is therefore widely used in every field。Such as, the g-C of two dimension3N4Nanometer sheet is a kind of highly effective photocatalyst, can conversion solar energy, this big specific surface area mainly having benefited from it and edge active site efficiently。One-dimensional g-C3N4Nano wire can as good adsorbent, photocatalytic activity material and sensing material。Additionally, the g-C of zero dimension3N4Nano dot is a good fluorescent nano particles of class bio-compatibility, is widely used in fluorescence imaging and fluorescent optical sensor。
At present, g-C3N4The synthetic method of quantum dot the best is hydro-thermal and solvent-thermal method；Compared to chemical vapour deposition (CVD) and mechanical stripping method, liquid phase stripping method is synthesis two dimension g-C3N4The best approach of nanometer sheet。The g-C of different-shape and dimension3N4Generally requiring different synthetic methods, this gives research g-C3N4The trouble that the physicochemical properties of nano material are brought。Additionally, different-shape g-C3N4Diversity in nano material synthetic method is likely to result in has different requirements to experimental facilities, condition and step, can increase synthesis cost。Therefore, exploitation a kind of easy, effective, controlled, synthesize g-C on a large scale3N4The method of nano material has very important realistic meaning。
Studying report recently, Methanamide is when reaction temperature is 180 DEG C, and by solvent-thermal method, reaction 0.5h can synthesize g-C3N4Quantum dot (S.Barman, M.Sadhukhan, Facilebulkproductionofhighlybluefluorescentgraphiticcarb onnitridequantumdotsandtheirapplicationashighlyselective andsensitivesensorsforthedetectionofmercuricandiodideion sinaqueousmedia, J.Mater.Chem., 22:21832-21837.)。The g-C of this method synthesis3N4The productivity of quantum dot is very low, and separating-purifying trouble。Based on this method, in the present invention, by systematically regulating and controlling reaction temperature and response time, we successfully prepare g-C3N4Nanometer sheet, nano wire and nanofiber。In the condition and range that we give, it is possible to achieve to g-C3N4The regulation and control of the pattern of nano material, size and thickness。G-C prepared by the present invention3N4The productivity of nano wire and nanofiber can to more than 90%, owing to its size compares g-C3N4Quantum dot is big, and separating-purifying is also more prone to。
Summary of the invention
It is an object of the invention to build the g-C of a kind of simple synthetic method energy controlled synthesis different-shape, dimension and thickness3N4Nano material, the invention solves the g-C of different-shape or dimension3N4The problem that nano material needs different synthetic method。
Technical scheme:
A kind of g-C for synthesizing different morphologies3N4The method of nano material, step is as follows:
Methanamide is placed in politef reactor, it is ensured that its volume accounts for the 60-80% of politef reactor volume；
1) reaction temperature is 170-220 DEG C, and the response time is 0.5-8h, gained g-C3N4Appearance of nano material is based on nanometer sheet, and average thickness is 0.75nm, its average length 200nm, and mean breadth is 20nm；
2) range of reaction temperature is at 170-220 DEG C, and the response time is at 8-12h, gained g-C3N4Appearance of nano material is based on nano wire, and average thickness is 1.5nm, and its average length is 900nm, and mean breadth is 60nm；
3) reaction temperature is not less than 220 DEG C, and the response time is no less than 12h, gained g-C3N4Appearance of nano material is based on nanofiber, and average thickness is 1.75nm, and its average length is 5 μm, and mean breadth is 70nm。
The present invention has the effect that
(1) reactant is single, and course of reaction is simple, without loaded down with trivial details post processing。
(2) g-C synthesized3N4The size of nano material and morphology controllable。
(3) simple to operate, productivity is high (productivity of nanofiber is 93%)。
Accompanying drawing explanation
Fig. 1 reaction temperature is 180 DEG C, and the response time is the g-C of 8h gained3N4TEM picture。
Fig. 2 reaction temperature is 180 DEG C, and the response time is the g-C of 12h gained3N4TEM picture。
Fig. 3 reaction temperature is 180 DEG C, and the response time is the g-C of 12h gained3N4The XRD spectra of nano material。
Fig. 4 reaction temperature is 180 DEG C, and the response time is the g-C of 12h gained3N4The FT-IR spectrogram of nano material。
Fig. 5 reaction temperature is 220 DEG C, and the response time is the g-C of 12h gained3N4The TEM picture of nano material。
Fig. 6 reaction temperature is 220 DEG C, and the response time is the g-C of 12h gained3N4The XRD spectra of nano material。
Fig. 7 along with reaction temperature raise or the response time prolongation (reaction temperature and response time have one to remain unchanged, and we set scope in), the g-C of different-shape3N4The schematic diagram of nano material growth course。
Detailed description of the invention
The present invention relates to a kind of g-C for synthesizing different morphologies3N4The method of nano material。This method is based on solvent thermal reaction process, by Methanamide in high temperature polymerization, and regulate and control reaction temperature and the response time synthesizes the g-C of different-shape3N4Nano material。The g-C that the present invention relates to3N4Nanometer sheet, nano wire and nanofiber pattern, refer to based on this pattern in products therefrom, because g-C3N4Nano material is a slowly continuous growth course, as shown in Figure 7。
Below technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment。
Embodiment 1: a kind of g-C for synthesizing different morphologies3N4The method of nano material, comprises the steps:
(1) being poured into by Methanamide in politef reactor, it is ensured that its volume is 80%, when reaction temperature is 190 DEG C, the response time is 8h, and Methanamide generation polyreaction forms g-C3N4Nano material；
(2) it is centrifugal 1h under 13000 revs/min by step (1) products therefrom at rotating speed, and low-temperature vacuum drying can obtain g-C3N4Nano material powder。
Gained g-C3N4The pattern of nano material is as it is shown in figure 1, be nanometer sheet, and the meansigma methods of its length is 120nm。Embodiment 2: a kind of g-C for synthesizing different morphologies3N4The method of nano material, comprises the steps:
(1) being poured into by Methanamide in politef reactor, it is ensured that its volume is 80%, when reaction temperature is 190 DEG C, the response time is 12h, and Methanamide generation polyreaction forms g-C3N4Nano material；
(2) it is centrifugal 1h under 13000 revs/min by step (1) products therefrom at rotating speed, and low-temperature vacuum drying can obtain g-C3N4Nano material powder。
Gained g-C3N4The pattern of nano material is as in figure 2 it is shown, be nano wire, and its length is at hundreds of ran。Fig. 3 is the g-C of synthesis under this condition3N4The XRD spectra of nano material, by known two characteristic peaks in 2 θ=27 ° and 2 θ=56 ° of spectrogram respectively with g-C3N4The characteristic peak of (002) and (004) crystal face corresponding, it was shown that products therefrom is g-C3N4。Fig. 4 is g-C3N4The FT-IR spectrogram of nano material, be shown in 3316,3619,1686,1603,1393,1301,1104,802cm-1There is its characteristic peak in place, represents functional group-NH respectivelyx,-C=N-, s-triazine ring stretching vibration, further demonstrate that products therefrom is g-C3N4。
Embodiment 3: a kind of g-C for synthesizing different morphologies3N4The method of nano material, comprises the steps:
(1) being poured into by Methanamide in politef reactor, it is ensured that its volume is 80%, when reaction temperature is 220 DEG C, the response time is 12h, and Methanamide generation polyreaction forms g-C3N4Nano material；
(2) it is centrifugal 1h under 13000 revs/min by step (1) products therefrom at rotating speed, and low-temperature vacuum drying can obtain g-C3N4Nano material powder。
Fig. 5 shows that the pattern of products therefrom is nanofiber, and to be different from the less nano wire of degree of crook (example 2), due to high surface energy and functional group, they there occurs certain reunion。In Fig. 6 XRD spectra be shown in 2 θ=27 ° and 2 θ=56 ° place have two characteristic peaks, it was shown that the composition of product is g-C3N4。By can be calculated, g-C under the reaction condition described in this example3N4The productivity of nanofiber is 93%。
Following table is that the present invention is synthesized g-C3N4The summary of the synthesis condition of nanometer sheet, nano wire and nanofiber。Response time in form, order corresponding to reaction temperature was contrary, and namely the reaction temperature more high required response time is more short。

Claims (1)

1. the g-C being used for synthesizing different morphologies3N4The method of nano material, it is characterised in that step is as follows:
Methanamide is placed in politef reactor, it is ensured that its volume accounts for the 60-80% of politef reactor volume；
1) reaction temperature is 170-220 DEG C, and the response time is 0.5-8h, gained g-C3N4Appearance of nano material is based on nanometer sheet, and average thickness is 0.75nm, its average length 200nm, and mean breadth is 20nm；
2) range of reaction temperature is at 170-220 DEG C, and the response time is at 8-12h, gained g-C3N4Appearance of nano material is based on nano wire, and average thickness is 1.5nm, and its average length is 900nm, and mean breadth is 60nm；
3) reaction temperature is not less than 220 DEG C, and the response time is no less than 12h, gained g-C3N4Appearance of nano material is based on nanofiber, and average thickness is 1.75nm, and its average length is 5 μm, and mean breadth is 70nm。
CN201610139398.6A 2016-03-11 2016-03-11 Method for synthesizing g-C3N4 nanomaterials with various shapes Pending CN105692572A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106542509A (en) * 2016-10-19 2017-03-29 张家港市东大工业技术研究院 A kind of efficient method for preparing class Graphene carbonitride
CN108598506A (en) * 2016-07-29 2018-09-28 杭州富阳伟文环保科技有限公司 A kind of composite nano materials and its application
CN113680361A (en) * 2021-08-09 2021-11-23 电子科技大学 Cobalt-ruthenium bimetallic monatomic photocatalyst and preparation method and application thereof

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Patent Citations (2)

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Title
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108598506A (en) * 2016-07-29 2018-09-28 杭州富阳伟文环保科技有限公司 A kind of composite nano materials and its application
CN108598506B (en) * 2016-07-29 2020-07-21 杭州富阳伟文环保科技有限公司 Application of composite nano material
CN106542509A (en) * 2016-10-19 2017-03-29 张家港市东大工业技术研究院 A kind of efficient method for preparing class Graphene carbonitride
CN106542509B (en) * 2016-10-19 2019-01-25 张家港市东大工业技术研究院 A kind of method of efficient preparation class graphene carbonitride
CN113680361A (en) * 2021-08-09 2021-11-23 电子科技大学 Cobalt-ruthenium bimetallic monatomic photocatalyst and preparation method and application thereof

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Application publication date: 20160622