CN110918115A - Highly crystalline wrinkles g-C3N4Nanosheet and template-free preparation method thereof - Google Patents
Highly crystalline wrinkles g-C3N4Nanosheet and template-free preparation method thereof Download PDFInfo
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- 230000037303 wrinkles Effects 0.000 title claims description 7
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- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000011229 interlayer Substances 0.000 claims abstract description 13
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 22
- 239000004202 carbamide Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 7
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 5
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- WZRRRFSJFQTGGB-UHFFFAOYSA-N 1,3,5-triazinane-2,4,6-trithione Chemical compound S=C1NC(=S)NC(=S)N1 WZRRRFSJFQTGGB-UHFFFAOYSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
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- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention provides a high-crystallinity wrinkled g-C3N4 nanosheet, wherein the band gap of the nanosheet is 2.0-3.0 eV, the thickness of the nanosheet is 5-30 nm, the interlayer spacing is 0.310-0.330 nm, and the size of the nanosheet is 80 nm-10 mu m. The invention also provides a template-free preparation method of the high-crystallinity wrinkled g-C3N4 nanosheet, which comprises the steps of pretreating a nitrogen-containing precursor in an air atmosphere; and calcining the pretreated precursor in a nitrogen atmosphere to obtain the high-crystallinity wrinkled g-C3N4 nanosheet. The invention synthesizes the g-C3N4 with high crystallinity and nano flaky structure. The size, interlayer spacing and band gap of the nanosheets can be controlled by changing the temperature, so that the visible light capturing capability of g-C3N4 and the separation efficiency of photon-generated carriers are greatly promoted, and the nanosheets have excellent performance when being applied to a hydrogen production reaction by photolysis of water.
Description
Technical Field
The invention belongs to the technical field of preparation of graphite-phase carbon nitride, and particularly relates to high-crystallinity folded g-C3N4Nanosheets and template-free preparation methods thereof.
Background
Graphite phase carbon nitride (g-C)3N4) As a cheap and easily-obtained non-metal photocatalytic material, the material has the advantages of high nitrogen content, stable physical and chemical properties, visible light response and the like, and is widely applied to reactions such as hydrogen production by photolysis, photocatalytic carbon dioxide reduction, photocatalytic pollutant degradation and the like. However, conventional pyrogenically prepared g-C3N4Is usually thatThe bulk structure has low specific surface area, poor light absorption capability and low carrier separation efficiency, resulting in low photocatalytic performance, which greatly limits the practical application thereof. The specific morphology of the assembled nano-sheets or the g-C of the cross-linked nano-sheets can be obtained by adopting a hard template method, adding easily decomposed salts (ammonium nitrate and the like) and ultrasonic stripping3N4Thereby increasing the specific surface area and remarkably improving the photocatalytic performance. But g-C prepared by these methods3N4The crystallinity of the nano-sheets is poor, and the defects are more, so that the improvement of the photocatalytic efficiency is limited. And the subsequent template removing process is complicated, the preparation cost is increased, and fluorine-containing toxicants can be used to cause environmental pollution. Thus, the synthesis of highly crystalline g-C by the template-free method3N4Nanoplatelets present an important challenge.
Disclosure of Invention
In order to solve the technical problem, the invention provides a high-crystallinity fold g-C3N4Nanosheet and template-free preparation method thereof, and high-crystallinity folded g-C3N4The nano sheet is prepared by pretreating different precursors at different temperatures and then calcining at high temperature. The technical scheme is as follows:
high-crystallinity fold g-C3N4The band gap of the nano-sheet is 2.0-3.0 eV; the thickness of the nanosheet is 5-30 nm, and the thickness can be adjusted; the interlayer spacing of the nano-sheets is 0.310-0.330 nm, and the interlayer spacing can be adjusted; the size of the nanosheet is 80 nm-10 mu m, and the size can be adjusted.
The invention also provides the high-crystallinity fold g-C3N4The template-free preparation method of the nanosheet comprises the following steps:
A. pretreating the nitrogen-containing precursor for 1-5 h at the temperature of 100-600 ℃ in the air atmosphere, wherein the heating rate is 1-10 ℃/min;
in a preferable mode, the nitrogen-containing precursor is one or a combination of more of urea, cyanamide, dicyandiamide, thiourea, trithiocyanuric acid or melamine;
B. calcining the precursor pretreated in the step A at the temperature of 700 ℃ under the nitrogen atmosphere0.5-10 h to obtain high-crystallinity folds g-C3N4Nanosheets.
The calcining atmosphere in the step B is nitrogen atmosphere, which is beneficial to improving g-C3N4Crystallinity and reduced defects.
The invention adopts a method of high-temperature pyrolysis of different precursors to synthesize g-C under the condition of no template3N4. Calcining at 500 deg.C to obtain g-C3N4The morphology of (A) tends to wrinkle the nanosheets, and increasing the temperature can significantly reduce the nanosheet size and interlayer spacing and improve its crystallinity.
And (3) further optimizing, wherein the nitrogen-containing precursor in the step A is one or a combination of urea, dicyandiamide and cyanamide.
The pre-treatment temperature in the step A is preferably 400-500 ℃, which is favorable for increasing the g-C3N4And (4) yield.
The pretreatment time in the step A is preferably 2 to 3 hours.
The calcination temperature in the step B is preferably 550-690 ℃, which is beneficial to preparing large-size and high-crystallinity folded g-C3N4Nanosheets.
The calcination time in step B is preferably 2 to 6 hours.
All conditions in this application that relate to a numerical range can be independently selected from any point within the numerical range.
The beneficial effects of the invention compared with the prior art comprise:
the present invention is directed to g-C3N4The problem of serious reduction of crystallinity of the nano-sheet can be caused in the preparation process of the nano-sheet, and g-C with high crystallinity and a nano flaky structure is synthesized under the conditions of inert atmosphere and high temperature by optimizing a precursor3N4. The size and interlayer spacing of the nanosheets can be controlled by varying the temperature. By controlling the proper calcining temperature, the high-crystallinity g-C with larger size and smaller interlayer spacing can be synthesized3N4Nanosheets having a highly extended conjugated pi-electron system with a band gap of 2.0-3.0 eV, pi → pi*And n → pi*The transition is easy to occur, and the g-C is greatly promoted3N4Visible light capturing ability and photogenerated carrier separation efficiency. The material has excellent performance when being applied to the reaction of hydrogen production by photolysis of water.
Drawings
FIG. 1 shows g-C of comparative example 13N4Scanning electron micrographs (A) and transmission electron micrographs (B).
FIG. 2 shows g-C of examples 1 to 4 of the present invention3N4Scanning electron microscopy (scale 1 μm), wherein A is example 1; b is example 2; c is example 3; d is example 4.
FIG. 3 shows g-C of examples 1 to 4 of the present invention3N4Transmission electron micrograph (scale 500 nm) where a is example 1; b is example 2; c is example 3; d is example 4.
FIG. 4 shows g-C of comparative example 1 and examples 1 to 43N4XRD pattern, where a is comparative example 1; b is example 1; c is example 2; d is example 3; e is example 4.
FIG. 5 shows g-C of example 5 of the present invention3N4Transmission electron micrographs.
FIG. 6 is g-C for comparative example 1 and example 43N4A performance diagram for hydrogen production by photolysis of water, wherein A is comparative example 1; b is example 4.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples. The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
Comparative example 1
g-C3N4The conventional synthesis method comprises the following steps:
A. heating the urea precursor to 550 ℃ in air atmosphere and calcining to obtain the g-C with thicker layered structure3N4。
In the step A, the dosage of the urea is 20 g, the heating rate is 3 ℃/min, and the calcination time at 550 ℃ is 3 h. The synthesized sample obtained by scanning electron microscope and transmission electron microscope has a thicker lamellar structure (as shown in FIG. 1A), and the XRD spectrum shows that the sample has standard g-C3N4Characteristic diffraction peak, whose interlayer spacing is 0.3241 nm according to Bragg equation (as shown in the sample of FIG. 4A).
Example 1
High-crystallinity fold g-C3N4The synthesis method of the nanosheet comprises the following steps:
a, heating a urea precursor to 400 ℃ in an air atmosphere, and calcining to obtain a pretreated precursor;
B. heating the pretreated precursor to 600 ℃ in a nitrogen atmosphere for calcining to obtain high-crystallinity folded g-C3N4Nanosheets.
In the step A, the using amount of urea is 20 g, the heating rate is 3 ℃/min, and the calcining time at 400 ℃ is 3 h; in the step B, the calcination time of the precursor at 600 ℃ is 2 h.
The sample synthesized by a scanning electron microscope and a transmission electron microscope is of a folded nanosheet structure, the size of the nanosheet is 2-10 microns, the thickness of the nanosheet is reduced to 10-30 nm (as shown in the samples in figures 2A and 3A), and the XRD (X-ray diffraction) spectrum shows that the diffraction peak of the sample is enhanced, the crystallinity of the sample is improved, the diffraction peak shifts to a high angle, and the interlayer spacing of the sample is reduced (as shown in the sample in figure 4B).
Example 2
Example 1 was repeated, but the calcination temperature in step B was 630 ℃.
g-C obtained with increasing temperature3N4The surface of the nano sheet becomes smooth, and the wrinkles become more. The size of the nano-sheet is 2-10 μm, the thickness is reduced to 10-25 nm (as shown in the samples in figures 2B and 3B), and the diffraction peak of the sample is strengthened and the crystallinity is improved, the diffraction peak shifts to a high angle and the interlayer spacing is reduced (as shown in the sample in figure 4C) according to an XRD (X-ray diffraction) pattern.
Example 3
Example 1 was repeated, but the calcination temperature in step B was 640 ℃.
g-C obtained with increasing temperature3N4The surface of the nano sheet becomes smooth, and the wrinkles become more. The nanometer sheet has size of 2-10 μm and thickness of 5-20 nm (shown in figure 2C and 3C), and the XRD pattern shows that the sample has strong diffraction peak and good crystallinityThe diffraction peak is shifted toward high angles and the interlayer spacing becomes smaller (as shown in the sample of fig. 4D).
Example 4
Example 1 was repeated, but the calcination temperature in step B was 650 ℃.
g-C obtained with increasing temperature3N4The surface of the nano sheet becomes smooth, and the wrinkles become more. The size of the nano-sheet is 2-10 μm, the thickness is reduced to 5-20 nm (as shown in the samples in figures 2D and 3D), and the diffraction peak of the sample becomes strong and good in crystallinity, shifts to a high angle and becomes small in interlayer spacing (as shown in the sample in figure 4E) according to an XRD (X-ray diffraction) pattern.
Example 5
Example 1 was repeated, but in step a the urea precursor was replaced by a mixed precursor of urea and dicyandiamide, and in step B the calcination temperature was 650 ℃.
High-crystallinity folded g-C still can be prepared after two mixed nitrogen-containing precursors are used for replacing urea3N4Nanoplatelets as shown in figure 5.
Example 6
The performance of the sample A prepared in the comparative example 1 and the sample B prepared in the example 4 for hydrogen production by water photolysis is compared, and the specific catalytic performance test comprises the following steps:
the A photocatalytic water decomposition hydrogen production is carried out in an 84 mL quartz glass reactor customized in a laboratory, the dosage of a sample A or B is 10 mg, the aqueous solution is 30 mL, the triethanolamine is 3 mL, the Pt loading capacity is 3 wt%, before reaction, ultrasonic treatment is carried out for 10 min, then nitrogen is introduced for evacuation for 30 min, then the reactor is vacuumized for 5 min, and a light source is turned on for reaction. After 5.5 hours of reaction, the whole reaction system is balanced with the atmospheric pressure by using argon, and after the gases in the reaction system are fully and uniformly mixed, 0.5 mL of gas is taken for chromatographic analysis, and the hydrogen yield is tested. As shown in FIG. 6, the hydrogen production rate of the sample A prepared in the comparative example 1 is only 1062 μmol/g/h, while the hydrogen production rate of the sample prepared in the example 4 of the present invention is 5120 μmol/g/h, which is about 5 times of that of the sample A.
Therefore, the g-C prepared by the invention has high crystallinity and a nano sheet structure3N4The catalyst can show excellent performance in the hydrogen production reaction by photolysis of waterThe performance of (c).
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (8)
1. High-crystallinity fold g-C3N4The nanosheet is characterized in that the band gap of the nanosheet is 2.0-3.0 eV, the thickness of the nanosheet is 5-30 nm, the interlayer spacing is 0.310-0.330 nm, and the size of the nanosheet is 80 nm-10 mu m.
2. The highly-crystallized wrinkles g-C of claim 13N4The template-free preparation method of the nanosheet is characterized by comprising the following steps:
A. pretreating the nitrogen-containing precursor for 1-5 h at the temperature of 100-600 ℃ in the air atmosphere, wherein the heating rate is 1-10 ℃/min;
B. calcining the precursor pretreated in the step A for 0.5-10 h at the temperature of 500-700 ℃ in the nitrogen atmosphere to obtain the high-crystallinity fold g-C3N4Nanosheets.
3. The highly-crystallized wrinkled g-C of claim 23N4The template-free preparation method of the nanosheet is characterized in that the nitrogen-containing precursor in the step A is one or a combination of urea, cyanamide, dicyandiamide, thiourea, trithiocyanuric acid and melamine.
4. The highly-crystallized wrinkled g-C of claim 33N4The template-free preparation method of the nanosheet is characterized in that in the step A, the nitrogen-containing precursor is one or a combination of urea, dicyandiamide and cyanamide.
5. The height of claim 2Crystalline pleating g-C3N4The template-free preparation method of the nano-sheet is characterized in that the pretreatment temperature in the step A is 400-500 ℃.
6. The highly-crystallized wrinkled g-C of claim 23N4The template-free preparation method of the nanosheet is characterized in that the pretreatment time in the step A is 2-3 h.
7. The highly-crystallized wrinkled g-C of claim 23N4The template-free preparation method of the nano-sheet is characterized in that the calcination temperature in the step B is 550-690 ℃.
8. The highly-crystallized wrinkled g-C of claim 23N4The template-free preparation method of the nanosheets is characterized in that the calcination time in the step B is 2-6 h.
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| CN110280299A (en) * | 2019-08-02 | 2019-09-27 | 合肥工业大学 | A kind of flakey g-C3N4Nanometer sheet and preparation method thereof |
| CN110420656A (en) * | 2019-08-13 | 2019-11-08 | 合肥工业大学 | A kind of gas phase acidification g-C3N4 nanometer sheet and preparation method thereof |
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| CN106563481A (en) * | 2016-10-08 | 2017-04-19 | 武汉理工大学 | Ammoniated ultrathin graphite-phase carbonitride photocatalyst and preparation method thereof |
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| CN109908937A (en) * | 2019-03-25 | 2019-06-21 | 黄河三角洲京博化工研究院有限公司 | A kind of preparation method of nanoscale visible light catalyst |
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