CN110280299A - A kind of flakey g-C3N4Nanometer sheet and preparation method thereof - Google Patents
A kind of flakey g-C3N4Nanometer sheet and preparation method thereof Download PDFInfo
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- CN110280299A CN110280299A CN201910712397.XA CN201910712397A CN110280299A CN 110280299 A CN110280299 A CN 110280299A CN 201910712397 A CN201910712397 A CN 201910712397A CN 110280299 A CN110280299 A CN 110280299A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000004615 ingredient Substances 0.000 claims abstract description 18
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 29
- 238000007146 photocatalysis Methods 0.000 abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 21
- 239000001257 hydrogen Substances 0.000 abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 21
- 150000003839 salts Chemical class 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 5
- 230000006798 recombination Effects 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 description 7
- 230000002776 aggregation Effects 0.000 description 7
- 238000005286 illumination Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Health & Medical Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to nano material and photocatalysis and water-splitting liberation of hydrogen detection technique fields, and in particular to one kind has flakey g-C3N4Nanometer sheet and preparation method thereof, flakey g-C of the invention3N4G-C in nanometer sheet3N4Nanometer sheet is the sclay texture of tiny rule, the g-C3N4Nanometer sheet is having a size of 50~600nm, g-C3N4Nanometer sheet thickness is 5~30nm.Flakey g-C of the invention3N4Nanometer sheet is made by calcining after three kinds of salt and the mixing of nitrogenous Organic Ingredients.G-C of the invention3N4Nanometer sheet, which has, shows unique sclay texture, with higher crystallinity, and it can effectively expand light abstraction width, reduce the recombination probability again of photo-generate electron-hole pair, its photocatalysis activity and water-splitting Hydrogen Evolution Performance are improved, can be effectively applied to photocatalysis water-splitting liberation of hydrogen technical field.
Description
Technical field
The present invention relates to nano materials and photocatalytic water splitting detection technique field, and in particular to a kind of flakey g-C3N4
Nanometer sheet and preparation method thereof.
Background technique
With the intensification of industrialization and urbanization process, tellurian fossil energy gradually moves towards exhausted, at the same time
Serious environmental problem is caused, irreversible destruction is produced to the ecological balance.Therefore it gradually eliminates with non-renewable fossil
The energy is the production method of raw material, seeks a kind of energy-efficient and environmentally friendly energy as being replaced into researcher instantly
One research emphasis.Currently, the favor of photocatalysis and photocatalysis water-splitting liberation of hydrogen technology by many research workers, g-C3N4
Nano material has good development prospect in terms of photocatalysis and photocatalysis water-splitting liberation of hydrogen.This is because its unique stratiform
The advantages that structure, suitable band gap and nontoxicity, makes it become a kind of excellent photochemical catalyst.But g-C3N4Have serious
Agglomeration, the disadvantages of visible absorption is lower and the recombination probability of photo-generate electron-hole pairs is higher greatly limit g-
C3N4Catalyst further applying in terms of photocatalysis and photocatalysis water-splitting liberation of hydrogen.How g-C is reduced3N4Catalyst agglomeration
Phenomenon enhances light absorpting ability and reduces photo-generate electron-hole recombination probability, and then promoting photocatalysis performance is a difficulty
Topic.Before this, have using removing, with the methods of narrow gap semiconductor is compound and monatomic nano particle modify.Wherein adopt
A more popular at present research direction with doping alkaline metal ions, traditional preparation method be mostly one to two kinds of salt with
It is calcined after urea or dicyandiamide mixing, obtains modified photochemical catalyst, but its pattern often easy-regulating and is not still
The promotion of unformed state, photocatalysis performance is also limited.It would therefore be desirable to which a kind of more efficient way prepares shape
Looks are controllable and the more excellent g-C of photocatalysis performance3N4Photochemical catalyst.
Summary of the invention
In view of the above-mentioned problems, the object of the present invention is to provide a kind of flakey g-C3N4Nanometer sheet and preparation method thereof, purport
Obtaining the regulatable g-C of pattern3N4Nanometer sheet enhances light absorpting ability and reduces photo-generate electron-hole recombination probability, with
Improve g-C3N4The photocatalysis performance of nanometer sheet under visible light illumination, and its spectral response range can be widened, it can effectively apply
In photocatalysis technology field.
To achieve the goals above, the technical scheme adopted by the invention is as follows:
A kind of flakey g-C3N4Nanometer sheet, the g-C3N4Nanometer sheet is the sclay texture of tiny rule, described
g-C3N4Nanometer sheet is having a size of 50~600nm, g-C3N4Nanometer sheet thickness is 5~30nm.
A kind of flakey g-C3N4The preparation method of nanometer sheet, comprising the following steps:
(1) nitrogenous Organic Ingredients and mixed inorganic are codissolved in distilled water, stirring is evaporated after 1~10 hour；
(2) mixture after being evaporated is placed in batch-type furnace, heating and thermal insulation prepares the g-C with flakey feature3N4It receives
Rice piece.
Preferably, the nitrogenous Organic Ingredients in step (1) is cyanamide, dicyandiamide, one or more of melamine
Mixture.
Preferably, the mixed inorganic in step (1) is the mixture of BaCl, KCl and NaCl.
Preferably, the mass ratio of BaCl, KCl and NaCl are 1:3:2~5:3:2 in mixed inorganic in step (1).
Preferably, the mass ratio of the nitrogenous Organic Ingredients in step (1) and mixed inorganic is 1:9~9:1.
Preferably, evaporated temperature is 60~90 DEG C in step (1).
Preferably, the heating temperature in step (2) is 560~620 DEG C, and soaking time is 1~4h.
Compared with prior art, the beneficial effects of the present invention are:
Preparation method of the invention is put with other nitrogenous Organic Ingredients compared to other one or two salt and is directly forged together
The preparation method of burning, obtained g-C3N4Nanometer sheet, which has, shows unique sclay texture, has higher crystallinity,
And light abstraction width can be effectively expanded, the recombination probability again of photo-generate electron-hole pair is reduced, improves its photocatalysis activity
And water-splitting Hydrogen Evolution Performance.
Detailed description of the invention
Fig. 1 is the g-C that nitrogenous Organic Ingredients dinectly bruning goes out3N4The g-C prepared with embodiment 1,2 and 33N4Nanometer sheet light
Catalytic hydrogen evolution performance comparison figure.
As can be seen from Figure 1 the g-C by being calcined out after three kinds of salt and the mixing of nitrogenous Organic Ingredients3N4Nanometer sheet photocatalysis
Hydrogen Evolution Performance is significantly promoted.
Fig. 2 is the g-C that nitrogenous Organic Ingredients dinectly bruning goes out3N4The g-C prepared with embodiment 13N4The TEM shape of nanometer sheet
Looks comparison, wherein (i) is nitrogenous Organic Ingredients dinectly bruning g-C3N4Pattern, (ii) are 1 sample topography of embodiment.
Specific embodiment
The present invention is further illustrated with reference to embodiments, it should be noted that is only to present inventive concept
Example and explanation, affiliated those skilled in the art make various modifications to described specific embodiment
Or supplement or be substituted in a similar manner, as long as it does not deviate from the concept of invention or surmount model defined in the claims
It encloses, is regarded as falling into protection scope of the present invention.
Embodiment 1
A kind of flakey g-C3N4The preparation method of nanometer sheet comprising the steps of:
(1) melamine mixes with three kinds of salt by 1:1 mass ratio to (wherein, three kinds of salt are BaCl, KCl and NaCl by matter
Amount ratio mixes for 5:3:2), it is poured into the beaker containing distilled water after mixing, is subsequently agitated for being evaporated (wherein, mixing time 1
~10 hours, preferably 5 hours, evaporated temperature are 60-90 DEG C, preferably 80 DEG C)；
(2) mixture after being evaporated is placed in batch-type furnace, is heated to 565 DEG C, keep the temperature 4h, prepared with flakey spy
The g-C of sign3N4Nanometer sheet.
After tested, the g-C prepared according to above-mentioned steps3N4Nanometer sheet, under visible light illumination, photocatalysis hydrolyze liberation of hydrogen
Rate is 25616 μm of olh-1·g-1, the nitrogenous Organic Ingredients for being about not added with three kinds of salt calcines out the photocatalytic water liberation of hydrogen of coarse powder
34.5 times of performance.
Embodiment 2
The preparation method is the same as that of Example 1 for the present embodiment, the difference is that heating temperature is 580 DEG C in step (2).
The sample that the present embodiment obtains, g-C3N4Nanometer sheet surface is evenly distributed, and without unformed agglomeration, has only
Special microscopic appearance, after tested, the g-C prepared according to above-mentioned steps3N4Nanometer sheet, under visible light illumination, photocatalysis hydrolysis
Liberation of hydrogen rate is 28036 μm of olh-1·g-1, the nitrogenous Organic Ingredients for being about not added with three kinds of salt calcines out the photocatalytic water of coarse powder
37.8 times of Hydrogen Evolution Performance.
Embodiment 3
The preparation method is the same as that of Example 1 for the present embodiment, the difference is that heating temperature is 600 DEG C in step (2).
The sample that the present embodiment obtains, g-C3N4Nanometer sheet surface is evenly distributed, and without unformed agglomeration, has only
Special microscopic appearance, after tested, the g-C prepared according to above-mentioned steps3N4Nanometer sheet, under visible light illumination, photocatalysis hydrolysis
Liberation of hydrogen rate is 25730 μm of olh-1·g-1, the nitrogenous Organic Ingredients for being about not added with three kinds of salt calcines out the photocatalytic water of coarse powder
34.6 times of Hydrogen Evolution Performance.
Embodiment 4
The preparation method is the same as that of Example 1 for the present embodiment, the difference is that heating temperature is 620 DEG C in step (2), soaking time
For 1h.
The sample that the present embodiment obtains, g-C3N4Nanometer sheet surface is evenly distributed, and without unformed agglomeration, has only
Special microscopic appearance, after tested, the g-C prepared according to above-mentioned steps3N4Nanometer sheet, under visible light illumination, photocatalysis hydrolysis
Liberation of hydrogen rate is 23044 μm of olh-1·g-1, the nitrogenous Organic Ingredients for being about not added with three kinds of salt calcines out the photocatalytic water of coarse powder
31.0 times of Hydrogen Evolution Performance.
Embodiment 5
The preparation method of the present embodiment is with embodiment 4, the difference is that soaking time is 1.5h in step (2).
The sample that the present embodiment obtains, g-C3N4Nanometer sheet surface is evenly distributed, and without unformed agglomeration, has only
Special microscopic appearance, after tested, the g-C prepared according to above-mentioned steps3N4Nanometer sheet, under visible light illumination, photocatalysis hydrolysis
Liberation of hydrogen rate is 21211 μm of olh-1·g-1, the nitrogenous Organic Ingredients for being about not added with three kinds of salt calcines out the photocatalytic water of coarse powder
28.5 times of Hydrogen Evolution Performance.
Embodiment 6
The preparation method of the present embodiment is with embodiment 4, the difference is that soaking time is 2h in step (2).
The sample that the present embodiment obtains, g-C3N4Nanometer sheet surface is evenly distributed, and without unformed agglomeration, has only
Special microscopic appearance, after tested, the g-C prepared according to above-mentioned steps3N4Nanometer sheet, under visible light illumination, photocatalysis hydrolysis
Liberation of hydrogen rate is 9433 μm of olh-1·g-1, the nitrogenous Organic Ingredients for being about not added with three kinds of salt calcines out the photocatalytic water of coarse powder
12.7 times of Hydrogen Evolution Performance.
Claims (8)
1. a kind of flakey g-C3N4Nanometer sheet, it is characterised in that: the g-C3N4Nanometer sheet is the flakey knot of tiny rule
Structure, the g-C3N4Nanometer sheet is having a size of 50~600nm, g-C3N4Nanometer sheet thickness is 5~30nm.
2. a kind of flakey g-C as described in claim 13N4The preparation method of nanometer sheet, it is characterised in that: it is specific comprising with
Lower step:
(1) nitrogenous Organic Ingredients and mixed inorganic are codissolved in distilled water, stirring is evaporated after 1~10 hour；
(2) mixture after being evaporated is placed in batch-type furnace, heating and thermal insulation prepares the g-C with flakey feature3N4Nanometer
Piece.
3. a kind of flakey g-C according to claim 23N4The preparation method of nanometer sheet, it is characterised in that: in step (1)
Nitrogenous Organic Ingredients be cyanamide, dicyandiamide, the mixture of one or more of melamine.
4. a kind of flakey g-C according to claim 23N4The preparation method of nanometer sheet, it is characterised in that: in step (1)
Mixed inorganic be BaCl, KCl and NaCl mixture.
5. a kind of flakey g-C according to claim 43N4The preparation method of nanometer sheet, it is characterised in that: in step (1)
The mass ratio of BaCl, KCl and NaCl are 1:3:2~5:3:2 in mixed inorganic.
6. a kind of flakey g-C according to claim 23N4The preparation method of nanometer sheet, it is characterised in that: in step (1)
Nitrogenous Organic Ingredients and mixed inorganic mass ratio be 1:9~9:1.
7. a kind of flakey g-C according to claim 23N4The preparation method of nanometer sheet, it is characterised in that: in step (1)
Evaporated temperature is 60~90 DEG C.
8. a kind of flakey g-C according to claim 23N4The preparation method of nanometer sheet, it is characterised in that: in step (2)
Heating temperature be 560~620 DEG C, soaking time be 1~4h.
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Cited By (3)
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| CN110918115A (en) * | 2019-12-16 | 2020-03-27 | 大连理工大学 | Highly crystalline wrinkles g-C3N4Nanosheet and template-free preparation method thereof |
| CN113318765A (en) * | 2021-05-28 | 2021-08-31 | 江苏大学 | Preparation method and application of ultrathin high-crystallization carbon nitride photocatalyst |
| CN113559911A (en) * | 2021-07-30 | 2021-10-29 | 中国科学院生态环境研究中心 | Monoatomic catalyst, preparation method and application thereof |
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| CN113318765B (en) * | 2021-05-28 | 2023-09-22 | 江苏大学 | Preparation method and application of ultrathin high-crystallization carbon nitride photocatalyst |
| CN113559911A (en) * | 2021-07-30 | 2021-10-29 | 中国科学院生态环境研究中心 | Monoatomic catalyst, preparation method and application thereof |
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