CN107876074B - g-C3N4Preparation method of nanoparticle/flower-shaped BiOI composite material - Google Patents
g-C3N4Preparation method of nanoparticle/flower-shaped BiOI composite material Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000002057 nanoflower Substances 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 230000010355 oscillation Effects 0.000 claims abstract description 4
- 238000010992 reflux Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000006185 dispersion 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
- 238000000643 oven drying Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 239000004065 semiconductor Substances 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 6
- 230000031700 light absorption Effects 0.000 abstract description 3
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000000969 carrier Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 238000000707 layer-by-layer assembly Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013501 sustainable material Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
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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
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention relates to the field of semiconductor materials, and aims to provide g-C3N4A method for preparing a nano-particle/flower-shaped BiOI composite material. The method comprises the following steps: after the nitrogen-rich precursor powder is subjected to heat treatment, grinding to obtain powdery g-C3N4(ii) a Dispersing in strong acid solution, condensing, refluxing, washing until the product is neutral to obtain g-C3N4A nanoparticle; adding Bi (NO)3)3·5H2Adding O and KI into a mixed solution of deionized water and ethylene glycol, stirring and dissolving, then carrying out hydrothermal reaction, washing the obtained precipitate, and drying to obtain flower-shaped BiOI; mixing flower-shaped BiOI with g-C3N4Dispersing the nano particles in deionized water, and stirring after ultrasonic oscillation; and (4) after centrifugation, cleaning and drying the precipitate to obtain a final product. The preparation method is simple and easy to operate. Can prepare g-C with uniform load3N4The nano-particle/flower-shaped BiOI composite material has high photogeneration carrier separation efficiency and high visible light absorption capacity and is g-C3N4The research of the base nano composite material provides a new idea.
Description
Technical Field
The invention relates to the field of semiconductor materials, in particular to g-C3N4A method for preparing a nano-particle/flower-shaped BiOI composite material.
Background
In recent years, semiconductor photocatalytic materials have attracted extensive attention as a novel green, environmentally-friendly and sustainable material which has great application prospects and research values in the aspects of water pollutant treatment, hydrogen energy preparation, greenhouse effect gas and organic pollutant gas removal. However, a single semiconductor has a problem of low separation efficiency of photogenerated carriers, so that the semiconductor heterojunction composite material is rapidly a hot spot in the research field. The two semiconductor composite materials realize the high-efficiency separation of photogenerated electron-hole pairs through the transfer of photogenerated electrons and holes between different semiconductor energy bands. Recently, a wide range of photocatalytic materials of the BiOX (X ═ Cl, Br, I) series have been studied. Among them, the BiOI is a very promising photocatalyst due to its narrow forbidden band width (-1.8 eV), high visible light absorption capability, proper energy band position, good stability and 2D layered structure. However, the problem of low separation efficiency of the photogenerated carriers also exists in the BiOI, so that the improvement of the separation efficiency of the photogenerated carriers by compounding the BiOI with other semiconductor materials is a research hotspot in the research field.
Graphite-like carbon nitride (g-C)3N4) The material is more and more widely concerned as a novel visible light catalytic material. g-C3N4Has a forbidden band width of 2.7eV, and has catalytic activity in a visible light region. Furthermore g-C3N4Consists of two chemical elements C and N which are most abundant on the earth, and has no toxicity and low preparation cost. Thus, g-C3N4Has bright application prospect in the field of photocatalysis due to the characteristics of excellent semiconductor characteristics, high chemical stability, no toxicity, easy preparation and low cost. The two are compounded by researchers to obtain g-C3N4a/BiOI composite material; researchers also prepare micron spherical BiOI assembled by BiOI nanosheets and g-C by an ionic liquid method3N4Compounding to greatly improve the capability of degrading methylene blue by photocatalysis; researchers also prepared BiOI micron tablets by a hydrothermal method and combined with blocky g-C3N4The specific surface area of the composite material is greatly improved by compounding, and the performance of degrading organic pollutants by visible light catalysis is also improved. However, the combination of the two still has the problem of uneven combination on the microstructure. It can be seen that it is necessary to work with g-C3N4The structure of the/BiOI composite material is adjusted to further improve the composite uniformity.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides g-C3N4A method for preparing a nano-particle/flower-shaped BiOI composite material.
In order to solve the problems, the solution of the invention is as follows:
providing a compound of g-C3N4The preparation method of the nanoparticle/flower-shaped BiOI composite material comprises the following steps:
step A: at least one of cyanamide, dicyandiamide or melamine is taken as a nitrogen-rich precursor, and powder of the nitrogen-rich precursor is poured into a corundum crucible boat and then placed into a vacuum tube furnace; introducing protective atmosphere to exhaust air in the vacuum tube furnace, and performing heat treatment to obtain blocky g-C3N4Further grinding to obtain powder g-C3N4；
And B: the obtained powder g-C3N4Dispersed in a strong acid solution, g-C3N4The mass ratio of the acid solution to the strong acid solution is 1: 50-1: 200; the strong acid solution is prepared from concentrated sulfuric acid and concentrated nitric acid with the mass ratio of 1: 1-1: 3, and the mass fractions of the concentrated sulfuric acid and the concentrated nitric acid are respectively 98% and 68%; condensing and refluxing the mixed solution obtained by dispersion at the temperature of 60-80 ℃ for 2-10 h, and repeatedly cleaning the product with deionized water until the product is neutral to obtain g-C3N4A nanoparticle;
and C: adding Bi (NO)3)3·5H2O and KI are added into the mixture, and the mixture is prepared from deionized water and ethylene glycol according to the mass ratio of 1: 1-1: 5In the mixed solution, the mass percentage concentration of KI is 1-5%, and the molar ratio of Bi element to I element is 1: 1; stirring and dissolving, and transferring to a reaction kettle for hydrothermal reaction at 130-180 ℃ for 12-24 h; centrifugally washing the obtained precipitate twice with deionized water, centrifugally washing twice with absolute ethyl alcohol, and drying in a drying oven at 60 ℃ to obtain flower-shaped BiOI;
step D: b, mixing the flower-shaped BiOI with the g-C obtained in the step B3N4Nanoparticles dispersed in deionized water, g-C3N4The mass ratio of the flower-shaped BiOI to the flower-shaped BiOI is 1: 10-1: 200; stirring for 12-24 hours after ultrasonic oscillation for 0.5-2 hours; centrifuging, washing the precipitate with anhydrous ethanol for three times, and oven drying at 60 deg.C to obtain g-C3N4Nanoparticle/flower-like BiOI composite materials.
In the step A, the heat treatment temperature is 500-600 ℃, and the heat treatment time is 2-10 hours.
In the invention, in the step A, the protective atmosphere of the tube furnace is argon or nitrogen.
The realization principle of the invention is as follows:
according to the invention, the flower-shaped BiOI material (which is composed of BiOI nanosheets with the thickness of 30-50 nm and the size of micron level) is prepared, and the BiOI material with a large surface area is obtained and is g-C with the size of about 30nm3N4The attachment of the nanoparticles provides the conditions. In addition, the surface of the BiOI in water is negatively charged, g-C3N4The surface of the nano particles is positively charged, so that the electrostatic self-assembly of the nano particles and the nano particles is realized.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method is simple and easy to operate.
2. The invention prepares uniformly loaded g-C3N4The nano-particle/flower-shaped BiOI composite material has high photogeneration carrier separation efficiency and high visible light absorption capacity and is g-C3N4The research of the base nano composite material provides a new idea.
Drawings
FIG. 1 shows g-C3N4Scanning electron microscope (apparent morphology picture) of the nano-particle/flower-like BiOI composite material.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments below:
g-C3N4the preparation method of the nanoparticle/flower-shaped BiOI composite material comprises the following steps:
step A: at least one of cyanamide, dicyandiamide or melamine is taken as a nitrogen-rich precursor, and powder of the nitrogen-rich precursor is poured into a corundum crucible boat and then placed into a vacuum tube furnace; introducing protective atmosphere to exhaust air in the vacuum tube furnace, and performing heat treatment to obtain blocky g-C3N4Further grinding to obtain powder g-C3N4；
And B: the obtained powder g-C3N4Dispersed in a strong acid solution, g-C3N4The mass ratio of the acid solution to the strong acid solution is 1: 50-1: 200; the strong acid solution is prepared from concentrated sulfuric acid and concentrated nitric acid with the mass ratio of 1: 1-1: 3, and the mass fractions of the concentrated sulfuric acid and the concentrated nitric acid are respectively 98% and 68%; condensing and refluxing the mixed solution obtained by dispersion at the temperature of 60-80 ℃ for 2-10 h, and repeatedly cleaning the product with deionized water until the product is neutral to obtain g-C3N4A nanoparticle;
and C: adding Bi (NO)3)3·5H2Adding O and KI into a mixed solution prepared from deionized water and ethylene glycol according to the mass ratio of 1: 1-1: 5, wherein the mass percentage concentration of KI is 1-5%, and the molar ratio of Bi element to I element is 1: 1; stirring and dissolving, and transferring to a reaction kettle for hydrothermal reaction at 130-180 ℃ for 12-24 h; centrifugally washing the obtained precipitate twice with deionized water, centrifugally washing twice with absolute ethyl alcohol, and drying in a drying oven at 60 ℃ to obtain flower-shaped BiOI;
step D: b, mixing the flower-shaped BiOI with the g-C obtained in the step B3N4Nanoparticles dispersed in deionized water, g-C3N4The mass ratio of the active carbon to the flower-shaped BiOI is 1: 10-1: 200; stirring for 12-24 hours after ultrasonic oscillation for 0.5-2 hours; centrifuging, washing the precipitate with anhydrous ethanol for three times, and oven drying at 60 deg.C to obtain g-C3N4Nanoparticle/flower-like BiOI composite materials.
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way. g-C was successfully prepared by 8 examples each3N4The experimental data for the nanoparticles/flower-like BiOI composite materials for each example are shown in Table 1 below.
Table 1 data table of examples
Finally, it should also be noted that the above list is only a specific implementation example of the present invention. It is obvious that the invention is not limited to the above embodiment examples, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (2)
1. g-C3N4The preparation method of the nano-particle/flower-shaped BiOI composite material is characterized by comprising the following steps of:
step A: at least one of cyanamide, dicyandiamide or melamine is taken as a nitrogen-rich precursor, and powder of the nitrogen-rich precursor is poured into a corundum crucible boat and then placed into a vacuum tube furnace; introducing protective atmosphere to exhaust air in the vacuum tube furnace, and performing heat treatment to obtain blocky g-C3N4Further grinding to obtain powder g-C3N4(ii) a The heat treatment temperature is 500-600 ℃, and the heat treatment time is 2-10 h;
and B: the obtained powder g-C3N4Dispersed in a strong acid solution, g-C3N4The mass ratio of the acid solution to the strong acid solution is 1: 50-1: 200; the strong acid solution is prepared from concentrated sulfuric acid and concentrated nitric acid with the mass ratio of 1: 1-1: 3, and the mass fractions of the concentrated sulfuric acid and the concentrated nitric acid are respectively 98% and 68%; condensing and refluxing the mixed solution obtained by dispersion at the temperature of 60-80 ℃ for 2-10 h, and repeatedly cleaning the product with deionized water until the product is neutral to obtain g-C3N4A nanoparticle;
and C: adding Bi (NO)3)3•5H2Adding O and KI into a mixed solution prepared from deionized water and ethylene glycol according to the mass ratio of 1: 1-1: 5, wherein the mass percentage concentration of KI is 1-5%, and the molar ratio of Bi element to I element is 1: 1; stirring and dissolving, and transferring to a reaction kettle for hydrothermal reaction at 130-180 ℃ for 12-24 h; centrifugally washing the obtained precipitate twice with deionized water, centrifugally washing twice with absolute ethyl alcohol, and drying in a drying oven at 60 ℃ to obtain flower-shaped BiOI;
step D: b, mixing the flower-shaped BiOI with the g-C obtained in the step B3N4Nanoparticles dispersed in deionized water, g-C3N4The mass ratio of the flower-shaped BiOI to the flower-shaped BiOI is 1: 10-1: 200; stirring for 12-24 hours after ultrasonic oscillation for 0.5-2 hours; centrifuging, washing the precipitate with anhydrous ethanol for three times, and oven drying at 60 deg.C to obtain g-C3N4Nanoparticle/flower-like BiOI composite materials.
2. The method according to claim 1, wherein in step A, the protective atmosphere of the tube furnace is argon or nitrogen.
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| CN109395777B (en) * | 2018-04-12 | 2020-03-20 | 常州大学 | Ternary composite photocatalyst BiOI @ UIO-66 (NH)2)@g-C3N4Preparation method of (1) |
| CN109847780A (en) * | 2019-01-30 | 2019-06-07 | 太原理工大学 | A kind of AgBr/BiOI/g-C3N4The preparation method and applications of tri compound catalysis material |
| CN110075923A (en) * | 2019-04-30 | 2019-08-02 | 江苏大学 | A kind of g-C3N4The bionical construction method and application thereof of/BiOI-pDA@PVDF photocatalysis membrana |
| CN114160172A (en) * | 2021-12-16 | 2022-03-11 | 中国船舶重工集团公司第七一九研究所 | For CO2Cu/BiOI catalyst for preparing methanol by catalytic hydrogenation and preparation method thereof |
| CN114522709B (en) * | 2022-01-14 | 2023-10-31 | 广东工业大学 | Three-dimensional porous graphite phase carbon nitride/bismuth oxyiodide/silver nanoparticle composite photocatalyst and preparation method and application thereof |
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