CN107651704B - Cadmium sulfide nanoflower with hierarchical structure constructed by exposed (001) crystal face ultrathin nano-sheets and preparation method thereof - Google Patents
Cadmium sulfide nanoflower with hierarchical structure constructed by exposed (001) crystal face ultrathin nano-sheets and preparation method thereof Download PDFInfo
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- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 71
- 239000002057 nanoflower Substances 0.000 title claims abstract description 44
- 239000013078 crystal Substances 0.000 title claims abstract description 41
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002135 nanosheet Substances 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 150000001661 cadmium Chemical class 0.000 claims abstract description 11
- 238000004729 solvothermal method Methods 0.000 claims abstract description 10
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 11
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Chemical compound [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 230000009467 reduction Effects 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 239000012153 distilled water Substances 0.000 abstract 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
-
- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- B01J35/615—
-
- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
Abstract
The invention discloses a cadmium sulfide nanoflower with a hierarchical structure constructed by exposed (001) crystal face ultrathin nanosheets and a preparation method thereof. The cadmium sulfide nanoflower with the hierarchical structure consists of ultrathin cadmium sulfide nano-pages with the thickness of about 2-4nm and exposed (001) crystal faces, the diameter of the ultrathin cadmium sulfide nano-pages is 300-1 um, and the specific surface area of the ultrathin cadmium sulfide nano-pages is up to 107m2(ii) in terms of/g. The preparation method comprises the following steps: uniformly mixing inorganic cadmium salt, deionized water, diethylenetriamine and sulfur powder, carrying out solvothermal reaction at the reaction temperature of 70-90 ℃, washing the reaction solution with distilled water and absolute ethyl alcohol in sequence, and drying to obtain the cadmium sulfide nanoflower with the hierarchical structure. The cadmium sulfide nanoflower with the hierarchical structure has excellent photocatalytic reduction of CO2The catalytic activity, the CO yield under visible light is 1.558umol/g/h, which is about 2 times of that of the nano-particles, and the operation process is simple and the energy consumption is low.
Description
Technical Field
The invention belongs to the field of photocatalytic nano materials, and particularly relates to a cadmium sulfide nano flower with a hierarchical structure constructed by exposed (001) crystal face ultrathin nano sheets and a preparation method thereof.
Background
The physical and chemical properties of the nano material are greatly dependent on the morphology and size of the material, so the research of different morphology structures becomes the leading-edge field of the present nano science and technology. CdS is an important direct band gap semiconductor material, has unique optical, electrical and catalytic properties, and has wide application in the fields of laser, light-emitting diode solar cells and catalysis. Therefore, the preparation, physical and chemical properties and application research of the CdS nano structures with different shapes have very important scientific significance.
At present, common CdS morphologies mainly include nanorods, nanotubes, nanosheets and the like. With the continuous and intensive research, the structures of the nano materials are increasingly diversified, and people find that a complex hierarchical nano structure with a special appearance and structure, which is obtained by self-assembly by taking a low-dimension as a building unit, has better physical or chemical properties, such as large specific surface area, difficult agglomeration and the like. The hydrothermal method and the solvothermal method are preferred methods for preparing the nano material due to the advantages of simple operation, high product yield, low investment and the like. Most of the current complex CdS hierarchical structures are synthesized by using the method. For example, Chen et al, using cadmium nitrate as a cadmium source, thiourea as a sulfur source, hexamethylenetetramine as a complexing agent, prepare a three-dimensional CdS nanoflower structure (Chen F, Zhou R, Yang L, et al, Large-scale and shape-controlled CdS nano crystals with flow lattice structure [ J ] in a 200 ℃ reaction temperature hydrothermal system]The Journal of Physical Chemistry C,2008,112(4): 1001-1007.). Jin et al uses CdCl2And thiourea as raw material, polyvinylpyrrolidone (PVP) as complexing agent, and preparing flower-like CdS (Jin R, Su M, Wang J, et al. Synthesis and enhanced hydrothermal activity of monocrystalline CdS nanofilled from CdS nanofilles with exposed {001} faces [ J]Materials research bulletin,2012,47(11): 3070-. Wang et al uses ethylenediamine as the moleculeTemplate in CdCl2-EDTA -H2Adding thioacetamide and ethylenediamine into the O solution, and carrying out hydrothermal 180-degree reaction to prepare CdS nanorod (diameter is 30nm and length is 100nm) assembled microspheres (Wang Z, Pan L, Wang L, et al, Urchin-like CdS microspheres-assembled from CdS nanoparticles and the same photocatalytic properties [ J]SolidState Sciences,2011,13(5):970- & 975.). CdCl adopted by Chen et al2-thiourea-dimethylformamide-H2In the O system, by changing the amount of Dimethylformamide (DMF), a hierarchical structure of nanometer twigs, flowers and polygons (Chen M, Kim Y N, Li C, et al. controlled synthesis of hyperbranched metals/nanocrystals [ J]Crystal Growth and Design,2008,8(2): 629-634.). The preparation methods have the advantages that the reaction temperature is over 150 ℃, the energy consumption is high, and the thickness of the monomer with the hierarchical structure is over 50nm generally. The thicker monomer thickness will result in a smaller specific surface area and fewer reactive sites, thereby affecting the catalytic activity thereof. Therefore, how to prepare the CdS with the hierarchical structure, which has the advantages of thin monomer thickness and high photocatalytic activity, at low temperature is of great significance.
Disclosure of Invention
The invention aims to provide a cadmium sulfide nanometer flower with a hierarchical structure constructed by mainly exposing (001) high-energy crystal face nanometer pages and a preparation method thereof.
The technical scheme of the invention is as follows: the cadmium sulfide nanoflower with the hierarchical structure is constructed by exposing (001) crystal face ultrathin nano pages, and the cadmium sulfide nanoflower with the hierarchical structure is composed of the exposing (001) crystal face ultrathin cadmium sulfide nano pages with the thickness of 2-4 nm.
The crystal form of the cadmium sulfide is wurtzite, and the diameter of the cadmium sulfide nanoflower with the hierarchical structure is 0.3-1 um.
A preparation method of a hierarchical cadmium sulfide nanoflower constructed by exposing (001) crystal face ultrathin nano-pages comprises the following preparation processes:
a) uniformly mixing inorganic cadmium salt, deionized water, diethylenetriamine and sulfur powder;
b) carrying out solvothermal reaction, washing and drying to obtain the cadmium sulfide nanoflower with the hierarchical structure constructed by the exposed (001) crystal face ultrathin nano-sheets.
The mass ratio of the sulfur powder to the inorganic cadmium salt is 4-8: 1, the ratio of the amount of deionized water to the amount of inorganic cadmium salt is 0.3-0.7: 1, and the ratio of diethylenetriamine to the amount of inorganic cadmium salt is 200-500: 1.
The inorganic cadmium salt is Cd (NO)3)2、CdCl2、Cd(CH3COO)2、Cd(NO3)2·4H2O、 CdCl2·2.5H2O or Cd (CH)3COO)2·2H2Any one or a mixture of two or more of O.
The solvothermal reaction temperature is 60-100 ℃, and the reaction time is 24-72 h.
The invention has the following technical effects: 1. the CdS nanoflower with the hierarchical structure prepared by the invention is constructed by ultrathin nanosheets with exposed (001) high-energy crystal faces with the thickness of 2-4nm, the diameter of the CdS nanoflower is about 300nm-1 um, and the CdS nanoflower has a specific surface area (107 m)2The per gram) is high, not only can the adsorption to the reaction substrate be increased, but also more reaction active sites can be provided. 2. The CdS nanoflower with the hierarchical structure prepared by the method is composed of ultrathin nano-pages which are very thin and expose (001) high-energy crystal faces. The thickness of the nanometer page is very thin, so that the distance from a photon-generated carrier to the surface of the photocatalytic material is greatly shortened, and the bulk phase recombination of a photon-generated electron hole pair is effectively inhibited; exposing the (001) high energy crystal plane can enhance the transfer of photo-generated charges. Both of these reasons contribute to the improvement of photocatalytic activity. Under the condition of irradiation of visible light with the wavelength of more than 400nm and without loading any cocatalyst, the CdS nanoflower photocatalytic reduction CO2CO was formed in a yield of 1.558umolg-1h-1Compared with the CdS nano particle CO generation rate under the same condition, the catalyst improves the generation rate by 100 percent, and shows excellent CO photocatalytic reduction2And (4) activity. 3. The preparation method greatly reduces the reaction temperature for preparing similar catalysts and reduces the production energy consumption. In addition, the method has simple operation process and good product repeatability.
Drawings
Fig. 1 is an XRD pattern of a CdS nanoflower with a hierarchical structure constructed by exposing (001) crystal face ultrathin nano-pages prepared in example 1 and a wurtzite CdS semiconductor standard PDF card (41-1049).
Fig. 2 is a Transmission Electron Microscope (TEM) image of a CdS nanoflower with a hierarchical structure constructed by the exposed (001) crystal plane ultrathin nanowhiskers prepared in example 1.
Fig. 3 is a Transmission Electron Microscope (TEM) image of a CdS nanoflower with a hierarchical structure constructed by the exposed (001) crystal plane ultrathin nanowhisker prepared in example 2.
Fig. 4 is a Fast Fourier Transform (FFT) and an inverse fourier transform diagram of a CdS nanoflower with a hierarchical structure constructed for an exposed (001) crystal plane ultrathin nanoweb prepared in example 2.
Fig. 5 is a nitrogen isothermal adsorption and desorption graph of the CdS nanoflower with the hierarchical structure constructed by the exposed (001) crystal face ultrathin nano-page prepared in example 1.
FIG. 6 shows CdS nanoflowers with hierarchical structures constructed by (001) crystal face exposed ultrathin nano-pages prepared in example 1 and CdS nanoparticles prepared in comparative example for photocatalytic reduction of CO2A graph of CO time dependence was generated and fig. 7 is a histogram of the corresponding CO generation rate.
Detailed Description
The technical solution of the invention is further described by the following specific examples.
Example 1
40mmol of S powder and 10.0mmol of Cd (NO)3)2·4H2O, 3mmol of deionized water and 1000.0mmol of diethylenetriamine are fully stirred and uniformly dispersed, and then the mixture is placed in a 120ml polytetrafluoroethylene reaction kettle to be subjected to solvothermal reaction for 72 hours at the reaction temperature of 70 ℃. And naturally cooling to room temperature, and respectively centrifugally washing with ethanol and deionized water to collect solvothermal products to obtain the cadmium sulfide nanoflower with the hierarchical structure constructed by the exposed (001) crystal face ultrathin nano-pages. The thickness of the CdS nanoflower petal slice is about 2nm measured by an atomic force microscope, and the diameter of the CdS nanoflower is about 0.5-1 um measured by a transmission electron microscope.
As shown in FIG. 1, the intensity of the (002) and (101) crystal plane diffraction peaks of the CdS semiconductor standard PDF card is not greatly different, but the intensity of the (001) crystal plane diffraction peak of the CdS nanobelt prepared by the method is far higher than that of the (101) crystal plane, which indicates that the CdS nanoflowers can preferentially expose the (001) crystal plane.
As shown in FIG. 2, the diameter of the prepared nanoflower is about 0.5-1 um.
As shown in fig. 3, the prepared nanoflower is assembled by nanosheets having a thickness of about 2 nm.
As shown in FIG. 4, the lattice stripes of 0.36nm can be respectively assigned to the (100), (010) and (110) crystal planes, and the included angles of the crystal planes are all about 120 degrees, which shows that the CdS nanoflower preferentially exposes the (001) crystal plane.
As shown in FIG. 5, the specific surface area was calculated to be 107.1m according to the BET formula2/g。
As shown in FIGS. 6 and 7, the amount of the catalyst used was 50mg, and CO was reduced by photocatalysis in a gas-solid system2The rate of CO generation is 1.29umol/g/h, which is about 2 times of CdS nano-particles.
Example 2:
16mmol of S powder and 2mmol of CdCl2·2.5H2O, 1.4mmol of deionized water and 1000.0mmol of diethylenetriamine are fully stirred and uniformly dispersed, and then the mixture is placed in a 120ml polytetrafluoroethylene reaction kettle to be subjected to solvothermal reaction for 48 hours at the reaction temperature of 60 ℃. And naturally cooling to room temperature, and respectively centrifugally washing with ethanol and deionized water to collect solvothermal products to obtain the cadmium sulfide nanoflower with the hierarchical structure constructed by the exposed (001) crystal face ultrathin nano-pages.
Example 3:
40mmol of S powder and 10.0mmol of Cd (NO)3)24.0mmol of deionized water and 800.0mmol of diethylenetriamine are fully stirred and uniformly dispersed, and then are placed in a 120ml polytetrafluoroethylene reaction kettle to carry out solvothermal reaction for 48 hours at the reaction temperature of 70 ℃. And naturally cooling to room temperature, and respectively centrifugally washing with ethanol and deionized water to collect solvothermal products to obtain the cadmium sulfide nanoflower with the hierarchical structure constructed by the exposed (001) crystal face ultrathin nano-pages.
Example 4:
40mmol of S powder and 5mmol of CdCl2、5mmol Cd(CH3COO)24.0mmol of deionized water and 1000.0mmol of diethylenetriamine are fully stirred and uniformly dispersed, and then the mixture is placed in a 120ml polytetrafluoroethylene reaction kettle to carry out solvothermal reaction for 24 hours at the reaction temperature of 100 ℃.And naturally cooling to room temperature, and respectively centrifugally washing with ethanol and deionized water to collect solvothermal products to obtain the cadmium sulfide nanoflower with the hierarchical structure constructed by the exposed (001) crystal face ultrathin nano-pages.
Comparative example:
1.2mmol of Cd (CH)3COO)2·2H2O and 3.6mmol NH2CSNH2Dissolved in 40ml of deionized water, fully stirred for 2h, and then the mixed solution is put into a 100ml hydrothermal reaction kettle for reaction at 180 ℃ for 12 h. And after the reaction kettle is cooled to room temperature, washing the reaction product with deionized water for three times, centrifugally collecting solids, and drying in a 60-DEG oven for 12 hours to obtain the CdS nanoparticles.
CdS nano-particle photocatalytic CO prepared in comparative example under same conditions2The reduction produced CO yield of about 0.776umol/h/g catalyst, only about 49.8% of CdS nanoflower CO yield (1.558 umol/h/g). The CdS nanoflower prepared by the method has good photocatalytic CO2The method has obvious advantages in reducing activity.
Claims (6)
1. A cadmium sulfide nanoflower with a hierarchical structure constructed by exposed (001) crystal face ultrathin nano-pages is characterized in that: the cadmium sulfide nanoflower with the hierarchical structure is composed of exposed (001) crystal face ultrathin cadmium sulfide nano-pages with the thickness of 2-4 nm.
2. The cadmium sulfide nanoflower with a hierarchical structure constructed by exposed (001) crystal surface ultrathin nano-pages as claimed in claim 1, wherein: the crystal form of the cadmium sulfide is wurtzite, and the diameter of the cadmium sulfide nanoflower with the hierarchical structure is 0.3-1 um.
3. A preparation method of a hierarchical structure cadmium sulfide nanometer flower constructed by exposed (001) crystal face ultrathin nanometer pages is characterized by comprising the following steps: the preparation process comprises the following steps:
a) uniformly mixing inorganic cadmium salt, deionized water, diethylenetriamine and sulfur powder;
b) carrying out solvothermal reaction, washing and drying to obtain the cadmium sulfide nanoflower with the hierarchical structure constructed by the exposed (001) crystal face ultrathin nano-sheets.
4. The method for preparing a cadmium sulfide nanoflower with a hierarchical structure constructed by exposing (001) crystal face ultrathin nano-pages as claimed in claim 3, wherein the method comprises the following steps: the ratio of the sulfur powder to the inorganic cadmium salt is 4-8: 1, the ratio of the deionized water to the inorganic cadmium salt is 0.3-0.7: 1, and the ratio of the diethylenetriamine to the inorganic cadmium salt is 200-500: 1.
5. The method for preparing a cadmium sulfide nanoflower with a hierarchical structure constructed by exposing (001) crystal plane ultrathin nano-pages as claimed in claim 3 or 4, wherein the method comprises the following steps: the inorganic cadmium salt is Cd (NO)3)2、CdCl2、Cd(CH3COO)2、Cd(NO3)2·4H2O、CdCl2·2.5H2O or Cd (CH)3COO)2·2H2Any one or a mixture of two or more of O.
6. The method for preparing a cadmium sulfide nanoflower with a hierarchical structure constructed by exposing (001) crystal face ultrathin nano-pages as claimed in claim 3, wherein the method comprises the following steps: the solvothermal reaction temperature is 60-100 ℃, and the reaction time is 24-72 h.
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| CN107043124A (en) * | 2017-05-19 | 2017-08-15 | 中南大学 | A kind of cadmium sulfide nano flower, preparation and its application |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107043124A (en) * | 2017-05-19 | 2017-08-15 | 中南大学 | A kind of cadmium sulfide nano flower, preparation and its application |
Non-Patent Citations (3)
| Title |
|---|
| Influence of the solvent on the structure, morphology and performance for H2 evolution of CdS photocatalysts prepared by solvothermal method;F. Vaquero等;《Applied Catalysis B: Environmental》;20161027;753–767 * |
| Jiali Lv等.Controllable synthesis of inorganic-organic Zn1−xCdxS-DETA solid solution nanoflowers and their enhanced visible-light photocatalytic hydrogen-production performance.《Dalton Trans》.2017,第11336页Experimental，第11338页图2b. * |
| Shape-Controlled Synthesis of CdS Nanostructures via a Solvothermal Method;Xiuli Wang等;《Crystal Growth & Design》;20101101;5312-5318页 * |
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