CN104801329A - CdS quantum dot/superthin g-C3N4 nanosheet composite photocatalyst and preparation method thereof - Google Patents
CdS quantum dot/superthin g-C3N4 nanosheet composite photocatalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a CdS quantum dot/superthin g-C3N4 nanosheet composite photocatalyst and a preparation method thereof. CdS quantum dot/superthin g-C3N4 is a composite visible light catalyst formed by loading CdS quantum dots on a superthin g-C3N4 nanosheet. Compared with a pure g-C3N4 catalyst, the CdS quantum dot/superthin g-C3N4 photocatalyst prepared by the preparation method disclosed by the invention is higher in photocatalyst activity; under the irradiation of visible light, the hydrogen production efficiency of the catalyst by photocatalytic decomposition reaches 998mu molh<-1>g<-1>. The CdS quantum dot/superthin g-C3N4 nanosheet composite photocatalyst and the preparation method thereof disclosed by the invention have the advantages that raw materials are low in price and easily obtained, an experiment method is simple, and the catalyst is wide in light response range and high in photocatalytic efficiency. The material is matched with other materials to form a corresponding photocatalytic device; the CdS quantum dot/superthin g-C3N4 nanosheet composite photocatalyst has good potential application prospect of promoting the industrial development of the solar scale hydrogen production technology and solar catalytic oxidation and synthesis.
Description
Technical field
The present invention relates to a kind of CdS quantum dot/ultra-thin g-C
3n
4nanometer sheet composite photo-catalyst and preparation method thereof.
Background technology
The energy is the basis of mankind's activity and the material premise of human social development, compared with traditional fossil energy (as coal, oil), hydrogen can be a kind of clean energy resource, it can obtain from water, product completely after burning is water, can not cause any pollution to environment, be the energy the cleanest in the world.Although utilize the fossil energies such as natural gas, oil, coal ripe by the Technical comparing of thermochemical method preparing hydrogen at present, but it is both uneconomical, again not environmentally, and the method power consumption of brine electrolysis is larger, if we can utilize regenerative resource (as solar energy) decomposition water to produce hydrogen, so hydrogen can be called real " green energy resource ".
Fujishima reported first in 1972 can with TiO
2in photoelectrochemical cell for light anode, break water into H with UV-irradiation light anode
2and O
2, this is an important discovery with " milestone " meaning, this imply that people can utilize cheap solar energy to make water decomposition by semiconductor catalysis thus obtain clean hydrogen fuel.In recent years, due to TiO
2have the advantage such as cheap, nontoxic by and be widely used in the every field of photocatalysis research.But this photochemical catalyst is unsatisfactory in actual applications, also exist that visible ray utilization rate is low, the not easily shortcoming such as recovery, preparation condition harshness, the easy compound of light induced electron and hole.Therefore, the photochemical catalyst of exploration and development of new is necessary.
Graphene-like C
3n
4, referred to as g-C
3n
4, because the physical property of its excellence and photoelectric properties become the hot material of current research.2008, University of Fuzhou king heart morning etc. for template with the Ludox of 12 nm, took cyanamide as raw material, has synthesized mesoporous g-C
3n
4/r(r=0.2 that 1.5,3.75,7.5,12.25 g Ludox are corresponding, 0.5,1,1.5), i.e. mpg-C
3n
4/ruse mpg-C
3n
4/rbe reductive water H
2experiment, in the water of 100 mL containing volume fraction be the triethanolamine of 10% as sacrifice agent, be greater than the radiation of visible light of 420 nm at wavelength under, the mpg-C of unmodified
3n
4/0.5hydrogen-producing speed is 0.2 μm of ol/h, and Photodeposition load quality mark is the mpg-C of the Pt of 3%
3n
4/0.5hydrogen-producing speed reaches 142 μm of ol/h.
2010, Japanese state-run Materials Research Laboratories Zhang etc. were with dicyandiamide and ionic liquid BmimPF
6for raw material synthesis P-g-C
3n
4, from the peak of its XPS analysis known existence 133.5 eV, be the peak of typical P-N key, and wherein there is not the particular peaks of P-C, illustrate C element replace by P element.Because the doping content of P element is less, P-g-C
3n
4keep more complete g-C
3n
4structure, but obviously change g-C
3n
4electronic structure, make its electrical conductivity in the dark improve 4 orders of magnitude, and the generation of photoelectric current improves 5 times, this is for photochemical catalyst g-C
3n
4the popularization of application has important meaning.
2011, the general colloid of German horse and Interface Study institute Li etc. synthesized graphene film/g-C
3n
4, due to interlayer structure and the g-C of graphene film
3n
4similar, and Graphene is very firm firm, and the speed at room temperature transmitting electronics is all faster than conductor, therefore graphene film can be used as electronics to body to modify g-C
3n
4.Graphene film/g-C
3n
4having outstanding selective oxidation methylene is the ability of ketone, and the yield that oxidizing ethyle alkyl generates cyclohexanone is 12%, and selective is 94%; It is 12% that Oxybenzene ethane generates the yield of acetophenone, selectively reaches 99%.
At present, g-C
3n
4light-catalysed problems are also undistinct, strengthen fundamental research and will promote the development in this field.Light-catalysed fundamental research, comprises multiple element or the composite modified g-C of compound
3n
4physical mechanism, modification g-C that the design of photochemical catalyst and synthesis, different modifier are separated with hole light absorption and light-catalysed synergy, light induced electron under modified condition
3n
4the chemical stabilities of photochemical catalyst etc. relate to multi-disciplinary intersection, still need to carry out a large amount of work.Explore new research means and method, build novel, continuous, stable, efficient g-C
3n
4photocatalysis system, further promotes photoresponse scope and quantum efficiency, and coordinates to other materials and forms corresponding photocatalytic device, the industrialization development etc. that promotion solar energy Hydrogen Production In Mass Scale technology and solar energy catalytic oxidation synthesize.
Summary of the invention
The object of the present invention is to provide a kind of novel C dS quantum dot/ultra-thin g-C
3n
4nanometer sheet composite photo-catalyst and preparation method thereof, provides new material for solving current energy problem.
Technical scheme of the present invention mainly comprises the following aspects.
1, a kind of CdS quantum dot/ultra-thin g-C
3n
4nanometer sheet composite photo-catalyst, is characterized in that CdS quantum dot to load to ultra-thin g-C
3n
4nanometer sheet is (referred to as g-C
3n
4) and formed, wherein CdS quantum dot and g-C
3n
4mass ratio be 10%-100%.
2, a kind of CdS quantum dot/ultra-thin g-C
3n
4the preparation method of nanometer sheet composite photo-catalyst, is characterized in that following steps:
(1) block g-C is prepared
3n
4: take 5-10 g urea with crucible, cover lid is placed in Muffle furnace, is first raised to 250 DEG C with the heating rate of 5 DEG C/min, then is raised to 550 DEG C with the heating rate of 8 DEG C/min, calcine 2 h at 550 DEG C.Temperature fall, mills, and obtains block g-C
3n
4.
(2) ultra-thin g-C is prepared
3n
4nanometer sheet: the block g-C taking preparation in 50-500 mg step (1)
3n
4be dispersed in the deionized water of 50-500 mL, ultrasonic stripping 10-20 h, then leave standstill 10-20 h, by the organic filter membrane collected by suction of even for upper strata turbid liquid, obtain ultra-thin g-C
3n
4nanometer sheet.
(3) CdS quantum dot/ultra-thin g-C is prepared
3n
4: take the ultra-thin g-C of 50 mg
3n
4nanometer sheet adds in the dimethyl sulfoxide (DMSO) (DMSO) of 50 mL, evenly ultrasonic, then adds 9 mg-100 mg cadmium acetates, stir, be finally transferred in the water heating kettle of 100 mL, carry out hydro-thermal reaction in an oven, temperature controls at 120 DEG C-200 DEG C, and the reaction time is 8-20 h.Carry out organic filter membrane suction filtration, drying after reaction terminates, obtain CdS quantum dot/ultra-thin g-C
3n
4nanometer sheet composite photo-catalyst.
Remarkable advantage of the present invention is: CdS quantum dot of the present invention/ultra-thin g-C
3n
4composite photo-catalyst preparation method, structure composition and photocatalysis performance in all with existing CdS quantum dot/g-C
3n
4catalyst is different.Material of main part of the present invention is the ultra-thin g-C of CdS quantum dot load
3n
4, be by block g-C
3n
4by the ultra-thin g-C that ultrasonic stripping method plug is elected
3n
4nanometer sheet, has higher photocatalytic activity.Catalyst of the present invention also has that photoresponse wide ranges, photocatalysis efficiency are high, the prices of raw and semifnished materials are cheaply easy to get, experimental technique simple operation and other advantages.Therefore, the present invention has a good application prospect in photocatalysis field and solution energy crisis.
Accompanying drawing explanation
Fig. 1 is ultra-thin g-C of the present invention
3n
4with CdS quantum dot/ultra-thin g-C
3n
4the XRD figure of photochemical catalyst.
Fig. 2 is ultra-thin g-C of the present invention
3n
4with CdS quantum dot/ultra-thin g-C
3n
4the UV-Vis DRS comparison diagram of photochemical catalyst.
Fig. 3 is block g-C of the present invention
3n
4, ultra-thin g-C
3n
4and CdS quantum dot/ultra-thin g-C
3n
4catalyst, under visible light conditions, take volume fraction as the triethanolamine of 10 vol% is sacrifice agent, and mass fraction is the Pt of 3 wt% is co-catalyst, the comparative effectiveness figure of photocatalysis Decomposition aquatic products hydrogen.
Detailed description of the invention
Illustrate below in conjunction with accompanying drawing and be described in further detail embodiments of the invention, the present embodiment is preferred embodiment, is not limited to the present invention, and every employing analog structure of the present invention and similar change thereof, all should list protection scope of the present invention in.
The synthesis of catalyst material of the present invention:
(1) block g-C is prepared
3n
4: take 6.5 g urea with crucible, cover lid is placed in Muffle furnace, is first raised to 250 DEG C with the heating rate of 5 DEG C/min, then is raised to 550 DEG C with the heating rate of 8 DEG C/min, calcine 2 h at 550 DEG C.Temperature fall, mills, and obtains block g-C
3n
4.
(2) ultra-thin g-C is prepared
3n
4nanometer sheet: by the block g-C of 200 mg prepared above
3n
4be dispersed in the deionized water of 200 mL, ultrasonic stripping 16 h, then leave standstill 12 h, by even for upper strata turbid liquid 0.22 μm of organic filter membrane collected by suction, obtain ultra-thin g-C
3n
4nanometer sheet.
(3) CdS quantum dot/ultra-thin g-C is prepared
3n
4: take the ultra-thin g-C of 50 mg
3n
4nanometer sheet adds in the dimethyl sulfoxide (DMSO) (DMSO) of 50 mL, evenly ultrasonic, then adds 92 mg cadmium acetates, stirs, and is finally transferred in the water heating kettle of 100 mL, carries out hydro-thermal reaction in an oven, and temperature controls at 180 DEG C, and the reaction time is 12 h.Carry out organic filter membrane suction filtration, drying after reaction terminates, obtain CdS quantum dot/ultra-thin g-C
3n
4nanometer sheet composite photo-catalyst.
As shown in Figure 1, show through X-ray powder diffraction test, CdS quantum dot of the present invention/ultra-thin g-C
3n
4photochemical catalyst and pure ultra-thin g-C
3n
4contrast, g-C in X-ray powder diffraction figure
3n
4peak position do not change, illustrate that the load of CdS quantum dot does not destroy g-C
3n
4structure, and two peaks containing CdS detected, illustrate that CdS quantum dot successfully loads to ultra-thin g-C
3n
4on.In addition as can be seen from Figure 2, CdS quantum dot/ultra-thin g-C
3n
4pure ultra-thin g-C compared by photochemical catalyst
3n
4absorption edge there occurs obvious Red Shift Phenomena, illustrates that ultra-thin g-C has been widened in the load of CdS quantum dot
3n
4light abstraction width, thus there is higher photocatalytic activity.Raman spectrum shows CdS quantum dot and ultra-thin g-C
3n
4there is weak force to exist between nanometer sheet, define hetero-junctions instead of simple mixture.As shown in Figure 3, CdS quantum dot of the present invention/ultra-thin g-C
3n
4photochemical catalyst, under visible light conditions, take volume fraction as the triethanolamine of 10 vol% is sacrifice agent, and mass fraction is the Pt of 3 wt% is co-catalyst, and photochemical catalyzing hydrogen-producing speed reaches 998 μm of olh
-1g
-1.With pure block g-C
3n
4with ultra-thin g-C
3n
4catalyst is compared, under same experimental conditions, and CdS quantum dot of the present invention/ultra-thin g-C
3n
4the photocatalysis Decomposition aquatic products hydrogen best results of photochemical catalyst.
Catalyst of the present invention also has that photoresponse wide ranges, photocatalysis efficiency are high, the prices of raw and semifnished materials are cheaply easy to get, experimental technique is simple to operate, is desirable photocatalysis Decomposition aquatic products hydrogen material.
Claims (2)
1. CdS quantum dot/ultra-thin g-C
3n
4nanometer sheet composite photo-catalyst, is characterized in that CdS quantum dot to load to ultra-thin graphene-like C
3n
4nanometer sheet is formed, wherein CdS quantum dot and g-C
3n
4mass ratio be 10%-100%.
2. CdS quantum dot according to claim 1/ultra-thin g-C
3n
4the preparation method of nanometer sheet composite photo-catalyst, is characterized in that method step is as follows:
(1) block g-C is prepared
3n
4: take 5-10 g urea with crucible, cover lid is placed in Muffle furnace, is first raised to 250 DEG C with the heating rate of 5 DEG C/min, then is raised to 550 DEG C with the heating rate of 8 DEG C/min, calcine 2 h, Temperature fall, mill at 550 DEG C, obtains block g-C
3n
4;
(2) ultra-thin g-C is prepared
3n
4nanometer sheet: the block g-C taking preparation in 50-500 mg step (1)
3n
4be dispersed in the deionized water of 50-500 mL, ultrasonic stripping 10-20 h, then leave standstill 10-20 h, by the organic filter membrane collected by suction of even for upper strata turbid liquid, obtain ultra-thin g-C
3n
4nanometer sheet;
(3) CdS quantum dot/ultra-thin g-C is prepared
3n
4: take the ultra-thin g-C of 50 mg
3n
4nanometer sheet adds in the dimethyl sulfoxide (DMSO) of 50 mL, evenly ultrasonic, then adds 9 mg-100 mg cadmium acetates, stir, be finally transferred in the water heating kettle of 100 mL, carry out hydro-thermal reaction in an oven, temperature controls at 120 DEG C-200 DEG C, and the reaction time is 8-20 h; Carry out organic filter membrane suction filtration, drying after reaction terminates, obtain CdS quantum dot/ultra-thin g-C
3n
4nanometer sheet composite photo-catalyst.
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| CN105056985A (en) * | 2015-09-29 | 2015-11-18 | 李若然 | g-C3N4/graphene oxide/nano-iron visible-light response catalytic membrane |
| CN105148744A (en) * | 2015-08-25 | 2015-12-16 | 华南理工大学 | Adjustable and controllable ultrathin two-dimensional nano g-C3N4 film, and preparation method and application thereof |
| CN105170172A (en) * | 2015-09-29 | 2015-12-23 | 李若然 | Strong-reducing-property visible light response photocatalyst with urea and ferric chloride as raw materials |
| CN105536847A (en) * | 2016-02-19 | 2016-05-04 | 浙江一清环保工程有限公司 | Method for synthesizing magnetic separation g-C3N4-Fe3O4 photocatalyst through water bath |
| CN105562055A (en) * | 2016-01-14 | 2016-05-11 | 天津理工大学 | Method for preparing cadmium sulfide graphite-like carbon nitride compound photocatalyst |
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