CN103381367A - Photocatalytic water splitting hydrogen production material CdS/Ba0.9Zn0.1TiO3 and preparation method thereof - Google Patents
Photocatalytic water splitting hydrogen production material CdS/Ba0.9Zn0.1TiO3 and preparation method thereof Download PDFInfo
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- 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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Abstract
A photocatalytic water splitting hydrogen production material CdS/Ba<sub>0.9</sub>Zn<sub>0.1</sub>TiO<sub>3 </sub> is a catalyst with a heterostructure formed by enabling CdS to be loaded to Ba<sub>0.9</sub>Zn<sub>0.1</sub>TiO<sub>3 </sub>, and the catalyst is obtained by a hydrothermal sol-gel process. When the molar ratio of CdS and Ba<sub>0.9</sub>Zn<sub>0.1</sub>TiO<sub>3 </sub> is 1:5, the expression is 20%CdS/Ba<sub>0.9</sub>Zn<sub>0.1</sub>TiO<sub>3 </sub>, and the catalytic effect of the material is optimal. Under the exposure of a xenon lamp of 300 watts, Na2S/Na2SO3 serves as a sacrifice reagent. The photocatalytic water splitting hydrogen production material CdS/Ba<sub>0.9</sub>Zn<sub>0.1</sub>TiO<sub>3 </sub> has the advantages that the catalyst is directly synthesized in a hydrothermal sol-gel process and is simple in operate, low in production cost, high in synthesis yield, extremely high in purity, good in repeatability and suitable for the requirements of expanded production; the catalyst is good in stability and convenient to recycle; and the catalyst is high in photocatalysis hydrogen production efficiency.
Description
Technical field
The present invention relates to a kind of hydrogen material from photocatalytic water decomposition CdS/Ba
0.9zn
0.1tiO
3and preparation method thereof.
Background technology
The energy is the basis of mankind's activity and the material premise of human social development, with traditional fossil energy (as coal, oil), compare, hydrogen can be a kind of clean energy resource, it can obtain from water, product after completing combustion is water, can not cause any pollution to environment, be the cleanest in the world energy.Although utilize at present the fossil energies such as natural gas, oil, coal by the technology comparative maturity of thermochemical method preparing hydrogen, but it is neither uneconomical, not environmental protection again, and the power consumption of the method for brine electrolysis is larger, if we can utilize regenerative resource (as solar energy) decomposition water to produce hydrogen, hydrogen can be called real " green energy resource " so.
Japanese scholars Fujishima A and Honda K are from the sixties in last century foot couple illumination n-type semiconductor TiO
2thereby the discovery that electrode causes the decomposition of water to produce this phenomenon of hydrogen, disclosed and utilized decomposing water with solar energy hydrogen manufacturing-in other words solar energy the is converted into possibility of chemical energy.At present, in numerous photochemical catalysts, TiO
2, the plurality of advantages such as photoetch little, non-secondary pollution suitable with its non-toxic inexpensive, conduction band valence band current potential, become the focus in multiphase photocatalysis field, and be considered to the current environmental type photochemical catalyst that has DEVELOPMENT PROSPECT most.Yet TiO
2have following problems: 1, the recombination rate of photo-induced hole and light induced electron is fast, and quantum efficiency is low; 2., TiO
2adsorptivity to pollutant is poor; 3, forbidden band wider (Eg=3.2ev).Therefore, be necessary the photochemical catalyst of exploration and development of new.
Summary of the invention
The object of the present invention is to provide a kind of novel photocatalysis hydrogen production by water decomposition material and preparation method thereof, for solving current energy problem, provide new material.Material of the present invention preparation is to adopt hydro-thermal melten gel method, and it is simple to operate, low production cost, synthetic productive rate are higher, and purity is also very high and reproducible, is applicable to the requirement that extension is produced.
The present invention is achieved like this, and it is characterized in that catalyst is to load to Ba by CdS
0.9zn
0.1tiO
3and the hetero-junctions catalyst formed.As CdS and Ba
0.9zn
0.1tiO
3mol ratio be 1: 5 o'clock, its expression formula is 20%CdS/Ba
0.9zn
0.1tiO
3, catalytic effect the best of material.Under 300 watts of xenon lamps irradiate, with Na
2s/Na
2sO
3for sacrificing reagent, material 20%CdS/Ba of the present invention
0.9zn
0.1tiO
3in the syncatalytic situation of non precious metal, photochemical catalyzing hydrogen producing efficiency reaches 1473
.
Catalyst CdS/Ba of the present invention
0.9zn
0.1tiO
3can be by changing CdS and Ba
0.9zn
0.1tiO
3mol ratio, thereby obtain the CdS/Ba of different loads ratio
0.9zn
0.1tiO
3the hetero-junctions catalyst.
Catalyst CdS/Ba of the present invention
0.9zn
0.1tiO
3the preparation method be: the Ba that 2 grams are prepared by the hydro-thermal sol method
0.9zn
0.1tiO
3powder is scattered in 30 ml waters, after stirring, adds the cadmium acetate of respective amount (according to CdS and Ba
0.9zn
0.1tiO
3mol ratio different and add the cadmium acetates of different amounts, the scope of its use amount is: 0.2256 ~ 0.9024 gram), ultrasonic dispersion 15 minutes, add the thiocarbamide of respective amount (according to CdS and Ba
0.9zn
0.1tiO
3mol ratio different and add the thiocarbamides of different amounts, the scope of its use amount is: 0.0644 ~ 0.2574 gram), ultrasonic dispersion 15 minutes, pack gained solution in the reactor of polytetrafluoroethylene (PTFE) of 100 milliliters into, puts into the Muffle furnace hydro-thermal reaction 10 hours of 150 ℃.Sample after hydro-thermal reaction is carried out to multiple times of filtration, washing, and dry rear the grinding, obtain the target catalyst.
Ba wherein
0.9zn
0.1tiO
3standby by hydro-thermal melten gel legal system, its preparation method is as follows: first the zinc acetate of 9 mMs of (2.4609 gram) barium acetates and 1 mM (0.2195 gram) being dissolved in to 10 ml concns is the volume ratio that 36%(acetic acid accounts for solution) acetic acid solution in, stir 30 minutes, obtain A solution.Then the tetra-n-butyl titanate of 10 mMs is dissolved in the isopropyl alcohol of 5 milliliters, and adds 1.5 milliliters of glacial acetic acids to stir all and obtain B solution.B solution slowly is added drop-wise in A solution, stirs after 30 minutes and obtain C solution.C solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 25 milliliters, put into the Muffle furnace hydro-thermal reaction 2 hours of 100 ℃.The xerogel obtained is ground, and, in 900 ℃ of calcinings 10 hours, grind and obtain Ba
0.9zn
0.1tiO
3powder.
Advantage of the present invention is: 1, catalyst of the present invention is to adopt the hydro-thermal melten gel directly synthetic, and it is simple to operate, low production cost, synthetic productive rate are higher, and purity is also very high and reproducible, is applicable to the requirement that extension is produced; 2, catalyst stability of the present invention is good, is convenient to recycling; 3, catalyst of the present invention is under simulated solar irradiation, and Photocatalyzed Hydrogen Production efficiency is very high.
The accompanying drawing explanation
Fig. 1 is catalyst of the present invention and pure Ba
0.9zn
0.1tiO
3, CdS and different loads ratio CdS/ Ba
0.9zn
0.1tiO
3(in figure, 0% represents Ba to the X-ray powder diffraction comparison diagram of hetero-junctions catalyst
0.9zn
0.1tiO
3, 10% represent 10%CdS/Ba
0.9zn
0.1tiO
3, 20% represent 20%CdS/Ba
0.9zn
0.1tiO
3, 30% represent 30%CdS/Ba
0.9zn
0.1tiO
3, 40% represent 40%CdS/Ba
0.9zn
0.1tiO
3and CdS represents the standard powder diffraction maximum of pure CdS).
Fig. 2 is catalyst of the present invention and pure BaTiO
3, Ba
0.9zn
0.1tiO
3, CdS and different loads ratio CdS/Ba
0.9zn
0.1tiO
3(in figure, 10% represents 10%CdS/Ba to the UV-Vis DRS comparison diagram of hetero-junctions catalyst
0.9zn
0.1tiO
3, 20% represent 20%CdS/Ba
0.9zn
0.1tiO
3, 30% represent 30%CdS/Ba
0.9zn
0.1tiO
3, 40% represent 40%CdS/Ba
0.9zn
0.1tiO
3and CdS, BaTiO
3and Ba
0.9zn
0.1tiO
3represent respectively pure CdS, BaTiO
3and Ba
0.9zn
0.1tiO
3).
Fig. 3 is catalyst of the present invention and Ba
0.4sr
0.6tiO
3and the CdS/Ba of different loads ratio
0.4sr
0.6tiO
3the hetero-junctions catalyst is under the inducing of simulated solar irradiation, with Na
2s/Na
2sO
3for sacrificing reagent, in the syncatalytic situation of non precious metal, (in figure, 0% represents Ba to the comparative effectiveness figure of photocatalysis Decomposition aquatic products hydrogen
0.9zn
0.1tiO
3, 10% represent 10%CdS/Ba
0.9zn
0.1tiO
3, 20% represent 20%CdS/Ba
0.9zn
0.1tiO
3, 30% represent 30%CdS/Ba
0.9zn
0.1tiO
3, 40% represent 40%CdS/Ba
0.9zn
0.1tiO
3).
The specific embodiment
1, compd B a
0.9zn
0.1tiO
3synthetic
First the zinc acetate of 9 mMs of (2.4609 gram) barium acetates and 1 mM (0.2195 gram) is dissolved in (acetic acid accounts for the volume ratio of solution) acetic acid solution that 10 ml concns are 36%, stirs 30 minutes, obtain A solution.Then the tetra-n-butyl titanate of 10 mMs is dissolved in the isopropyl alcohol of 5 milliliters, and adds 1.5 milliliters of glacial acetic acids to stir all and obtain B solution.B solution slowly is added drop-wise in A solution, stirs after 30 minutes and obtain C solution.C solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 25 milliliters, put into the Muffle furnace hydro-thermal reaction 2 hours of 100 ℃.The xerogel obtained is ground, and, in 900 ℃ of calcinings 10 hours, grind and obtain Ba
0.9zn
0.1tiO
3powder.
2, catalyst 10%CdS/Ba
0.9zn
0.1tiO
3synthetic
Take the Ba that 2 restraints are got ready
0.9zn
0.1tiO
3powder is scattered in 30 ml waters, drip the solution that 0.2256 gram cadmium acetate is made into after stirring, ultrasonic dispersion 15 minutes, drip the solution that 0.0644 gram thiocarbamide is made into, ultrasonic dispersion 15 minutes, gained solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 100 milliliters, put into the Muffle furnace hydro-thermal reaction 10 hours of 150 ℃.Sample after hydro-thermal reaction is carried out to multiple times of filtration, washing, and dry rear the grinding, obtain the target catalyst.
3, catalyst 20%CdS/Ba
0.9zn
0.1tiO
3synthetic
Take the Ba that 2 restraints are got ready
0.9zn
0.1tiO
3powder is scattered in 30 ml waters, drip the solution that 0.4514 gram cadmium acetate is made into after stirring, ultrasonic dispersion 15 minutes, drip the solution that 0.1286 gram thiocarbamide is made into, ultrasonic dispersion 15 minutes, gained solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 100 milliliters, put into the Muffle furnace hydro-thermal reaction 10 hours of 150 ℃.Sample after hydro-thermal reaction is carried out to multiple times of filtration, washing, and dry rear the grinding, obtain the target catalyst.
4, catalyst 30%CdS/Ba
0.9zn
0.1tiO
3synthetic
Take the Ba that 2 restraints are got ready
0.9zn
0.1tiO
3powder is scattered in 30 ml waters, drip the solution that 0.6769 gram cadmium acetate is made into after stirring, ultrasonic dispersion 15 minutes, drip the solution that 0.1933 gram thiocarbamide is made into, ultrasonic dispersion 15 minutes, gained solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 100 milliliters, put into the Muffle furnace hydro-thermal reaction 10 hours of 150 ℃.Sample after hydro-thermal reaction is carried out to multiple times of filtration, washing, and dry rear the grinding, obtain the target catalyst.
5, catalyst 40%CdS/Ba
0.9zn
0.1tiO
3synthetic
Take the Ba that 2 restraints are got ready
0.9zn
0.1tiO
3powder is scattered in 30ml water, drip the solution that 0.9024 gram cadmium acetate is made into after stirring, ultrasonic dispersion 15 minutes, drip the solution that 0.2574 gram thiocarbamide is made into, ultrasonic dispersion 15 minutes, gained solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 100 milliliters, put into the Muffle furnace hydro-thermal reaction 10 hours of 150 ℃.Sample after hydro-thermal reaction is carried out to multiple times of filtration, washing, and dry rear the grinding, obtain the target catalyst.
As shown in Figure 1, through X-ray powder diffraction test, show catalyst of the present invention and pure Ba
0.9zn
0.1tiO
3contrasted, in X-ray powder diffraction figure, peak position does not change, and illustrates that the sulfur loaded cadmium do not destroy Ba
0.9zn
0.1tiO
3structure, and, along with the load capacity of cadmium sulfide increases, the peak of cadmium sulfide strengthens gradually, illustrates that cadmium sulfide loads to Ba
0.9zn
0.1tiO
3rather than be doped to Ba
0.9zn
0.1tiO
3in structure.In addition as can be seen from Figure 2, BaTiO
3after doping zinc, the red shift to some extent of its absorption edge, Ba
0.9zn
0.1tiO
3after the sulfur loaded cadmium, along with the band gap width that increases catalyst (Eg value) of cadmium sulfide content presents orderly variation.As shown in Figure 3, catalyst 20%CdS/Ba of the present invention
0.9zn
0.1tiO
3under the inducing of simulated solar irradiation, with Na
2s/Na
2sO
3for sacrificing reagent, in the syncatalytic situation of non precious metal, the hydrogen-producing speed of photochemical catalyzing reaches 1473
.With single Ba
0.9zn
0.1tiO
3and the CdS/Ba of other load ratios
0.9zn
0.1tiO
3the hetero-junctions catalyst is compared, under same experimental conditions, and catalyst 20%CdS/Ba of the present invention
0.4sr
0.6tiO
3photocatalysis Decomposition aquatic products hydrogen catalysis best results.The result of elementary analysis shows catalyst 20%CdS/Ba in addition
0.4sr
0.6tiO
3in only contain Cd, S, Ba, Sr, Ti, six kinds of elements of O, and the ratio between element also conforms to substantially with the ratio in expression formula.Catalyst of the present invention is to adopt the hydro-thermal sol method synthetic, and it is simple to operate, low production cost, synthetic productive rate are higher, and purity is also very high and reproducible, is applicable to the requirement that extension is produced; Catalyst stability of the present invention is good, is convenient to recycling; Catalyst of the present invention is under the xenon lamp irradiation of 300 watts, and the Photocatalyzed Hydrogen Production effect is better, is desirable photocatalysis Decomposition aquatic products hydrogen material.
Claims (4)
1. a hydrogen material from photocatalytic water decomposition CdS/Ba
0.9zn
0.1tiO
3, it is characterized in that by CdS and Ba
0.9zn
0.1tiO
3and the hetero-junctions formed, as CdS and Ba
0.9zn
0.1tiO
3mol ratio while being 1:5, its expression formula is 20%CdS/Ba
0.9zn
0.1tiO
3, catalytic effect the best of material, under the xenon lamps of 300 watts irradiate, with Na
2s/Na
2sO
3for sacrificing reagent, material 20%CdS/Ba of the present invention
0.9zn
0.1tiO
3in the syncatalytic situation of non precious metal, photochemical catalyzing hydrogen producing efficiency reaches 1473
.
2. a kind of hydrogen material from photocatalytic water decomposition CdS/Ba as claimed in claim 1
0.9zn
0.1tiO
3, it is characterized in that can be by changing CdS and Ba
0.9zn
0.1tiO
3mol ratio, thereby obtain the CdS/Ba of different loads ratio
0.9zn
0.1tiO
3the hetero-junctions catalyst, CdS and Ba
0.9zn
0.1tiO
3the mol ratio excursion be 10% ~ 40%.
3. a kind of hydrogen material from photocatalytic water decomposition CdS/Ba as claimed in claim 1
0.9zn
0.1tiO
3, it is characterized in that: Ba
0.9zn
0.1tiO
3the preparation method be:
First the zinc acetate of 9 mMs of barium acetates and 1 mM is dissolved in the acetic acid solution that 10 ml concns are 36%, stir 30 minutes, obtain A solution, then the tetra-n-butyl titanate of 10 mMs is dissolved in the isopropyl alcohol of 5 milliliters, and add 1.5 milliliters of glacial acetic acids to stir to obtain B solution, B solution slowly is added drop-wise in A solution, stir and obtain C solution after 30 minutes, C solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 25 milliliters, put into the Muffle furnace hydro-thermal reaction 2 hours of 100 ℃, the xerogel obtained is ground, and in 900 ℃ of calcinings 10 hours, grinding obtains Ba
0.9zn
0.1tiO
3powder.
4. a hydrogen material from photocatalytic water decomposition CdS/Ba claimed in claim 1
0.9zn
0.1tiO
3the preparation method, it is characterized in that:
Ba prepared by the hydro-thermal sol method by 2 grams
0.9zn
0.1tiO
3powder is scattered in 30 ml waters, adds the cadmium acetate of respective amount after stirring, according to CdS and Ba
0.9zn
0.1tiO
3mol ratio different and add the cadmium acetates of different amounts, the scope of its use amount is: 0.2256 ~ 0.9024 gram; Ultrasonic dispersion 15 minutes, add the thiocarbamide of respective amount, according to CdS and Ba
0.9zn
0.1tiO
3mol ratio different and add the thiocarbamides of different amounts, the scope of its use amount is: 0.0644 ~ 0.2574 gram, ultrasonic dispersion 15 minutes, gained solution is packed in the reactor of polytetrafluoroethylene (PTFE) of 100 milliliters, put into the Muffle furnace hydro-thermal reaction 10 hours of 150 ℃, sample after hydro-thermal reaction is carried out to multiple times of filtration, washing, and dry rear the grinding, obtain the target catalyst.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104261464A (en) * | 2014-09-29 | 2015-01-07 | 浙江大学 | Preparation method of one-dimensional lead titanate/cadmium sulfide composite nano structure |
CN104261463A (en) * | 2014-09-29 | 2015-01-07 | 浙江大学 | Method for preparing lead titanate nanosheet and cadmium sulfide nano-particle composite material |
CN105727997A (en) * | 2016-01-29 | 2016-07-06 | 上海师范大学 | Cadmium sulfide/sodium titanate supported type compound visible-light-driven photocatalyst and preparation method and application thereof |
CN111304671A (en) * | 2020-02-19 | 2020-06-19 | 台州学院 | Sr-doped BaTiO3Preparation method of/ZnTe photocathode material |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104261464A (en) * | 2014-09-29 | 2015-01-07 | 浙江大学 | Preparation method of one-dimensional lead titanate/cadmium sulfide composite nano structure |
CN104261463A (en) * | 2014-09-29 | 2015-01-07 | 浙江大学 | Method for preparing lead titanate nanosheet and cadmium sulfide nano-particle composite material |
CN105727997A (en) * | 2016-01-29 | 2016-07-06 | 上海师范大学 | Cadmium sulfide/sodium titanate supported type compound visible-light-driven photocatalyst and preparation method and application thereof |
CN111304671A (en) * | 2020-02-19 | 2020-06-19 | 台州学院 | Sr-doped BaTiO3Preparation method of/ZnTe photocathode material |
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