CN101157044B - Ni doping Cd0.1Zn0.9S micrometre ball photocatalyst and preparation method - Google Patents

Ni doping Cd0.1Zn0.9S micrometre ball photocatalyst and preparation method Download PDF

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CN101157044B
CN101157044B CN200710018881XA CN200710018881A CN101157044B CN 101157044 B CN101157044 B CN 101157044B CN 200710018881X A CN200710018881X A CN 200710018881XA CN 200710018881 A CN200710018881 A CN 200710018881A CN 101157044 B CN101157044 B CN 101157044B
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郭烈锦
张相辉
敬登伟
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Xian Jiaotong University
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Abstract

The invention discloses Ni-doped Cd0.1Zn0.9 S microsphere photocatalyst and the preparation method thereof, the particle shape of the produced photocatalyst is a microsphere formed by nanometer crystals, and the doping amount of Ni is 0.1 percent to 0.5 percent of the weight of the catalyst. The invention has the preparation method that zinc sulfate, cadmium sulfate, nickel nitrate, and thioacetamide are taken as raw materials to form mixed solution which is sealed in a hydrothermal caldron and then laid in a baking oven to be insulated, naturally cooled to the room temperature, a resultant is obtained through cleaning, drying, and grinding. The Ni-doped Cd0.1Zn0.9S microsphere photocatalyst is prepared by the invention, and the anti-surface oxidation capability in air and the photo-corrosion resistant capability in the photocatalytic reaction are evenly enhanced greatly. Because the particle of the photocatalyst is microsphere-shaped, the photocatalytic activity for photocatalytic water splitting into hydrogen of visible light of the catalyst is greatly enhanced, and the highest hydrogen production rate reaches 191.01 micromole /(g*h). The quantum efficiency reaches 6.77 percent at the 420 nm position. After Pt of 0.6 wt percent is loaded, the highest hydrogen production rate reaches 585.45 micromole /(g*h), which is three times than the hydrogen production rate when the Pt is not loaded. The quantum efficiency reaches 15.9 percent at the 420 nm position, the activity is high, and the stability is good.

Description

Ni doping Cd 0.1Zn 0.9S micron ball photocatalyst and preparation method
Technical field
The invention belongs to the Hydrogen Energy preparation field, relate to the clean technology of preparing of photocatalysis of Hydrogen Energy, is the photocatalysis Decomposition hydrogen producing technology of raw material with water under the simulated solar visible light illumination condition promptly.Be particularly related to the sulphur zinc cadmium Cd that a kind of nickel (Ni) mixes 0.1Zn 0.9S micron ball photocatalyst and preparation method thereof.
Background technology
Conventional primary energy is under-supply, liquid fuel is short, the fossil energy utilization causes severe contamination, CO 2Reduce discharging pressure and outlying district, rural area and made China face multiple pressure, impel people to have to seek new clean alternative energy source with energy problem etc.Strengthen the fundamental research that renewable energy conversion is utilized energetically, the regenerative resource high-quality of development high efficiency, low cost transforms with scale utilizes technology, become China energy science and technology field from now on ten or twenty year urgent task the most.China has very abundant regenerative resource resource, and potentiality to be exploited is huge, from long term growth, can satisfy the demand of national sustainable development to energy resources fully.Yet because most regenerative resource energy densities are low, dispersed strong, unstable, discontinuous, in time, season and weather and change and make us still lack the effective means that high efficiency, low cost utilizes regenerative resource on a large scale so far.
Hydrogen is desirable secondary energy sources, has the energy density height, and advantages such as can storing, can transport, be pollution-free is renewable energy conversion a Hydrogen Energy, is the desirable approach that solves above-mentioned difficulties.Along with 21 century is the fast development that the various Hydrogen Energies of representative are utilized technology with the fuel cell, following China will rise significantly to the demand of hydrogen, and the regenerative resource scale hydrogen producing technology of development high efficiency, low cost has important social, economic benefit.International community is always in " the hydrogen economy " that promotes to form sustainable development energetically.The key factor that Hydrogen Energy economy forms is to obtain cheap hydrogen energy source.And utilize the hydrogen manufacturing of solar energy photocatalytic decomposition water scale is the current and even following new and high technology that is hopeful most to accomplish scale production and obtains cheap hydrogen.
The principle of photocatalysis hydrogen production is: under the irradiation of certain energy light, catalyst be subjected to exciting produce electronics and the hole right, electron transfer is reduced to hydrogen to catalyst surface with water, and the hole is consumed by the sacrifice agent of the suitable cheapness that is added in the system.The key that realizes the solar energy photocatalytic decomposition water is to seek the visible light-responded photochemical catalyst with appropriate bandgap.Although the report of visible light-responded in a large number photochemical catalyst is arranged at present in the world, mostly active on the low side and less stable.
Cadmium sulfide is a kind of generally acknowledged photochemical catalyst with higher photocatalytic hydrogen production activity, be widely studied in later 1980s, though the feature limits of the active higher very easily photoetch of cadmium sulfide its development.For this reason, the cadmium sulfide photochemical catalyst is carried out modification, as at cadmium sulfide area load noble metal (Pt), cadmium sulfide is inserted in the layered catalyst by multiple means.The research report is arranged in addition, and the cadmium sulfide photochemical catalyst can be compounded to form solid solution with wide bandgap semiconductor, thereby improves its photocatalytic activity.Sulphur zinc cadmium is exactly a kind of important ternary sulfide mischcrystal photocatalyst, along with the difference of cadmium, zinc content ratio, can obtain the sulphur zinc cadmium photochemical catalyst of a series of different band gap.
But when forming solid solution, valence band, the conduction band of photochemical catalyst change simultaneously, and conduction band reduces when band gap narrows down, and the easy like this product hydrogen activity of photochemical catalyst that makes descends.In addition, doping transition metal element in than the broad stopband photochemical catalyst, thus in the forbidden band, form impurity energy level, the catalyst band gap is narrowed down, can improve and produce hydrogen activity.
Summary of the invention
The objective of the invention is to, a kind of Ni doping Cd is provided 0.1Zn 0.9S mischcrystal photocatalyst and preparation method thereof, the photochemical catalyst of the present invention's preparation can improve the efficient of hydrogen production by water decomposition greatly.
In order to realize above-mentioned task, the present invention takes following technical scheme:
A kind of Ni doping Cd 0.1Zn 0.9S micron ball photocatalyst is characterized in that, the grain shape of the photochemical catalyst that makes is the micron ball of nanocrystalline composition, and wherein, the doping of Ni is 0.1%～0.5% of a catalyst weight.
Above-mentioned Ni doping Cd 0.1Zn 0.9The preparation method of S micron ball photocatalyst is characterized in that, carries out according to the following steps:
1) with zinc sulfate ZnSO 47H 2O, cadmium sulfate 3CdSO 48H 2O, nitric acid nickel (NO 3) 26H 2O and thioacetamide are dissolved in the deionized water according to stoichiometric proportion, form mixed solution;
2) mixed solution is transferred to respectively in the water heating kettle, is placed on 160 ℃ of following maintenances 8 hours in the baking oven after the sealing fully;
3) take out water heating kettle, naturally cool to room temperature;
4) product spends deionised water for several times, and is at room temperature dry in the vacuum drying chamber then, promptly obtains Ni doping Cd after grinding at last 0.1Zn 0.9S micron ball photocatalyst;
Ni doping Cd of the present invention 0.1Zn 0.9S micron ball photocatalyst produces hydrogen activity and is greatly enhanced.The even significant improvement of anti-photoetch ability in aerial anti-surface oxidation and the light-catalyzed reaction.In addition, the Ni doping Cd for preparing 0.1Zn 0.9The S photochemical catalyst is shaped as the micron ball of being made up of nanocrystalline, the existence of this micron ball can be greatly enhanced so that photochemical catalyst decomposes the aquatic products hydrogen activity at visible light photocatalysis, the highest hydrogen-producing speed is 191.01 μ mol/ (gh), and quantum efficiency reaches 6.77% at the 420nm place.Hydrogen-producing speed can reach 585.45 μ mol/ (gh) especially after carrying platinum, then is 15.9% in 420nm place quantum efficiency.The Ni doping Cd that this method is prepared 0.1Zn 0.9S micron ball photocatalyst has the characteristics of active height, good stability.
Description of drawings
Fig. 1 is different Ni doping Cd 0.1Zn 0.9The XRD figure of S micron ball photocatalyst;
Fig. 2 is different Ni doping Cd 0.1Zn 0.9The uv-visible absorption spectra figure of S micron ball photocatalyst;
Fig. 3 is different Ni doping Cd 0.1Zn 0.9The ESEM picture figure of S micron ball photocatalyst, wherein: (a) do not mix; (b) the Ni doping is 0.1wt%; (c) the Ni doping is 0.2wt%; (d) the Ni doping is 0.5wt%.
Fig. 4 is different Ni doping Cd 0.1Zn 0.9The N of S micron ball photocatalyst 2Suction-desorption isotherm.
Fig. 5 is visible light photocatalysis decomposition water experimental system figure;
Fig. 6 is different Ni doping Cd 0.1Zn 0.9The product hydrogen figure of S micron ball photocatalyst.Produce hydrogen condition: photochemical catalyst 0.2g, reactant liquor 200mL, light source 350W xenon lamp, optical filter 〉=420nm, sacrifice agent: 9.6g Na 2SO 3+ 2gNa 2S;
Fig. 7 is Ni doping per hour product hydrogen figure of photochemical catalyst behind the different amount of the load Pt when being 0.1wt%.
The embodiment that provides below in conjunction with accompanying drawing and inventor is described in further detail the present invention.
The specific embodiment
The present invention adopts the synthetic Ni doping Cd that obtains better crystallinity degree of hydro-thermal method 0.1Zn 0.9S micron ball photocatalyst, concrete processing step is as follows:
Embodiment 1:
1) takes by weighing ZnSO 47H 2O:5.17g, 3CdSO 48H 2O:0.51g, thioacetamide: 1.50g is dissolved in the 50mL deionized water, forms mixed solution;
2) mixed solution is transferred in the water heating kettle, is placed in the baking oven after the sealing fully, kept 8 hours with 160 ℃;
3) take out water heating kettle, naturally cool to room temperature;
4) product at room temperature places vacuum drying chamber dry, after grinding promptly obtains the not Cd of Ni doped by the deionized water washing for several times then 0.1Zn 0.9The S photochemical catalyst.
Embodiment 2:
1) takes by weighing ZnSO 47H 2O:5.17g, 3CdSO 48H 2O:0.51g, Ni (NO 3) 26H 2O:0.0102g, thioacetamide: 1.50g is dissolved in the 50mL deionized water, forms mixed solution;
2) mixed solution is transferred in the water heating kettle, is placed on 160 ℃ of following maintenances 8 hours in the baking oven after the sealing fully;
3) take out water heating kettle, naturally cool to room temperature;
4) product places vacuum drying chamber dry under room temperature by the deionized water washing for several times then, grinds at last.Can obtain the Cd that the Ni doping is 0.1wt% 0.1Zn 0.9S photochemical catalyst, its grain shape are the micron ball of nanocrystalline composition.
Embodiment 3:
1) takes by weighing ZnSO 47H 2O:5.17g, 3CdSO 48H 2O:0.51g, Ni (NO 3) 26H 2O:0.0203g, thioacetamide: 1.50g is dissolved in the 50mL deionized water, forms mixed solution;
2) mixed solution is transferred in the water heating kettle, is placed on 160 ℃ of following maintenances 8 hours in the baking oven after the sealing fully;
3) take out water heating kettle, naturally cool to room temperature;
4) product places vacuum drying chamber dry under room temperature, after grinding promptly obtains the Cd that the Ni doping is 0.2wt% by the deionized water washing for several times then 0.1Zn 0.9S photochemical catalyst, its grain shape are the micron ball of nanocrystalline composition.
Embodiment 4:
1) takes by weighing ZnSO 47H 2O:5.17g, 3CdSO 48H 2O:0.51g, Ni (NO 3) 26H 2O:0.0509g, thioacetamide: 1.50g is dissolved in the 50mL deionized water, forms mixed solution;
2) mixed solution is transferred to respectively in the water heating kettle, sealing back fully kept 8 hours under 160 ℃ in baking oven;
3) take out water heating kettle, naturally cool to room temperature;
4) product places vacuum drying chamber dry under room temperature, after grinding promptly obtains the Cd that the Ni doping is 0.5wt% by the deionized water washing for several times then 0.1Zn 0.9S photochemical catalyst, its grain shape are the micron ball of nanocrystalline composition.
The all right exclusive list of the foregoing description needs only the scope that provides in the present invention, all can make the Cd that Ni mixes 0.1Zn 0.9The S mischcrystal photocatalyst experiment showed, that through the applicant parameter that embodiment 2 provides is optimal selection.
Fig. 1 has provided different Ni doping Cd 0.1Zn 0.9The X-ray diffractogram (XRD) of S micron ball photocatalyst, used instrument are X ' the Pert PRO X-ray diffractometer of Dutch PANalytical company.As seen from the figure, the Cd of each doping 0.1Zn 0.9The S photochemical catalyst all possesses good crystal formation.
Fig. 2 is different Ni doping Cd 0.1Zn 0.9The uv-visible absorption spectra figure (UV-Vis) of S micron ball photocatalyst, used instrument are the U4100 type spectrophotometers of Japanese Hitachi company.As can be seen from the figure, the ABSORPTION EDGE of each photochemical catalyst and moves to the long wave direction along with the increase of Ni doping all about 550nm.This result proves Ni 2+Cd well mixes 0.1Zn 0.9In the lattice of S.
Fig. 3 has provided different Ni doping Cd 0.1Zn 0.9The ESEM picture of S micron ball photocatalyst (SEM, the JEOL JSM-6700FE of company of NEC type field emission scanning electron microscope).By Fig. 3 a as seen, the Cd of Ni doped not 0.1Zn 0.9S is the irregular group that is made up of nano particle.And the spherical that all can see many micron order sizes among Fig. 3 b, 3c and the 3d forms, and wherein the micron ball size homogeneous among Fig. 3 b is about 5 μ m, and the micron ball size differences among other two figure is very big.This explanation is to the optimum N i doping that is formed with of micron ball.
Fig. 4 provides different Ni doping Cd 0.1Zn 0.9The N of S micron ball photocatalyst 2Suction-desorption isotherm, this result is by U.S.'s Beckman Coulter SA3100 plus specific surface and aperture analysis-e/or determining.Can see by figure, return the ring that stagnates and appear at the higher zone of relative pressure, belong to the IV type H1 class suction-desorption curve of typical IUPAC (IUPAC) regulation.BET result of calculation shows 0.0wt%, 0.1wt%, 0.2wt% and 0.5wt%Ni-Cd 0.1Zn 0.9The specific area of S photochemical catalyst is respectively 8.60m 2/ g, 28.84m 2/ g, 15.93m 2/ g and 10.79m 2/ g.As seen Ni 2+Mix and can effectively increase the specific area of photochemical catalyst, and mix the Ni amount and be 0.1wt% time specific surface area of catalyst maximum.
Platinum (Pt) can greatly improve whole system photocatalysis hydrogen-producing speed as co-catalyst.Adopt photoreduction met hod that Pt is loaded on the cadmium sulfide surface in the experiment, the photo-reduction process does not add optical filter, adopts UV-irradiation.The concrete Pt step of carrying is as follows:
1. in reactor, add the 0.2g photochemical catalyst; 9.6g Na 2SO 3, 2g Na 2S is as sacrifice agent; The 200mL deionized water; Add a certain amount of H 2PtCl 66H 2O (Pt source);
2. logical nitrogen purges 10min in the illumination forward reaction device, with the oxygen in the system of removing;
3. open the electric fan in the xenon lamp device, drive magnetic stirring apparatus;
4. open xenon lamp power supply;
5. behind the photo-reduction 1h, close xenon lamp.
It below is the concrete confirmatory experiment that the inventor provides.
1. hydrogen performance evaluation is produced in photocatalysis
The Ni doping Cd of the present invention's preparation 0.1Zn 0.9S micron ball photocatalyst, the test and validation experiment of all relevant visible light photocatalysis hydrogen production by water decomposition performances is all finished in experimental system shown in Figure 5, experimental system mainly comprises following components: pyrex (Pyrex) glass reactor, magnetic stirring apparatus, cut-off type optical filter (λ 〉=420nm) and 350W xenon lamp device.350W xenon lamp device mainly comprises an xenon lamp control cabinet, a 350W xenon lamp, a reflective tile and a small electric fan.Because xenon lamp work the time can follow a large amount of heat to emit, to carry out air-cooledly so the rear portion has installed an electric fan additional, the temperature constant of practical measurement light-catalyzed reaction system is at 35 ± 5 ℃.
Concrete experimental procedure is:
1) in reactor, adds Ni doping Cd 0.1Zn 0.9S micron ball photocatalyst: 0.2g, sacrifice agent Na 2SO 3: 9.6g+Na 2S:2g, the 200mL deionized water;
2) logical nitrogen purges 10min in the illumination forward reaction device, with the oxygen in the system of removing;
3) add optical filter, open the electric fan in the xenon lamp device, drive magnetic stirring apparatus;
4) open xenon lamp power supply;
5) behind the reaction certain hour, in reactor, get 100 μ L gases and be expelled to and carry out gas composition and constituent analysis (the SP-2100 type gas chromatograph that the BeiFen Instrument Techogy Co., Ltd., BeiJing City produces, TCD detector, 5A molecular sieve column) in the gas chromatograph.
Fig. 6 has provided each photochemical catalyst visible light photocatalysis product hydrogen result when not carrying Pt, and as seen from the figure, the Ni doping of the present invention's preparation is that the product hydrogen activity and the stability of the photochemical catalyst of 0.1wt% all is better than other three, and producing hydrogen is 191.01 μ mol/ (gh).After its photo-reduction supporting Pt, the Ni doping Cd of this method preparation 0.1Zn 0.9S micron ball photocatalyst produces hydrogen activity and improves more obviously (Fig. 7), and the Pt of load 0.6wt% reaches the highest, and producing hydrogen is 585.45 μ mol/ (gh), during for supporting Pt not 3 times.
2. catalyst efficiency evaluation
The product hydrogen meter of light-catalyzed reaction is seen quantum efficiency and is calculated by following formula:
Figure G200710018881XD00081
The quantum efficiency of catalyst photocatalysis hydrogen production adopts single line light method to measure.The 350W xenon source installs the single line light that dominant wavelength is the logical type optical filter acquisition of band 420 ± 5nm of 420nm additional.(photoelectric instrument factory of Beijing Normal University produces, and model is: (λ: 400-1000nm) probe records add 350W xenon lamp behind the 420nm bandpass filter average to see through unit light intensity is W=1.598mW/cm the UV-B type) subsidiary FZ-A type to use the light intensity irradiatometer 2. because of effective irradiated area of reactor is A=π R 2=π * 2 2=12.56cm 2Can be regarded as on average by Q=WA is Q=20.07mW through luminous energy.Adopting the logical type optical filter of 420nm band to do photocatalysis with the 350W xenon lamp and produce the hydrogen test, is 8.5876 μ mol/h when recording hydrogen-producing speed and not carrying Pt, and carrying behind the 0.6wt%Pt is 20.19 μ mol/h.After installing the logical type optical filter of band additional, because of only having the photon of 420 ± 5nm scope, xenon source can see through, and light intensity greatly reduces, so hydrogen output produces hydrogen than all band light source that adopts the cut-off type optical filter to obtain λ 〉=420nm obvious decline is arranged.By following formula calculate not during supporting Pt the Ni doping be the Cd of 0.1wt% 0.1Zn 0.9The S photochemical catalyst is 6.77% in the 420nm place sub-efficient of hydrogen output.And the quantum efficiency of this photochemical catalyst is 15.9% behind the load 0.6wt%Pt.

Claims (2)

1. Ni doping Cd 0.1Zn 0.9S micron ball photocatalyst is characterized in that, the grain shape of the photochemical catalyst that makes is the micron ball of nanocrystalline composition, and wherein, the doping of Ni is 0.1%～0.5% of a catalyst weight.
2. the described Ni doping of claim 1 Cd 0.1Zn 0.9The preparation method of S micron ball photocatalyst is characterized in that, carries out according to the following steps:
1) with zinc sulfate ZnSO 47H 2O, cadmium sulfate 3CdSO 48H 2O, nitric acid nickel (NO 3) 26H 2O and thioacetamide are dissolved in the deionized water according to stoichiometric proportion, form mixed solution;
2) mixed solution is transferred to respectively in the water heating kettle, is placed on after the sealing fully in the baking oven with 160 ℃ of maintenances 8 hours;
3) take out water heating kettle, naturally cool to room temperature;
4) product is washed for several times by deionized water, and is at room temperature dry in vacuum drying chamber then, after promptly obtain the Cd that Ni mixes after grinding 0.1Zn 0.9The S mischcrystal photocatalyst.
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