CN101254467A - Precipitating-hydrothermal preparation with high visible light catalytic activity nano CdxZn1-xS photocatalyst - Google Patents
Precipitating-hydrothermal preparation with high visible light catalytic activity nano CdxZn1-xS photocatalyst Download PDFInfo
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- CN101254467A CN101254467A CNA2008100603785A CN200810060378A CN101254467A CN 101254467 A CN101254467 A CN 101254467A CN A2008100603785 A CNA2008100603785 A CN A2008100603785A CN 200810060378 A CN200810060378 A CN 200810060378A CN 101254467 A CN101254467 A CN 101254467A
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Abstract
The invention discloses a deposition-hydrothermal method for preparing a nano-sized CdxZn<1-x>S photocatalyst with high visible-light photocatalytic activity. The method includes the following steps: 1) adding dropwise a mixed solution of cadmium nitrate and zinc nitrate into a sodium sulfide solution, stirring at a medium rate for 0.5-3 hours, maintaining the temperature at 10-40 DEG C to obtain a nano-sized powdery precursor precipitate; 2) placing the nano-sized powdery precursor precipitate in a reaction vessel, raising the temperate at a rate of 1-5 DEG C/min up to 150-240 DEG C, maintaining the temperature, allowing hydrothermal reactions for 12-24 hours, stopping the hydrothermal reactions, naturally cooling down to room temperature, taking out the reaction products, washing with the deionized water and the anhydrous alcohol for 3-4 times, drying at 50-80 DEG C in a vacuum drying oven to obtain a solid solution of nano-sized CdxZn<1-x>S photocatalyst. The production method is carried out in water phase with easy operation and low cost. The product has uniform distribution of particle size, the forbidden band width and optical properties thereof are controlled by changing components, and the product has high visible-light photocatalytic activity and good prospects in industrial application.
Description
Technical field
The present invention relates to a kind of nanometer Cd that forms solid solution
xZn
1-xPrecipitation-the hydrothermal preparing process of S photochemical catalyst, this powder possesses high visible light catalytic activity.
Background technology
In recent decades, because environmental pollution and energy crisis are on the rise, people have carried out extensive studies for the environmental protection treatment technology of exploring novel practical.The conductor photocatalysis technology provides opportunity for the solution of this problem, and wherein studying many is titanium dioxide.Because TiO
2Energy gap big (Eg ≈ 3.0-3.2ev), its absorption spectrum be in the black light district (λ＜400nm), low to the utilization rate of sunshine, be necessary the photochemical catalyst of development of new.
Semi-conductor nano particles causes that recently the binary sulphur of people's very big concern, especially second family is the research of metallic compound.Mainly be because it has nonlinear optics and fluorescent effect, quantum size effect and some other important physics and chemical property.
Ternary compound Cd
xZn
1-xS is by changing its chemical composition, and it absorbs band edge can be extended to green glow from ultraviolet light, therefore can obtain continuously adjustable optical property.Cd
xZn
1-xS as the catalyst of photocatalysis Decomposition aquatic products hydrogen under a kind of visible light, also can be applied to highdensity optical recording and short-wave laser diode, Cd
xZn
1-xThe S film is obtaining application widely as the broad-band gap window material aspect heterojunction solar battery and the photoconductive device.Because Cd
xZn
1-xThe S energy gap can be regulated and control along with chemical composition, will be a kind of potentiality material that has higher catalytic activity under visible light.
Current C d
xZn
1-xThe method that adopts for preparing that S is nanocrystalline has: sintering process, hydro-thermal method, microemulsion method, organic solvent high-temperature synthesis.Obviously, the system dispersing uniformity poor, need starvation, high temperature crystallization, poisonous reagent or complicated shortcomings such as synthesis device to make Cd by these methods preparations
xZn
1-xThe S photochemical catalyst has unstable properties, production technology is difficult to shortcomings such as control and cost height, has limited it to promote the use of, therefore must the new preparation technology of exploitation.
Summary of the invention
The object of the invention provide a kind of easy, have a high visible light catalytic activity nano Cd reliably, cheaply
xZn
1-xPrecipitation-the hydrothermal preparing process of S photochemical catalyst.
Comprise the steps:
1) nano-powder forerunner precipitated liquid preparation:
The mixed solution that will contain cadmium nitrate, zinc nitrate dropwise adds in the sodium sulfide solution, and middling speed stirs 0.5～3h, and mixeding liquid temperature is 10 ℃～40 ℃, obtains nano-powder pioneer precipitated liquid;
2) preparation of nano-powder under the hydrothermal condition:
Above-mentioned nano-powder pioneer precipitated liquid is put into reactor, be warming up to 150～240 ℃ of insulations with the speed of 1～5 ℃/min and carry out hydro-thermal reaction, after 12～24h reaction, stop heating, the question response still takes out after being as cold as room temperature naturally, with deionized water and absolute ethanol washing 3～4 times, put into vacuum drying chamber in 50～80 ℃ of dryings, obtain forming the nanometer Cd of solid solution
xZn
1-xThe S photochemical catalyst.
Zinc nitrate in the described step 1): the mol ratio of cadmium nitrate is 1: (0.1～3), cadmium nitrate+zinc nitrate: the mol ratio of vulcanized sodium is 1: (1～1.2), the concentration of cadmium nitrate are 10
-5～10
-1Every liter of mole.
The beneficial effect that the present invention has:
1, the nanometer Cd that under precipitation-hydrothermal condition, synthesizes
xZn
1-xThe S homogeneous grain diameter forms the solid solution structure, and cadmium ion enters into the ZnS lattice;
2, by selecting suitable composition and preparation condition, can control the composition ratio and the grain size of solid solution, obtain energy gap and optical property according to the adjustable Cd of composition
xZn
1-xThe nano-powder of S;
3, nanometer Cd
xZn
1-xThe preparation technology of S is simple, and cost is low;
4, have high visible light catalytic activity, greatly improved the solar energy utilization ratio, the organic pollution of certain kind of effectively degrading.
Description of drawings
Fig. 1 is nano-photocatalyst Cd among the embodiment 1
0.15Zn
0.85The SEM picture of S;
Fig. 2 is nano-photocatalyst Cd
xZn
1-xThe diffuse reflectance spectra of S (a → f:x=0,0.15,0.25,0.5,0.75,1).
The specific embodiment
Elaborate below in conjunction with embodiment:
Has high visible light catalytic activity nano Cd
xZn
1-xPrecipitation-the hydrothermal preparing process of S photochemical catalyst is to utilize first post precipitation hydrothermal condition to prepare the method for nano-powder, use inorganic salts such as cadmium nitrate, zinc nitrate, vulcanized sodium to be raw material, obtained being uniformly dispersed, energy gap and optical property with composition adjustable and have a high visible light catalytic activity nano Cd
xZn
1-xThe S powder.
The mixed solution that will contain 0.0075mol cadmium nitrate and 0.0425mol zinc nitrate splashes in the solution that contains 0.06mol vulcanized sodium gradually, overall solution volume is remained on about 80ml, mixeding liquid temperature is 10 ℃, behind the stirring 1.5h, obtains nano-powder pioneer precipitation;
Above-mentioned nano-powder pioneer precipitation is put into reactor, be warming up to 180 ℃ of insulations with the speed of 1 ℃/min and carry out hydro-thermal reaction, after the 24h reaction, stop heating, the question response still takes out after being as cold as room temperature naturally, with deionized water and absolute ethanol washing 3 times, put into vacuum drying chamber in 80 ℃ of dryings, obtained forming the nanometer Cd of solid solution
xZn
1-xThe S photochemical catalyst.
This nanometer Cd
xZn
1-xThe S photochemical catalyst is to consist of Cd
0.15Zn
0.85The solid solution of S.We are set at the catalytic organism object with the methyl orange solution of the 20mg/L of 10ml, are catalyst with the powder 20mg of above-mentioned preparation, are light source with the German Ou Silang HQI-BT 400W/D of company metal halide lamp, have carried out the photocatalysis experiment.
X-ray diffraction analysis (XRD) shows: gained Cd
xZn
1-xThe S nano-powder is a zincblende lattce structure; At visible light according to (after carrying out the photocatalytic degradation experiment of 60min under the λ＞400nm), finding nanometer Cd
xZn
1-xThe S powder can reach 96% to the degradation rate of methyl orange.Illustrated that the cadmium doping reduces the energy gap of zinc sulphide, makes its absorption spectrum red shift to visible region, thereby can degrade to organic matter under visible light.
Embodiment 2
The mixed solution that will contain 0.005mol cadmium nitrate and 0.045mol zinc nitrate splashes in the solution that contains 0.06mol vulcanized sodium gradually, and overall solution volume is remained on about 80ml, and mixeding liquid temperature is 40 ℃, behind the stirring 2.5h, obtains nano-powder pioneer precipitation;
Above-mentioned nano-powder pioneer precipitation is put into reactor, be warming up to 200 ℃ of insulations with the speed of 5 ℃/min and carry out hydro-thermal reaction, after the 20h reaction, stop heating, the question response still takes out after being as cold as room temperature naturally, with deionized water and absolute ethanol washing 3 times, put into vacuum drying chamber in 80 ℃ of dryings, obtained forming the nanometer Cd of solid solution
xZn
1-xThe S photochemical catalyst.Get off to test its photocatalysis performance with experiment condition identical among the embodiment 1.
Compare with P25 (Degussa), obtained the photocatalysis effect similar to embodiment 1.
Embodiment 3
The mixed solution that will contain 0.00625mol cadmium nitrate and 0.01875mol zinc nitrate splashes in the solution that contains 0.025mol vulcanized sodium gradually, overall solution volume is remained on about 80ml, mixeding liquid temperature is 15 ℃, behind the stirring 3h, obtains nano-powder pioneer precipitation;
Above-mentioned nano-powder pioneer precipitation is put into reactor, be warming up to 240 ℃ of insulations with the speed of 2 ℃/min and carry out hydro-thermal reaction, after the 12h reaction, stop heating, the question response still takes out after being as cold as room temperature naturally, with deionized water and absolute ethanol washing 3 times, put into vacuum drying chamber in 50 ℃ of dryings, obtained forming the nanometer Cd of solid solution
xZn
1-xThe S photochemical catalyst.Get off to test its photocatalysis performance with experiment condition identical among the embodiment 1.
Compare with P25 (Degussa), obtained the photocatalysis effect similar to embodiment 1.
Embodiment 4
The mixed solution that will contain 0.00625mol cadmium nitrate and 0.01875mol zinc nitrate splashes in the solution that contains 0.03mol vulcanized sodium gradually, overall solution volume is remained on about 80ml, mixeding liquid temperature is 25 ℃, behind the stirring 0.5h, obtains nano-powder pioneer precipitation;
Above-mentioned nano-powder pioneer precipitation is put into reactor, be warming up to 200 ℃ of insulations with the speed of 2 ℃/min and carry out hydro-thermal reaction, after the 18h reaction, stop heating, the question response still takes out after being as cold as room temperature naturally, with deionized water and absolute ethanol washing 4 times, put into vacuum drying chamber in 60 ℃ of dryings, obtained forming the nanometer Cd of solid solution
xZn
1-xThe S photochemical catalyst.Get off to test its photocatalysis performance with experiment condition identical among the embodiment 1.
Compare with P25 (Degussa), obtained the photocatalysis effect similar to embodiment 1.
Embodiment 5
The mixed solution that will contain 0.01875mol cadmium nitrate and 0.00625mol zinc nitrate splashes in the solution that contains 0.0285mol vulcanized sodium gradually, overall solution volume is remained on about 80ml, mixeding liquid temperature is 15 ℃, behind the stirring 2.5h, obtains nano-powder pioneer precipitation;
Above-mentioned nano-powder pioneer precipitation is put into reactor, be warming up to 150 ℃ of insulations with the speed of 5 ℃/min and carry out hydro-thermal reaction, after the 22h reaction, stop heating, the question response still takes out after being as cold as room temperature naturally, with deionized water and absolute ethanol washing 4 times, put into vacuum drying chamber in 60 ℃ of dryings, obtained forming the nanometer Cd of solid solution
xZn
1-xThe S photochemical catalyst.Get off to test its photocatalysis performance with experiment condition identical among the embodiment 1.
Compare with P25 (Degussa), obtained the photocatalysis effect similar to embodiment 1.
Claims (2)
1. one kind has high visible light catalytic activity nano Cd
xZn
1-xPrecipitation-the hydrothermal preparing process of S photochemical catalyst is characterized in that comprising the steps:
1) nano-powder forerunner precipitated liquid preparation:
The mixed solution that will contain cadmium nitrate, zinc nitrate dropwise adds in the sodium sulfide solution, and middling speed stirs 0.5～3h, and mixeding liquid temperature is 10 ℃～40 ℃, obtains nano-powder pioneer precipitated liquid;
2) preparation of nano-powder under the hydrothermal condition:
Above-mentioned nano-powder pioneer precipitated liquid is put into reactor, be warming up to 150～240 ℃ of insulations with the speed of 1～5 ℃/min and carry out hydro-thermal reaction, after 12～24h reaction, stop heating, the question response still takes out after being as cold as room temperature naturally, with deionized water and absolute ethanol washing 3～4 times, put into vacuum drying chamber in 50～80 ℃ of dryings, obtain forming the nanometer Cd of solid solution
xZn
1-xThe S photochemical catalyst.
2. a kind of high visible light catalytic activity nano Cd that has according to claim 1
xZn
1-xPrecipitation-the hydrothermal preparing process of S photochemical catalyst is characterized in that the zinc nitrate in the described step 1): the mol ratio of cadmium nitrate is 1: (0.1～3), cadmium nitrate+zinc nitrate: the mol ratio of vulcanized sodium is 1: (1～1.2), the concentration of cadmium nitrate are 10
-5～10
-1Every liter of mole.
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