CN103708532A - Dendritic cadmium sulfide superfine nanorod grade structural material and preparation method thereof - Google Patents
Dendritic cadmium sulfide superfine nanorod grade structural material and preparation method thereof Download PDFInfo
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- CN103708532A CN103708532A CN201410008447.3A CN201410008447A CN103708532A CN 103708532 A CN103708532 A CN 103708532A CN 201410008447 A CN201410008447 A CN 201410008447A CN 103708532 A CN103708532 A CN 103708532A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a dendritic cadmium sulfide superfine nanorod grade structural material and a preparation method thereof. The preparation method comprises the following steps: firstly, enabling zinc nitrate and thiourea to react in a mixed solvent of ethanediamine and water for 8-10 hours at 150-200 DEG C to obtain zinc sulfide hybrid nanosheets; dispersing the zinc sulfide hybrid nanosheets in ethanediamine, and adding water and cadmium chloride to react for 3-6 hours at 120-200 DEG C to obtain the cadmium sulfide superfine nanorod grade structural material. The preparation method is simple in process and low in cost due to the adoption of an ion exchange hydrothermal synthesis method; the prepared dendritic CdS (cadmium sulfide) nanorod is 80-150 nanometers in length and 8-15 nanometers in diameter and has favorable catalytic performance.
Description
Technical field
The present invention relates to semiconductor nano material technical field, more particularly, relate to about dendritic cadmium sulfide superfine nano rod hierarchical organization material and preparation method thereof.
Background technology
Fossil energy shortage and problem of environmental pollution are the significant challenge that current mankind faces.Hydrogen Energy is considered to have one of clean energy of development potentiality most in future source of energy structure.Traditional hydrogen production process need to consume huge conventional energy resources, and hydrogen manufacturing cost is improved greatly, has greatly limited the development of Hydrogen Energy and has applied.If can effectively utilize sun power to carry out photolysis water hydrogen, the development of the Hydrogen Energy of just can making greater efforts to promote, likely fundamentally solves energy shortage and the environmental problem of facing mankind.
Japanese scholars Fujishima in 1972 and Hondo find illumination TiO
2can the hydrogen manufacturing of catalytic decomposition water, opened new era of conductor photocatalysis hydrogen manufacturing.Semi-conductor is the material of a kind of conductivity between conductor and isolator, has a very large application photocatalysis Decomposition is waterborne.In recent years, II-VI semiconductor material can be used as photoelectric material, sensor material etc., thereby had been subject to paying close attention to widely.Cadmium Sulfide is as a member in this based semiconductor material, with traditional TiO
2, the metal oxide wide bandgap semiconductor photocatalyst such as ZnO compares, it is because having suitable band gap and applicable valence band and conduction band position is considered to good visible light catalyst.Development along with nanotechnology, the Cadmium Sulfide of various patterns is constantly synthesized out, and comparing of dendritic Cadmium Sulfide report is less, and the method for the synthetic dendritic cadmium sulfide of report is mainly by adding cadmium salt, thiocarbamide and a kind of modifier at present, adopt one step hydro thermal method to synthesize.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of low cost, less energy-consumption, technique simply to prepare the method for dendritic cadmium sulfide superfine nano rod hierarchical organization, the mol ratio of final nano-scale structure two components that generate reaches equimolar ratio example substantially.
Technical purpose of the present invention is achieved by following technical proposals:
Dendritic cadmium sulfide superfine nano rod hierarchical organization material and preparation method thereof, is prepared according to following step:
In technical scheme of the present invention, after step 2 reaction finishes, remove supernatant liquid, collect yellow mercury oxide, use second alcohol and water centrifuge washing 4-6 time, be finally placed in 40 ℃ of vacuum drying ovens dry 12 hours, obtain cadmium sulfide nano hierarchical organization material.
The length of the dendritic cadmium sulfide superfine nano rod hierarchical organization material of preparing according to aforesaid method is in 80-150 nanometers, and diameter is 8-15 nanometers.
Chemical reagent used in the present invention is analytical pure, the reaction vessel that utilizes autoclave to use as step 1 and step 2, and general employing be take the reactor that tetrafluoroethylene is liner.
Described dendritic cadmium sulfide superfine nano rod hierarchical organization material produces the application in hydrogen in catalysis, wherein uses the reaction soln being comprised of water, dehydrated alcohol and triethylamine, and the volume ratio of described water, dehydrated alcohol and triethylamine is 15:15:2.
What preparation method's technical scheme of Cadmium Sulfide superfine nano hierarchical organization material of the present invention adopted is two one-step hydrothermals, has the advantages such as cost is low, synthesis temperature is low, product purity is high, specific surface is large, product hydrogen performance is good.Technical scheme of the present invention is from hybridized nanometer sheet, by ion exchange method, synthesizes dendritic Cadmium Sulfide superfine nano rod hierarchical organization material, has a very excellent performance photocatalysis Decomposition is waterborne.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the zinc sulphide hybridized nanometer sheet of step 1 preparation.
Fig. 2 is the SEM photo of the cadmium sulfide nano-stick hierarchical organization material prepared by the present invention.
Fig. 3 is the TEM photo of the cadmium sulfide nano-stick hierarchical organization material prepared by the present invention.
Fig. 4 is the X-ray diffractogram of the zinc sulphide hybridized nanometer sheet of step 1 preparation.
Fig. 5 is the cadmium sulfide nano-stick hierarchical organization material prepared by the present invention and the ultraviolet-visible light comparison diagram of cadmium sulfide nanoparticles, and wherein 1 is the prepared Cadmium Sulfide of the present invention; The 2 Cadmium Sulfide particles of preparing for reference literature.
Fig. 6 is the sample hydrogen output of 5 milligrams and the graph of a relation of light application time, and wherein 1 is the prepared Cadmium Sulfide of the present invention; The 2 Cadmium Sulfide particles of preparing for reference literature.
Embodiment
Below in conjunction with specific embodiment, further illustrate technical scheme of the present invention.
Embodiment 1:
1. raw material: analytical pure quadrol, thiocarbamide, zinc nitrate hexahydrate, five aquation Cadmium Sulfides.
2. get respectively quadrol and water (totally 18 milliliters, volume ratio is 4:1) in 50 milliliters of autoclaves, magnetic agitation 10 minutes.
3. in the mixed solution stirring, add 1.5mmol zinc nitrate hexahydrate, at room temperature magnetic agitation is to clarification.
4. in the mixing solutions of clarification, add 1.5mmol thiocarbamide, magnetic agitation was placed in 180 ℃ of baking ovens 10 hours by its sealing after 20 minutes.Reactor is taken out and naturally cools to room temperature, and reacted product autoreaction still is transferred to centrifuge tube, and water carries out centrifugation and supersound washing to product, repeats 4 times, obtains pure organic-inorganic hybrid nanometer sheet.
5. the organic-inorganic hybrid nanometer sheet of preparation is dispersed in 28.8 milliliters of quadrols again to ultrasonic 10 minutes.
6. get 4.8 milliliters of dispersion liquids in 50 milliliters of autoclaves, then add therein 13.2 ml waters, magnetic agitation 10 minutes.
7. add 0.6mmol Cadmium chloride fine powder, magnetic agitation was placed in 160 ℃ of baking ovens 6 hours by its sealing after 20 minutes.Reactor is taken out and naturally cools to room temperature, and product autoreaction still is transferred to centrifuge tube, and water and ethanol carry out centrifugation and supersound washing to product, repeat 4 times, is placed in 40 ℃ of vacuum drying ovens dry 12 hours, obtains target product.
Embodiment 2:
1. raw material: analytical pure quadrol, thiocarbamide, zinc nitrate hexahydrate, five aquation Cadmium Sulfides.
2. get respectively quadrol and water (totally 18 milliliters, volume ratio is 4:1) in 50 milliliters of autoclaves, magnetic agitation 10 minutes.
3. in the mixed solution stirring, add 1.5mmol zinc nitrate hexahydrate, at room temperature magnetic agitation is to clarification.
4. in the mixing solutions of clarification, add 1.5mmol thiocarbamide, magnetic agitation was placed in 180 ℃ of baking ovens 10 hours by its sealing after 20 minutes.Reactor is taken out and naturally cools to room temperature, and product autoreaction still is transferred to centrifuge tube, and water carries out centrifugation and supersound washing to product, repeats 4 times, obtains pure organic-inorganic hybrid nanometer sheet.
5. the organic-inorganic hybrid nanometer sheet of preparation is dispersed in 14.4 milliliters of quadrols again to ultrasonic 10 minutes.
6. get 2.4 milliliters of dispersion liquids in 50 milliliters of autoclaves, then add therein 15.6 ml waters, magnetic agitation 10 minutes.
7. add 0.6mmol Cadmium chloride fine powder, magnetic agitation was placed in 160 ℃ of baking ovens 6 hours by its sealing after 20 minutes, reactor is taken out and naturally cools to room temperature, reacted product autoreaction still is transferred to centrifuge tube, water and ethanol carry out centrifugation and supersound washing to product, repeat 4 times, be placed in 40 ℃ of vacuum drying ovens dry 12 hours, obtain target product.
Embodiment 3:
1. raw material: analytical pure quadrol, thiocarbamide, zinc nitrate hexahydrate, five aquation Cadmium Sulfides.
2. get respectively quadrol and water (totally 18 milliliters, volume ratio is 4:1) in 50 milliliters of autoclaves, magnetic agitation 10 minutes.
3. in the mixed solution stirring, add 1.5mmol zinc nitrate hexahydrate, at room temperature magnetic agitation is to clarification.
4. in the mixing solutions of clarification, add 1.5mmol thiocarbamide, magnetic agitation was placed in 180 ℃ of baking ovens 10 hours by its sealing after 20 minutes.Reactor is taken out and naturally cools to room temperature, and reacted product autoreaction still is transferred to centrifuge tube, and water carries out centrifugation and supersound washing to product, repeats 4 times, obtains pure organic-inorganic hybrid nanometer sheet.
5. the organic-inorganic hybrid nanometer sheet of preparation is dispersed in 28.8 milliliters of quadrols again to ultrasonic 10 minutes.
6. get 19.2 milliliters of dispersion liquids in 150 milliliters of autoclaves, then add therein 52.8 ml waters, magnetic agitation 10 minutes.
7. add 1.8mmol gram of Cadmium chloride fine powder, magnetic agitation was placed in 160 ℃ of baking ovens 6 hours by its sealing after 20 minutes, reactor is taken out and naturally cools to room temperature, product autoreaction still is transferred to centrifuge tube, water and ethanol carry out centrifugation and supersound washing to product, repeat 4 times, be placed in 40 ℃ of vacuum drying ovens dry 12 hours, obtain target product.
Embodiment 4:
Step is with example 1, and difference is in the 7th step it is that autoclave is placed at 200 ℃, baking oven and takes out and be cooled to room temperature after 3 hours, and other reaction conditionss all remain unchanged, and acquired results is close to example 1 acquired results.
Embodiment 5:
Step is with example 1, and difference is in the 7th step it is that autoclave is placed at 120 ℃, baking oven and takes out and be cooled to room temperature after 6 hours, and other reaction conditionss all remain unchanged, and acquired results is close to example 1 acquired results.
Utilize XRD to test zinc sulphide hybridized nanometer sheet, as shown in Figure 4, by with document (small, 2005,1, No.3,320 – 325) contrast, synthesized be the nanometer sheet precursor of ZnS really.
Utilize EDX to analyze the cadmium sulfide nano-stick hierarchical organization material of preparing by the present invention, result is as shown in the table, and known S, Cd than on keep equimolar ratio substantially at atomic molar.
| ? | S | Cd |
| Atomic percent/% | 48.52 | 51.48 |
Reference literature (J.Catal.266 (2009), 165) synthesizing cadmium sulfide particle, then the nano particle of using respectively the prepared sample of the present invention (above-described embodiment) and reference literature to prepare is done Photocatalyzed Hydrogen Production test.Concrete steps are as follows: take 5 milligrams of samples and add in photolysis pond (band water-cooling jacket), then add respectively 15 ml waters, 15 milliliters of dehydrated alcohols and 2 milliliters of triethylamines, stir.The first oxygen of the nitrogen of logical 30 minutes to go out wherein before illumination, reaction pressure maintains 1 normal atmosphere, temperature of reaction remains on 20-30 degree Celsius, by gas-chromatography, detect online hydrogen, can find no matter be ultraviolet-visible light comparison diagram, or hydrogen output comparison diagram, prepared sample of the present invention is obviously better than Cadmium Sulfide particle.
Above the present invention has been done to exemplary description; should be noted that; in the situation that not departing from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (10)
1. dendritic cadmium sulfide superfine nano rod hierarchical organization material, is characterized in that, the length of described dendritic cadmium sulfide superfine nano rod hierarchical organization material is in 80-150 nanometers, and diameter is 8-15 nanometers, according to following step, is prepared:
Step 1, zinc nitrate and thiocarbamide are placed in to the mixed solvent being comprised of quadrol and water, the mol ratio of wherein said zinc nitrate and thiocarbamide is 1:(1-1.2), the volume ratio of described quadrol and water is (3-4): 1, to be mixedly seal after evenly, at 150-200 ℃, react 8-10h, obtain zinc sulphide hybridized nanometer sheet;
Step 2, after the zinc sulphide hybridized nanometer sheet of step 1 preparation is dispersed in quadrol, add again water to carry out twice dispersing, then add Cadmium chloride fine powder, to be mixedly seal after evenly, at 120-200 ℃, react 3-6 hour, in the thiocarbamide using in element cadmium and step 1 in wherein said Cadmium chloride fine powder, the mol ratio of elementary sulfur is equimolar ratio.
2. dendritic cadmium sulfide superfine nano according to claim 1 rod hierarchical organization material, is characterized in that, in described step 1, to be mixedly seals after evenly, preferably reacts at 180-200 ℃.
3. dendritic cadmium sulfide superfine nano according to claim 1 rod hierarchical organization material, is characterized in that, in described step 2, to be mixedly seals after evenly, preferably reacts 4-5 hour at 150-180 ℃.
4. according to the dendritic cadmium sulfide superfine nano rod hierarchical organization material one of claim 1-3 Suo Shu, it is characterized in that, after step 2 reaction finishes, remove supernatant liquid, collect yellow mercury oxide, with second alcohol and water centrifuge washing 4-6 time, be finally placed in 40 ℃ of vacuum drying ovens dry 12 hours, obtain cadmium sulfide nano hierarchical organization material.
5. according to the dendritic cadmium sulfide superfine nano rod hierarchical organization material one of claim 1-3 Suo Shu, it is characterized in that, the reaction vessel that utilizes autoclave to use as step 1 and step 2, general employing be take the reactor that tetrafluoroethylene is liner.
6. the preparation method of dendritic cadmium sulfide superfine nano rod hierarchical organization material, is characterized in that, according to following step, is prepared:
Step 1, zinc nitrate and thiocarbamide are placed in to the mixed solvent being comprised of quadrol and water, the mol ratio of wherein said zinc nitrate and thiocarbamide is 1:(1-1.2), the volume ratio of described quadrol and water is (3-4): 1, to be mixedly seal after evenly, at 150-200 ℃, react 8-10h, obtain zinc sulphide hybridized nanometer sheet;
Step 2, after the zinc sulphide hybridized nanometer sheet of step 1 preparation is dispersed in quadrol, add again water to carry out twice dispersing, then add Cadmium chloride fine powder, to be mixedly seal after evenly, at 120-200 ℃, react 3-6 hour, in the thiocarbamide using in element cadmium and step 1 in wherein said Cadmium chloride fine powder, the mol ratio of elementary sulfur is equimolar ratio.
7. the preparation method of dendritic cadmium sulfide superfine nano according to claim 6 rod hierarchical organization material, is characterized in that, in described step 1, to be mixedly seals after evenly, preferably reacts at 180-200 ℃; In described step 2, to be mixedly seal after evenly, preferably react 4-5 hour at 150-180 ℃.
8. the preparation method of dendritic cadmium sulfide superfine nano according to claim 6 rod hierarchical organization material, it is characterized in that, after step 2 reaction finishes, remove supernatant liquid, collect yellow mercury oxide, with second alcohol and water centrifuge washing 4-6 time, be finally placed in 40 ℃ of vacuum drying ovens dry 12 hours, obtain cadmium sulfide nano hierarchical organization material.
9. the preparation method of dendritic cadmium sulfide superfine nano according to claim 6 rod hierarchical organization material, is characterized in that, the reaction vessel that utilizes autoclave to use as step 1 and step 2, and general employing be take the reactor that tetrafluoroethylene is liner.
10. the rod of the dendritic cadmium sulfide superfine nano as described in one of claim 1-5 hierarchical organization material produces the application in hydrogen in catalysis, wherein use the reaction soln being comprised of water, dehydrated alcohol and triethylamine, the volume ratio of described water, dehydrated alcohol and triethylamine is 15:15:2.
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| CN201510117542.1A CN104760991A (en) | 2014-01-02 | 2014-01-02 | Application of dendritic cadmium sulfide ultrathin nanorod-scale-structure material in catalytic hydrogen production |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106830053A (en) * | 2017-02-09 | 2017-06-13 | 西南科技大学 | A kind of preparation method of the CdS nanometer material of structure-controllable |
| CN108715439A (en) * | 2018-05-23 | 2018-10-30 | 中国科学技术大学先进技术研究院 | A kind of cadmium base chalcogenide nanometer rods and preparation method, elctro-catalyst and application |
| CN109772365A (en) * | 2017-11-14 | 2019-05-21 | 天津大学 | A kind of double-layer porous nanometer tube composite materials of zinc sulphide-cadmium sulfide and its preparation method and application |
| CN110975886A (en) * | 2019-12-09 | 2020-04-10 | 西北大学 | Porous two-dimensional zinc cadmium sulfide nanosheet and preparation method and application thereof |
| CN110975890A (en) * | 2019-12-24 | 2020-04-10 | 福州大学 | Method for preparing Mo-doped CdS photocatalyst by cation replacement method |
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| CN116371423A (en) * | 2023-04-14 | 2023-07-04 | 辽宁石油化工大学 | Mn with leaf petal-shaped three-dimensional dendritic structure x Cd 1-x Preparation method and application of S photocatalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106830053A (en) * | 2017-02-09 | 2017-06-13 | 西南科技大学 | A kind of preparation method of the CdS nanometer material of structure-controllable |
| CN109772365A (en) * | 2017-11-14 | 2019-05-21 | 天津大学 | A kind of double-layer porous nanometer tube composite materials of zinc sulphide-cadmium sulfide and its preparation method and application |
| CN109772365B (en) * | 2017-11-14 | 2021-08-24 | 天津大学 | Zinc sulfide-cadmium sulfide double-layer porous nanotube composite material and preparation method and application thereof |
| CN108715439A (en) * | 2018-05-23 | 2018-10-30 | 中国科学技术大学先进技术研究院 | A kind of cadmium base chalcogenide nanometer rods and preparation method, elctro-catalyst and application |
| CN110975886A (en) * | 2019-12-09 | 2020-04-10 | 西北大学 | Porous two-dimensional zinc cadmium sulfide nanosheet and preparation method and application thereof |
| CN110975890A (en) * | 2019-12-24 | 2020-04-10 | 福州大学 | Method for preparing Mo-doped CdS photocatalyst by cation replacement method |
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| CN103708532B (en) | 2015-09-30 |
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