CN103332724A - Preparation method of sea urchin-shaped cadmium sulfide nanospheres - Google Patents
Preparation method of sea urchin-shaped cadmium sulfide nanospheres Download PDFInfo
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- CN103332724A CN103332724A CN2013101939065A CN201310193906A CN103332724A CN 103332724 A CN103332724 A CN 103332724A CN 2013101939065 A CN2013101939065 A CN 2013101939065A CN 201310193906 A CN201310193906 A CN 201310193906A CN 103332724 A CN103332724 A CN 103332724A
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Abstract
The invention discloses a preparation method of sea urchin-shaped cadmium sulfide nanospheres. The preparation method comprises the following steps of mixing a single-source precursor, an organic alcohol and distilled water into a mixed solution, carrying out microwave heating of the mixed solution at a temperature of 80-100 DEG C for 3-7min with continuous stirring along the same direction, then carrying out microwave heating at a temperature of 150-165DEG C for 4-10min, washing the reaction solution orderly by distilled water and anhydrous ethanol, and carrying out drying to obtain the sea urchin-shaped cadmium sulfide nanospheres. The sea urchin-shaped cadmium sulfide nanospheres prepared by an ordinary pressure microwave method have high photocatalytic activity, and performances superior to performances of commercial cadmium sulfide, wherein after xenon lamp irradiation for 20min, the sea urchin-shaped cadmium sulfide nanospheres have a rhodamine B degradation rate of 75% and commercial cadmium sulfide has a rhodamine B degradation rate of 15%, and after xenon lamp irradiation for 140min, the sea urchin-shaped cadmium sulfide nanospheres have a rhodamine B degradation rate more than 95% and commercial cadmium sulfide has a rhodamine B degradation rate of 50%. The preparation method has simple processes, adopts the cheap raw materials stored easily, has a short preparation period and high repeatability, and is suitable for large-scale production.
Description
(1) technical field
The present invention relates to inorganic nano material synthetic technology and II-VI family semiconductor nano material field, be specifically related to a kind of preparation method of sea urchin shape cadmium sulfide nano ball.
(2) background technology
Cadmium Sulfide is a kind of important semiconductor material, because its character is superior, has caused numerous scientists' research interest in the last few years.Cadmium Sulfide is a kind of typical II-VI family direct band-gap semicondictor material, its at room temperature body phase Cadmium Sulfide band gap width be 2.42eV, nano level Cadmium Sulfide band gap is greater than 2.45eV.Because of its special optics, electrical properties, aspects such as opto-electronic conversion, photoluminescence, photochemical catalysis, magneticsubstance, biological detection have been widely used in.
Great majority research at present lays particular emphasis on the dimensional effect of nanoparticle, and in fact, the physicochemical property of nano material are not only relevant with size, and are also relevant with its shape.Up to now, under specific reaction conditions, successfully prepare various Cadmium Sulfide crystal with special appearance, as people such as Chen Hongzheng (CN101172642A) with the mixing solutions of cadmium presoma, sulphur presoma and sequestrant after reacting 10min～60h under 90～300 ℃ of conditions, prepare a kind of floriform cadmium sulfide; People such as Huang Wei (CN101113016A) do cadmium source and sulphur source with Cadmium chloride fine powder and thiocarbamide respectively, and 140～160 ℃ of reaction 3～4h synthesize a kind of starfish-shaped cadmium sulfide nanostructure in autoclave; People such as Huang Jianfeng (CN101844796A) mix with two water cadmium acetates, a water quadrol and thiocarbamide, regulate PH, and 110～150 ℃ of microwave hydrothermals behind reaction 1～10min, are prepared the graduation hexagonal flake cadmium sulfide; People such as Li (Journal of Materials Chemistry2012,22 (45), 23815-23820.) do the cadmium source with cadmium acetate, do the sulphur source with thiocarbamide, following assisting of hydrogen fluoride and Neutral ammonium fluoride, 200 ℃ of hydro-thermals, behind the reaction 20h, prepare the Cadmium Sulfide of shaped-like leaf.
Existing synthetic method mainly is physical vapor deposition, chemical vapour deposition, microemulsion method, colloid chemistry method, hydrothermal method, solvent-thermal method etc.These methods or because of the equipment requirements height are relatively more expensive; Or because of the high and difficult storage of raw materials cost; Or because complex process, preparation cycle are long, repeatable poor; Or because of product pattern heterogeneity and easy generation reunion etc., do not realize the suitability for industrialized production of cadmium sulfide nano material, also hindered the large-scale application of cadmium sulfide nano material simultaneously.
(3) summary of the invention
The object of the invention provides a kind of preparation method of sea urchin shape cadmium sulfide nano ball, and the existing method of solution prepares the Cadmium Sulfide complex process, preparation cycle is long, cost is high, is difficult to the problem of scale operation.
The technical solution used in the present invention is:
The invention provides a kind of preparation method of sea urchin shape cadmium sulfide nano ball, described method is carried out as follows: single source presoma and organic pure and mild distilled water a are mixed and made into mixed solution, continue under the equidirectional stirring mixed solution microwave heating after 3～7 minutes under 80～100 ℃ of conditions, microwave heating 4～10min under 150～165 ℃ of conditions again, then reaction solution is used successively distilled water b and absolute ethanol washing (preferably washing 2～3 times) back dry, obtained described sea urchin shape cadmium sulfide nano ball; Described organic alcohol is the alcoholic solvent of C2～C6; Described single source presoma is preferably cadmium diethyl dithiocarbamate, the volumetric usage of described organic alcohol is counted 90～800ml/mmol with single source presoma amount of substance, and the volumetric usage of described distilled water a is counted 3～20ml/mmol with single source presoma amount of substance.
Further, preferably under 80～100 ℃ of conditions and the power of microwave heating under 150～165 ℃ of conditions be 500W.
Further, described organic alcohol is preferably the mixing of arbitrary proportion more than one or both kinds in ethylene glycol, glycerol or the 1,3 butylene glycol, more preferably ethylene glycol.
Further, described stirring is magnetic agitation, and described magnetic agitation rotating speed is 500～1000 rev/mins.
Further, the volumetric usage of described organic alcohol is counted 200～450ml/mmol with single source presoma amount of substance, and the volumetric usage of described distilled water a is counted 8～18ml/mmol with single source presoma amount of substance.
Further, with mixed solution microwave heating after 4～6 minutes under 85～95 ℃, 500W condition, microwave heating 5～9 minutes under 155～165 ℃, 500W condition again.
The sea urchin shape cadmium sulfide nano ball shape of the present invention's preparation is sea urchin seemingly, its sphere diameter 100～200nm, and the ball surface has a large amount of untapered cylindrical thorns to be distributed in the ball surface, the long 20～50nm of thorn, wide 10～30nm.
Distilled water a of the present invention and distilled water b are distilled water, and to add the amount of distilled water different and name for ease of distinguishing different step, and letter itself does not have implication.
Compared with prior art, beneficial effect of the present invention is mainly reflected in: the present invention adopts the normal pressure microwave method to make the presoma cadmium diethyl dithiocarbamate pyrolysis in the mixing solutions of polyvalent alcohol and distilled water of single source prepare sea urchin shape cadmium sulfide nano ball; The sea urchin shape cadmium sulfide nano ball of the present invention's preparation has higher photocatalytic activity, its performance is better than commercial Cadmium Sulfide, after xenon lamp shines 20 minutes, degradation rate to the degraded rhodamine B can reach 75% and commercial Cadmium Sulfide has only 15%, after 140 minutes, degradation rate can reach more than 95% and commercial Cadmium Sulfide has only 50%; The inventive method technology is simple, raw material is relatively inexpensive and be easy to storage, and preparation cycle is short, and is repeatable high, is expected to scale operation.
(4) description of drawings
Fig. 1 is scanning electron microscope (SEM) figure and transmission electron microscope (TEM) figure of the sea urchin shape cadmium sulfide nano ball of embodiment 1 preparation, wherein A is scanning electron microscope (SEM) figure under 100,000 times, B is scanning electron microscope (SEM) figure under 400,000 times, C is transmission electron microscope (TEM) figure under 300,000 times, and D is transmission electron microscope (TEM) figure under 500,000 times.
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of the sea urchin shape cadmium sulfide nano ball of embodiment 1 preparation.
Fig. 3 is degrade the respectively degradation rate change curve in time of rhodamine B of the sea urchin shape cadmium sulfide nano ball of embodiment 1 preparation and commercial Cadmium Sulfide.
(5) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
The normal pressure microwave-assisted that following embodiment uses is synthetic/the extractive reaction instrument is the MAS-I type normal pressure microwave-assisted that Xinyi Microwave Chemistry Tech Co., Ltd. produces synthetic/extractive reaction instrument, and its operating frequency is 2450MHz.
Taking by weighing 0.05g(0.12mmol) cadmium diethyl dithiocarbamate puts into flask, measuring 48ml ethylene glycol and 2ml distilled water pours into respectively and makes mixed solution in the flask, above-mentioned flask is put into the normal pressure microwave-assisted to be synthesized/extractive reaction instrument (flask has prolong and logical tap water), following 90 ℃ of magnetic agitation (rotating speed is 500 rev/mins), the 500W heating is after 5 minutes, 160 ℃ then, 500W heating 5 minutes, with the centrifugal (8000rpm of reaction solution, 10min), get precipitation and use distilled water and absolute ethanol washing successively 2～3 times, then at 50 ℃ of following dry 1h, namely obtain sea urchin shape cadmium sulfide nano ball 15mg, productive rate 86.5%.
Sea urchin shape cadmium sulfide nano ball scanning electron microscope (SEM) figure sees among Fig. 1 shown in the A and B, the product monodispersity better as can be known, pattern homogeneous, cleaning surfaces inclusion-free, shape be like sea urchin by A and B, its sphere diameter 140～170nm, the ball surface has a large amount of untapered cylindrical thorns to be distributed in the ball surface, long 30～the 40nm of thorn, wide 20～25nm.The transmission electron microscope TEM figure of product sees among Fig. 1 that shown in the C and D, the product of being prepared as can be known by C and D is solid sea urchin shape nanometer ball.X ray (XRD) collection of illustrative plates of the sea urchin shape cadmium sulfide nano ball that present embodiment obtains can find out that the product inclusion-free of preparing is the Cadmium Sulfide of pure six side's phases as shown in Figure 2.All peak positions and literature value be complementary [referring to Joint Committee on Powder Diffraction Standards (JCPDS), File No41-1049.] do not find the dephasign peak, show that product purity is higher.
Embodiment 2
The amount of ethylene glycol and pure water among the embodiment 1 is changed into respectively: get 48ml ethylene glycol and 2ml distilled water is poured in the flask respectively, the magnetic agitation rotating speed is 1000 rev/mins then, other operations are identical with embodiment 1, obtain sea urchin shape cadmium sulfide nano ball 14mg, sphere diameter 130～160nm, the ball surface has a large amount of untapered cylindrical thorns to be distributed in the ball surface, the long 20～40nm of thorn, wide 10～20nm.
Embodiment 3
Change the consumption of cadmium diethyl dithiocarbamate among the embodiment 1 into 0.1g(0.24mmol), other operations are identical with embodiment 1.Obtain sea urchin shape cadmium sulfide nano ball 30mg, sphere diameter 140～180nm, the ball surface has a large amount of untapered cylindrical thorns to be distributed in the ball surface, the long 30～50nm of thorn, wide 15～25nm.
Embodiment 4
Measure 49ml ethylene glycol and 1ml distilled water is poured in the flask respectively.Other operations are identical with embodiment 1.Obtain sea urchin shape cadmium sulfide nano ball 15mg, sphere diameter 140～180nm, the ball surface has a large amount of untapered cylindrical thorns to be distributed in the ball surface, the long 30～40nm of thorn, wide 15～25nm.
Embodiment 5
Measure 98ml ethylene glycol and 2ml distilled water is poured in the flask respectively.The consumption of cadmium diethyl dithiocarbamate changes 0.1g(0.24mmol into), other operations are identical with embodiment 1.Obtain sea urchin shape cadmium sulfide nano ball 31mg, sphere diameter 145～180nm, the ball surface has a large amount of untapered cylindrical thorns to be distributed in the ball surface, the long 30～50nm of thorn, wide 15～25nm.
Embodiment 6
Measure 48ml glycerol and 2ml distilled water and pour into respectively in the flask, other operations are identical with embodiment 1.Obtain sea urchin shape cadmium sulfide nano ball 14mg, sphere diameter 140～170nm, the ball surface has a large amount of untapered cylindrical thorns to be distributed in the ball surface, the long 20～40nm of thorn, wide 10～20nm.
Embodiment 7
Measure 2 * 10 of the sea urchin shape cadmium sulfide nano ball of 20mg embodiment 1 preparation and 100ml
-5After mixing, mol/L rhodamine B (Tianjin A Faaisha chemistry company limited) puts into the beaker of 250ml, in the dark magnetic agitation (500 rev/mins of rotating speeds) is 5 hours, make its adsorption equilibrium, take a sample and get supernatant liquor after centrifugal at 200～700nm scope test light absorption value, the absorbance of climax correspondence is designated as A
0(Science and Technology Ltd. is freely opened up in Beijing, PLS-SXE300) irradiation and magnetic agitation (500 rev/mins of rotating speeds) down always at the xenon lamp of 300W with the mixed solution after the above-mentioned adsorption equilibrium then.It is 20A that the xenon lamp electric current is set, and the mixed solution liquid level is apart from xenon lamp 10cm.Every 20 minutes, from mixed solution, remove out 4ml liquid.Behind the centrifugal that takes out, (day island proper Tianjin, UV-1800) at 200～700nm scope test light absorption value, the absorbance of climax correspondence is designated as A at ultraviolet-visual spectrometer to get supernatant liquid
x, calculate the degradation rate of sea urchin shape cadmium sulfide nano ball degraded rhodamine B according to formula (1).
Degradation rate=(A
0– A
x)/A
0* 100%, formula (1)
A in the formula (1)
0Be the absorbance after the sea urchin shape cadmium sulfide nano ball miscible fluid adsorption equilibrium, A
xBe the absorbance of sea urchin shape cadmium sulfide nano ball miscible fluid after the adsorption equilibrium after shining X minute under the hernia lamp.
Replace sea urchin shape cadmium sulfide nano ball in contrast with the commercial Cadmium Sulfide of 20mg (Shanghai Aladdin reagent company limited) under the similarity condition.
Calculate degrade the respectively degradation rate change curve in time of rhodamine B of the sea urchin shape cadmium sulfide nano ball of the present invention preparation and commercial Cadmium Sulfide, as shown in Figure 3.As seen from Figure 3, the sea urchin shape cadmium sulfide nano ball of the present invention's preparation has higher photocatalytic activity, its performance is better than commercial Cadmium Sulfide, and after xenon lamp irradiation 20 minutes, the sea urchin shape Cadmium Sulfide degradation rate of the present invention's preparation can reach 75% and commercial Cadmium Sulfide has only 15%.After 140 minutes, the sea urchin shape Cadmium Sulfide degradation rate of the present invention preparation can reach more than 95% and commercial Cadmium Sulfide has only 50%.
Claims (7)
1. the preparation method of a sea urchin shape cadmium sulfide nano ball, it is characterized in that described method carries out as follows: single source presoma and organic pure and mild distilled water a are mixed and made into mixed solution, continue under the equidirectional stirring mixed solution microwave heating after 3～7 minutes under 80～100 ℃ of conditions, microwave heating 4～10 minutes under 150～165 ℃ of conditions again, then reaction solution is used successively behind distilled water b and the absolute ethanol washing dryly, obtained described sea urchin shape cadmium sulfide nano ball; Described organic alcohol is the alcoholic solvent of C2～C6; Described single source presoma is cadmium diethyl dithiocarbamate, and the volumetric usage of described organic alcohol is counted 90～800ml/mmol with single source presoma amount of substance, and the volumetric usage of described distilled water a is counted 3～20ml/mmol with single source presoma amount of substance.
2. the preparation method of sea urchin shape cadmium sulfide nano ball according to claim 1, it is characterized in that under 80～100 ℃ of conditions and the power of microwave heating under 150～165 ℃ of conditions be 500W.
3. the preparation method of sea urchin shape cadmium sulfide nano ball according to claim 1 is characterized in that described organic alcohol is the mixing of arbitrary proportion more than one or both kinds in ethylene glycol, glycerol or the 1,3 butylene glycol.
4. the preparation method of sea urchin shape cadmium sulfide nano ball according to claim 1 is characterized in that described stirring is magnetic agitation.
5. as the preparation method of sea urchin shape cadmium sulfide nano ball as described in the claim 4, it is characterized in that described magnetic agitation rotating speed is 500～1000 rev/mins.
6. the preparation method of sea urchin shape cadmium sulfide nano ball according to claim 1, the volumetric usage that it is characterized in that described organic alcohol is counted 200～450ml/mmol with the cadmium amount of substance, and the volumetric usage of described distilled water a is counted 8～18ml/mmol with single source presoma amount of substance.
7. the preparation method of sea urchin shape cadmium sulfide nano ball according to claim 1 is characterized in that mixed solution microwave heating after 4～6 minutes under 85～95 ℃, 500W condition, microwave heating 5～9 minutes under 155～165 ℃, 500W condition again.
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Cited By (5)
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| CN103771487A (en) * | 2013-12-26 | 2014-05-07 | 江苏大学 | Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave |
| CN106698500A (en) * | 2015-11-16 | 2017-05-24 | 天津大学 | Cadmium sulfide ultrathin nanometer flaky material preparation method and application thereof |
| CN107055589A (en) * | 2017-05-18 | 2017-08-18 | 西北师范大学 | The method that Microwave reduction method liquid phase prepares CdS nanometer material |
| CN110787821A (en) * | 2019-09-10 | 2020-02-14 | 温州大学 | Graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with burr-like structure and preparation method and application thereof |
| CN115364897A (en) * | 2022-08-10 | 2022-11-22 | 中国科学院空间应用工程与技术中心 | Waterborne polyurethane-cadmium sulfide nanocomposite coating and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771487A (en) * | 2013-12-26 | 2014-05-07 | 江苏大学 | Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave |
| CN106698500A (en) * | 2015-11-16 | 2017-05-24 | 天津大学 | Cadmium sulfide ultrathin nanometer flaky material preparation method and application thereof |
| CN107055589A (en) * | 2017-05-18 | 2017-08-18 | 西北师范大学 | The method that Microwave reduction method liquid phase prepares CdS nanometer material |
| CN107055589B (en) * | 2017-05-18 | 2018-10-30 | 西北师范大学 | The method that Microwave reduction method liquid phase prepares CdS nanometer material |
| CN110787821A (en) * | 2019-09-10 | 2020-02-14 | 温州大学 | Graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with burr-like structure and preparation method and application thereof |
| CN110787821B (en) * | 2019-09-10 | 2022-06-03 | 温州大学 | Graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nano composite material with burred spherical structure and preparation method and application thereof |
| CN115364897A (en) * | 2022-08-10 | 2022-11-22 | 中国科学院空间应用工程与技术中心 | Waterborne polyurethane-cadmium sulfide nanocomposite coating and preparation method thereof |
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