CN103771487A - Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave - Google Patents

Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave Download PDF

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CN103771487A
CN103771487A CN201310731176.XA CN201310731176A CN103771487A CN 103771487 A CN103771487 A CN 103771487A CN 201310731176 A CN201310731176 A CN 201310731176A CN 103771487 A CN103771487 A CN 103771487A
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cds
microwave
nano structure
nanostructure
gained
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朱国兴
鲍春林
季振源
沈小平
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Jiangsu University
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Jiangsu University
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Abstract

The invention relates to a method for synthetizing an Ag2S-CdS hetero-nanostructure employing a microwave, and belongs to the field of preparation of a functional nanostructure material. The method comprises the following steps: firstly, mixing nano silver sulfide powder, a precursor of cadmium and oleylamine; heating at 140-170 DEG C for a period of time by using the microwave, so as to obtain the Ag2S-CdS hetero-nanostructure. The Ag2S-CdS hetero-nanostructure obtained by the method forms a mushroom structure, and is uniform in form, and good in monodispersity; the hetero-nanostructure can be well dispersed in a low-polarity solvent. The preparation method related to the invention is carried out by a single pot in a single step, and is short in time, free of charging in the process, simple in technology, convenient to operate and good in repeatability, and easily achieves industrial implementation. The multi-component hetero-nanostructure material has the functional characteristics of silver sulfide and cadmium sulfide, and has good application prospect in the fields of photoelectricity, catalysis and the like.

Description

The synthetic Ag of a kind of microwave 2the method of S-CdS hetero nano structure
Technical field
The invention belongs to functional nanostructure technical field of material, relate to the preparation of sulfide hetero nano structure, particularly the synthetic Ag of a kind of microwave 2the preparation method of S-CdS hetero nano structure.
Background technology
Chemistry and the physical property that nanoparticle determines due to its particle diameter, form and be different from that body phase material is optical, electrical, magnetic property, has shown wide application prospect, is also subject to numerous investigators' extensive concern.Hetero nano structure combines two or more function ingredients on micro-nano-scale, often has several functions characteristic and has good application space.In addition, due to the close contact of different components, heterojunction structure also usually has unique coupling effect, demonstrates performance enhancing or that single-component does not have.As on photoelectric material, combine two kinds of energy bands and there is the semiconductor material that II-type mates, can promote the separation of photo-generated carrier, make hole and electronics trend towards being distributed in different components, thereby suppress the compound of photo-generated carrier, be conducive to improve its photoelectric transformation efficiency, photocatalysis performance etc.Therefore, the various semiconductor-based hetero nano structures of design preparation have great importance.
The various heterojunction semiconductors of preparation generally adopt gas phase approach at present, and this usually needs complicated equipment and higher temperature, and is difficult to obtain the nanostructure compared with small particle size.Investigators more and more pay close attention to the preparation that realizes heterogeneous semiconductor nanostructure by liquid phase approach.The tensio-active agent that can select various different performances and structure in liquid phase approach, solvent carries out crystal-growth-modified and optimization, thereby realizes the growth of heterojunction semiconductor.
Ag 2s be a kind of chemical stability high, can, with narrow semiconductor material, have good photoelectricity, thermoelectricity capability, be widely used in the fields such as photocell, photocon, infrared detector, fast-ionic conductor.The energy gap of CdS is 2.41 eV, is a kind of typical N-shaped semiconductor material, is widely used in photocatalysis field, and can form sosoloid as laser apparatus with zinc sulphide, cadmium selenide etc.CdS low price, is suitable for broad area device.Therefore, utilize liquid phase approach design preparation Ag 2s-CdS heterojunction is expected to obtain the functional materials with outstanding photoelectricity or photocatalysis performance.At present for Ag 2the existing two pieces of reports of chemical synthesis in liquid phase of S-CdS hetero nano structure.Be respectively by the method for solvent thermal and oil bath.These two kinds of methods have all related to more complicated preparation flow, expensive poisonous reagent, and strict experiment parameter (as temperature, concentration etc.) is controlled.
The invention provides one easily microwave route of synthesis high yield prepare monodispersed Ag 2s-CdS hetero nano structure.Adopt microwave heating approach, reaction times section, technical process is simple.
 
Summary of the invention
The object of the present invention is to provide a kind of simple microwave route of synthesis high yield to prepare monodispersed Ag 2s-CdS Heterogeneous Composite structure.The method is simple to operate, low for equipment requirements, and is easy to mass-producing.The present invention is by the following technical solutions:
(1) in appropriate oleyl amine, add silver sulfide nanometer particles (Ag 2s) powder;
(2) in step (1) gained mixed system, add presoma (cadmium diethyl dithiocarbamate, the Cd (DDTC) of cadmium 2), stir, wherein oleyl amine, silver sulfide nanometer particles (Ag 2s) usage ratio of powder and cadmium diethyl dithiocarbamate is: 7:10:(7-28) mg/mL/mg;
(3) compound system of gained in step (2) is placed in to microwave oven, magnetic agitation, reacts 2 ~ 10 min, naturally cooling at microwave heating to 140 ~ 170 ℃;
(4) filter or gained mixture in reactions steps (3) carried out to centrifugal treating with supercentrifuge, removing supernatant liquid, precipitation is used to hexanaphthene and absolute ethanol washing repeatedly, until clear liquid is colourless, drying rear collection product, obtaining Ag 2s-CdS heterojunction.
Technique effect of the present invention is embodied in:
Silver sulfide powder of the present invention is nano level Ag 2s powder;
The mol ratio of silver sulfide of the present invention and cadmium presoma is 1:0.7-2, and described oleyl amine is the common chemical in market.
Method of the present invention is that microwave is synthetic, once reinforced, and reaction is middle without any operation.Preparation is simple, and flow process is short.
The present invention adopts Cd (DDTC) 2do He Ge source, sulphur source, because its thermo-cracking temperature is lower, can slowly provide sulphur and cadmium, be of value to polycomponent Ag 2the formation of S-CdS heterojunction.
Ag of the present invention 2it is 140 ~ 170 ℃ that temperature of reaction in step (3) is stated in the reaction of S-CdS hetero nano structure, and the time is 2-12 min.Related temperature is lower, and particularly the time is shorter.
Ag prepared by the present invention 2s-hetero nano structure is mushroom, Ag 2s component is in mushroom top, and CdS component is in mushroom bar-like portion, and radical length is 30 nm left and right.
Ag prepared by the present invention 2s-CdS hetero nano structure surface has abundant oleyl amine hydrophobic group, dispersibles in low polar solvent.
The Ag of gained of the present invention 2s-CdS hetero nano structure has good application prospect in the field such as photoelectricity, catalysis.
accompanying drawing explanation:
Fig. 1 is process flow diagram of the present invention.
Fig. 2 is Ag prepared by embodiment 1 2x-ray diffraction (XRD) figure of S-CdS Heterogeneous Composite structure.Wherein X-coordinate is diffraction angle (2 θ), unit for degree ( 0), ordinate zou is diffracted intensity.
Fig. 3 is Ag prepared by embodiment 1 2transmission electron microscope (TEM) figure of S-CdS hetero nano structure.Can be observed sample is mushroom-shaped structure, and size evenly.
Fig. 4 is Ag prepared by embodiment 1 2high resolving power transmission electron microscope (HRTEM) figure of S-CdS Heterogeneous Composite structure.
Embodiment
The present embodiment is implemented under take technical solution of the present invention as prerequisite, has provided detailed embodiment, but the invention is not restricted to these embodiment.
Embodiment 1:
(1) 7 mg silver sulfides and 10 mL oleyl amines are joined in flask, then add 14 mg Cd (DDTC) 2, magnetic agitation homogeneous mixture system.
(2) (1) gained mixed system is placed in to microwave and heats, microwave reaction instrument is set as 400 W, and 150 ℃, the time is set as 12 min, is then cooled to room temperature.
(3) with supercentrifuge, reaction gained mixture is carried out to centrifugal treating, remove upper strata liquid, will precipitate with after hexanaphthene and ethanol repetitive scrubbing, obtain black Ag 2s-CdS Heterogeneous Composite structure.
The Ag preparing according to embodiment 1 2s-CdS Heterogeneous Composite structure is through X-ray diffraction test (Fig. 2), and other dephasign peaks do not appear in demonstration, and sample crystallinity is good, and diffraction peak corresponds to six side's phase CdS and monoclinic phase Ag 2s.
The Ag preparing according to embodiment 1 2s-CdS Heterogeneous Composite structure shows that through transmissioning electric mirror test (Fig. 3) sample presents mushroom heterojunction structure, and size evenly.
The Ag preparing according to embodiment 1 2s-CdS Heterogeneous Composite structure shows that through high resolving power transmissioning electric mirror test (Fig. 4) heterogeneous interface is bright and sharp clear.
Embodiment 2:
(1) 7 mg silver sulfides and 10 mL oleyl amines are joined in flask, then add 28 mg Cd (DDTC) 2, magnetic agitation homogeneous mixture system.
(2) (1) gained mixed system is placed in to microwave and heats, microwave reaction instrument is set as 400 W, and 150 ℃, the time is set as 5 min, is then cooled to room temperature.
(3) with supercentrifuge, reaction gained mixture is carried out to centrifugal treating, remove upper strata liquid, will precipitate with after hexanaphthene and ethanol repetitive scrubbing, obtain black Ag 2s-CdS Heterogeneous Composite structure.
Embodiment 3:
(1) 7 mg silver sulfides and 10 mL oleyl amines are joined in flask, then add 7 mg Cd (DDTC) 2, magnetic agitation homogeneous mixture system.
(2) (1) gained mixed system is placed in to microwave and heats, microwave reaction instrument is set as 400 W, and 140 ℃, the time is set as 10 min, is then cooled to room temperature.
(3) with supercentrifuge, reaction gained mixture is carried out to centrifugal treating, remove upper strata liquid, will precipitate with after hexanaphthene and ethanol repetitive scrubbing, obtain black Ag 2s-CdS Heterogeneous Composite structure.
Embodiment 4:
(1) 7 mg silver sulfides and 10 mL oleyl amines are joined in flask, then add 14 mg Cd (DDTC) 2, magnetic agitation homogeneous mixture system.
(2) (1) gained mixed system is placed in to microwave and heats, microwave reaction instrument is set as 400 W, and 170 ℃, the time is set as 2 min, is then cooled to room temperature.
(3) with supercentrifuge, reaction gained mixture is carried out to centrifugal treating, remove upper strata liquid, will precipitate with after hexanaphthene and ethanol repetitive scrubbing, obtain black Ag 2s-CdS Heterogeneous Composite structure.

Claims (6)

1. the synthetic Ag of microwave 2the method of S-CdS hetero nano structure, carry out according to following step:
(1) in appropriate oleyl amine, add silver sulfide powder;
(2) in step (1) gained mixed system, add the presoma cadmium diethyl dithiocarbamate of cadmium, stir, wherein the usage ratio of oleyl amine, silver sulfide nanometer particles powder and cadmium diethyl dithiocarbamate is: 7:10:(7-28) mg/mL/mg;
(3) compound system of gained in step (2) is placed in to microwave oven, magnetic agitation, reacts 2 ~ 10 min, naturally cooling at microwave heating to 140 ~ 170 ℃;
(4) filter or gained mixture in reactions steps (3) carried out to centrifugal treating with supercentrifuge, removing supernatant liquid, precipitation is used to hexanaphthene and absolute ethanol washing repeatedly, until clear liquid is colourless, drying rear collection product, obtaining Ag 2s-CdS heterojunction.
2. the synthetic Ag of microwave according to claim 1 2the method of S-CdS hetero nano structure, is characterized in that the described silver sulfide powder of step (1) is nano level silver sulfide powder.
3. the synthetic Ag of microwave according to claim 1 2the method of S-CdS hetero nano structure, is characterized in that the mol ratio of the cadmium presoma in silver sulfide and the step (2) in step (1) is 1:0.7-2, and the oleyl amine in described step (2) is the conventional oleyl amine in market.
4. the synthetic Ag of microwave according to claim 1 2the method of S-CdS hetero nano structure, is characterized in that the Ag of step (4) gained 2s-hetero nano structure is mushroom, Ag 2s component is in mushroom top, and CdS component is in mushroom bar-like portion, and radical length is 30 nm left and right.
5. the synthetic Ag of microwave according to claim 1 2the method of S-CdS hetero nano structure, is characterized in that the Ag of step (4) gained 2s-CdS hetero nano structure surface has abundant oleyl amine hydrophobic group, dispersibles in low polar solvent.
6. the Ag of gained in claim 1-5 2the application of S-CdS hetero nano structure in photoelectricity, catalytic field.
CN201310731176.XA 2013-12-26 2013-12-26 Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave Pending CN103771487A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104925852A (en) * 2015-05-25 2015-09-23 新疆大学 Method for preparing cadmium sulphide-silver sulphide heterostructured nanomaterial by solid phase
CN106554034A (en) * 2015-09-30 2017-04-05 浙江安诺其助剂有限公司 A kind of sulfuration silver nano material dispersion and preparation method and application
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
CN108831748A (en) * 2018-06-27 2018-11-16 安徽大学 A kind of nitrogen-doped graphene modification four vulcanization seven bronze medals/copper sulfide composite material and preparation methods and application down
CN112536047A (en) * 2019-09-20 2021-03-23 中国科学技术大学 Chiral nano material and preparation method thereof

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CN103332724A (en) * 2013-05-22 2013-10-02 温州大学 Preparation method of sea urchin-shaped cadmium sulfide nanospheres

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104925852A (en) * 2015-05-25 2015-09-23 新疆大学 Method for preparing cadmium sulphide-silver sulphide heterostructured nanomaterial by solid phase
CN106554034A (en) * 2015-09-30 2017-04-05 浙江安诺其助剂有限公司 A kind of sulfuration silver nano material dispersion and preparation method and application
CN106554034B (en) * 2015-09-30 2019-03-19 嘉兴安诺其助剂有限公司 A kind of vulcanization silver nano material dispersion and the 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
CN108831748A (en) * 2018-06-27 2018-11-16 安徽大学 A kind of nitrogen-doped graphene modification four vulcanization seven bronze medals/copper sulfide composite material and preparation methods and application down
CN112536047A (en) * 2019-09-20 2021-03-23 中国科学技术大学 Chiral nano material and preparation method thereof

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Application publication date: 20140507