CN102814185A - Preparation method of silver sulfide-zinc sulfide semiconductor nanometer heterojunction - Google Patents
Preparation method of silver sulfide-zinc sulfide semiconductor nanometer heterojunction Download PDFInfo
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Abstract
The invention provides a preparation method of a silver sulfide-zinc sulfide semiconductor nanometer heterojunction. The preparation method comprises a step (A) of enabling reaction precursor silver dibutyl dithiocarbamate to undergo pyrolysis in a mixed solvent to obtain silver sulfide particles; and a step (B) of enabling the silver sulfide obtained in the step (A) to serve as a catalyst, enabling an intermediate product formed by pyrolysis of zinc dibutyl dithiocarbamate to be dissolved in the mixed solvent containing the silver sulfide particles, separating out zinc sulfide nanorods from the silver sulfide particles under the effect of trioctylphosphine and n-octadecyl mercaptan, and forming the silver sulfide-zinc sulfide semiconductor nanometer heterojunction. The preparation method of the silver sulfide-zinc sulfide semiconductor nanometer heterojunction is simple and convenient, high in rate of production and suitable for industrial production. The shape and the structure of the silver sulfide-zinc sulfide semiconductor nanometer heterojunction can be controlled under normal pressure, and the rate of production can be over 80%.
Description
Technical field
The present invention relates to the nano material preparation technical field, specifically relate to the synthetic method of a kind of silver sulfide-zinc sulfide nano hetero-junctions.
Background technology
Semiconductor sulfuration thing nano material has quantum size effect and skin effect, has aspect performances such as excellent light, electricity, magnetic, catalysis, has broad application prospects in industries such as electronics, biology, coating, pharmacy.
The heterostructure semiconductor nano material promptly is grouped together the nano material of two kinds of different chemical compositions, and it not only can bring into play the functional characteristics of component separately, and also the combination because of heterogeneity produces new characteristic.Nano heterojunction is different with single nano material; Because nanocrystal not only can keep the character of original material in the orderly combination of micro-scale, effective contact of group element material simultaneously (chemical bond and Van der Waals force combination) will make the performance of heterogeneous structure material be enhanced.Semi-conducting material with nano-heterogeneous structure becomes one of most active content of current research because of its unrivaled excellent properties, and being proved to be in fields such as semiconductor light emitting, photocatalysis and novel photoelectric devices like chalcogenide heterogeneous structural nano material has very important theory and application prospect.
In the heterostructure semiconductor nano material; The one dimension heterogeneous structural nano material (line, rod, band and pipe) that can realize specific function has special significance to nano electron device, nano-photon device, also so under study for action receives maximum attention.What adopted in this area research at present mainly is that method of vapor-phase growing prepares one dimension heterogeneous structural nano line, comprises radial heterostructure and axial heterojunction structure.In the vapor phase growth process, adjust each constituent content in the gas phase repeatedly, rely on the gas phase-liquid phase-solid phase mechanism (VLS mechanism) in the vapor phase growth in nano wire, to form the heterogeneous structural nano line to two or more combination of components.Yet the desired apparatus expensive of vapor phase method requires height to vacuum, and the preparation process is also comparatively loaded down with trivial details.The compare VLS mechanism of gas phase condition, liquid-phase condition preparation solution-liquid phase-solid phase mechanism (SLS mechanism) that nano wire adopted down can show extra advantage, like nanowire size narrowly distributing, controllable diameter, the preparation of liquid phase low temperature system etc.
As a kind of sulfur family heterogeneous structural nano material and preparation method thereof is provided among the patent documentation CN102008966.Described nano-heterogeneous structure is bismuth sulfide and cadmium sulfide, and the mol ratio in bismuth source and cadmium source is 1: 1, and when it was applied to photocatalysis degradation organic contaminant, degradation efficiency significantly promoted.As behind UV-irradiation methyl red 20min under this nano-heterogeneous structure catalysis, methyl red 430nm characteristic peak intensity weakens to 10% of initial intensity; And to reach same palliating degradation degree, and commercial titania powder need about 80min, and the mixture of bismuth sulfide and cadmium sulfide approximately needs 60min.Said according to this article; The higher reason of ultraviolet catalytic degradation efficiency of bismuth sulfide/cadmium sulfide nano heterojunction structure paramethyl red is: in heterojunction structure; The valence band of bismuth sulfide and conduction band all are in the valence band and the conduction band inside of cadmium sulfide; Electronics that illumination in the cadmium sulfide produced and hole can be moved to bismuth sulfide, but the speed that electronics moves will be far longer than the rate travel in hole, thereby the raising photocatalysis efficiency takes place effectively to separate electron-hole pair.
Summary of the invention
The present invention provides the preparation method of silver sulfide-zinc sulfide nano hetero-junctions that a kind of method is easy, productive rate is high, suitability for industrialized is produced.Preparation method of the present invention divides following steps, steps A: reaction precursor body dibutyl dithiocaarbamate silver pyrolytic in first mixed solvent obtains the silver sulfide particle; Step B: utilize the silver sulfide that obtains in the steps A to be catalyst; The intermediate product that the zinc dibutyl dithiocarbamate pyrolytic is formed is dissolved in second mixed solvent that contains said silver sulfide particle; Under the effect of positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, from the silver sulfide particle, separate out the zinc sulfide nano rod, form silver sulfide-zinc sulfide semiconductor nano heterojunction.
First mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan in the preferred said steps A, and said steps A is under 180 ℃ temperature, to carry out.Dibutyl dithiocaarbamate silver is 1: 100～1: 500 with the mol ratio of octadecylamine in the preferred said steps A; Dibutyl dithiocaarbamate silver is 1: 50～1: 400 with the mol ratio of positive trioctylphosphine oxide (TOPO); Dibutyl dithiocaarbamate silver is 1: 200～1: 800 with the mol ratio of positive stearylmercaptan.
Second mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan among the preferred said step B, and said step B carries out under 210 ℃ temperature.The mol ratio of zinc dibutyl dithiocarbamate and octadecylamine is 1: 20～1: 320 among the preferred said step B; Zinc dibutyl dithiocarbamate is 1: 20～1: 160 with the mol ratio of positive trioctylphosphine oxide (TOPO); Zinc dibutyl dithiocarbamate is 1: 40～1: 320 with the mol ratio of positive stearylmercaptan.
The mol ratio of silver sulfide particle and said zinc dibutyl dithiocarbamate is 1: 1～1: 100 among the preferred said step B of the present invention.
Be that the preferred concrete operations step of the present invention is steps A: reaction precursor body dibutyl dithiocaarbamate silver 10～20mg (is the round-bottomed flask of 0.02～0.04mmol) adding 50mL, adds octadecylamine 4～10mmol, positive trioctylphosphine oxide (TOPO) 2～8mmol, positive stearylmercaptan 8～16mmol successively; With the oil bath that flask is put into 180 ℃ of constant temperature, magnetic agitation reaction 5min is after reaction finishes cooling; Take out solution to test tube with dropper, the gained deposition is with the n-hexane dilution, behind the sonic oscillation 10min; Centrifugation 10min under the rotating speed of 12000rpm; Product is sunken to container bottom, abandoning supernatant, and it is subsequent use to obtain silver sulfide nano particle; Step B: 0.5～5.0mg silver sulfide nano particle is scattered in the n-hexane, splashes into the round-bottomed flask of 50mL, add octadecylamine 4～16mmol; The oil bath heating 10min that puts into 210 ℃ of constant temperature adds zinc dibutyl dithiocarbamate 0.05～0.2mmol, positive trioctylphosphine oxide (TOPO) 4～8mmol, positive stearylmercaptan 8～16mmol then to remove n-hexane, magnetic agitation reaction 30min; Reaction finishes to be cooled to room temperature, takes out solution to test tube, dilutes with n-hexane; Sonic oscillation 5min; Centrifugation 5min under the 8000rpm rotating speed, abandoning supernatant, nano heterojunction is sunken to container bottom.
Silver sulfide of the present invention-zinc sulfide semiconductor nano heterojunction can be used for efficient industrial catalyst; The photocatalytic degradation catalyst material that can be used as harmful organic substance contaminant water environment gross contamination thing; The manufacturing materials that can be used as highly sensitive gas and biology sensor; Can be used as the luminescent material that ultraviolet laser is made.
The present invention has overcome shortcomings such as reaction conditions such as adopting inert gas shielding among the prior art semiconductor nano hetero-junctions preparation method is complicated, control is loaded down with trivial details fully; Only need laboratory instrument and equipment commonly used among the present invention; Like flask, agitator and oil bath pan etc., under normal pressure, can realize nano heterogeneous junction configuration of silver sulfide-zinc sulfide semiconductor and structure control through the ratio that prolongs growth time or change mixed solvent; And the productive rate of silver sulfide among the present invention-zinc sulfide semiconductor nano heterojunction can reach more than 80%.
Description of drawings
Fig. 1 is the transmission electron microscope picture of silver sulfide in the embodiment of the invention 1-zinc sulfide nano hetero-junctions;
Fig. 2 is the high-resolution-ration transmission electric-lens figure of silver sulfide in the embodiment of the invention 1-zinc sulfide nano hetero-junctions;
Fig. 3 is scanning transmission electron microscope (STEM) figure of silver sulfide in the embodiment of the invention 1-zinc sulfide nano hetero-junctions.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is described in further detail.Below be merely preferred implementation of the present invention, protection scope of the present invention is not limited thereto, and any those skilled in the art can be easy to the change of carrying out or change be encompassed within protection scope of the present invention in technical scope disclosed by the invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Embodiment 1:
Round-bottomed flask with reaction precursor body dibutyl dithiocaarbamate silver 10mg adding 50mL adds octadecylamine 6mmol, positive trioctylphosphine oxide (TOPO) 2mmol, positive stearylmercaptan 8mmol successively, and flask is put into the oil bath of 180 ℃ of constant temperature; Magnetic agitation reaction 5min after reaction finishes cooling, takes out solution to test tube with dropper; Dilute with n-hexane; Behind the sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom; Abandoning supernatant, it is subsequent use to obtain silver sulfide nano particle.The 0.5mg silver sulfide nano particle is scattered in the n-hexane, splashes into the round-bottomed flask of 50mL, add octadecylamine 4mmol; The oil bath heating 10min that puts into 210 ℃ of constant temperature adds zinc dibutyl dithiocarbamate 0.05mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 8mmol then to remove n-hexane, magnetic agitation reaction 30min; Reaction finishes to be cooled to room temperature, takes out solution to test tube, dilutes with n-hexane; Sonic oscillation 5min; Centrifugation 5min under the 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.The silver sulfide of preparing-zinc sulfide nano hetero-junctions length is 350nm, width 25nm, productive rate 88%.
Embodiment 2:
Round-bottomed flask with reaction precursor body dibutyl dithiocaarbamate silver 12mg adding 50mL adds octadecylamine 6mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 8mmol successively, and flask is put into the oil bath of 180 ℃ of constant temperature; Magnetic agitation reaction 5min after reaction finishes cooling, takes out solution to test tube with dropper; Dilute with n-hexane; Behind the sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom; Abandoning supernatant, it is subsequent use to obtain silver sulfide nano particle.The 1.0mg silver sulfide nano particle is scattered in the n-hexane, splashes into the round-bottomed flask of 50mL, add octadecylamine 8mmol; The oil bath heating 10min that puts into 210 ℃ of constant temperature adds zinc dibutyl dithiocarbamate 0.1mmol, positive trioctylphosphine oxide (TOPO) 6mmol, positive stearylmercaptan 12mmol then to remove n-hexane, magnetic agitation reaction 30min; Reaction finishes to be cooled to room temperature, takes out solution to test tube, dilutes with n-hexane; Sonic oscillation 5min; Centrifugation 5min under the 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.The silver sulfide of preparing-zinc sulfide nano hetero-junctions length is 300nm, width 25nm, productive rate 85%.
Embodiment 3:
Round-bottomed flask with reaction precursor body dibutyl dithiocaarbamate silver 15mg adding 50mL adds octadecylamine 8mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 16mmol successively, and flask is put into the oil bath of 180 ℃ of constant temperature; Magnetic agitation reaction 5min after reaction finishes cooling, takes out solution to test tube with dropper; Dilute with n-hexane; Behind the sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom; Abandoning supernatant, it is subsequent use to obtain silver sulfide nano particle.The 2.0mg silver sulfide nano particle is scattered in the n-hexane, splashes into the round-bottomed flask of 50mL, add octadecylamine 16mmol; The oil bath heating 10min that puts into 210 ℃ of constant temperature adds zinc dibutyl dithiocarbamate 0.1mmol, positive trioctylphosphine oxide (TOPO) 6mmol, positive stearylmercaptan 10mmol then to remove n-hexane, magnetic agitation reaction 30min; Reaction finishes to be cooled to room temperature, takes out solution to test tube, dilutes with n-hexane; Sonic oscillation 5min; Centrifugation 5min under the 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.The silver sulfide of preparing-zinc sulfide nano hetero-junctions length is 300nm, width 20nm, productive rate 85%.
Embodiment 4:
Round-bottomed flask with reaction precursor body dibutyl dithiocaarbamate silver 20mg adding 50mL adds octadecylamine 10mmol, positive trioctylphosphine oxide (TOPO) 8mmol, positive stearylmercaptan 12mmol successively, and flask is put into the oil bath of 180 ℃ of constant temperature; Magnetic agitation reaction 5min after reaction finishes cooling, takes out solution to test tube with dropper; Dilute with n-hexane; Behind the sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom; Abandoning supernatant, it is subsequent use to obtain silver sulfide nano particle.The 5.0mg silver sulfide nano particle is scattered in the n-hexane, splashes into the round-bottomed flask of 50mL, add octadecylamine 12mmol; The oil bath heating 10min that puts into 210 ℃ of constant temperature adds zinc dibutyl dithiocarbamate 0.2mmol, positive trioctylphosphine oxide (TOPO) 8mmol, positive stearylmercaptan 16mmol then to remove n-hexane, magnetic agitation reaction 30min; Reaction finishes to be cooled to room temperature, takes out solution to test tube, dilutes with n-hexane; Sonic oscillation 5min; Centrifugation 5min under the 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.The silver sulfide of preparing-zinc sulfide nano hetero-junctions length is 200nm, width 18nm, productive rate 88%.
Embodiment 5:
Round-bottomed flask with reaction precursor body dibutyl dithiocaarbamate silver 12mg adding 50mL adds octadecylamine 4mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 8mmol successively, and flask is put into the oil bath of 180 ℃ of constant temperature; Magnetic agitation reaction 5min after reaction finishes cooling, takes out solution to test tube with dropper; Dilute with n-hexane; Behind the sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom; Abandoning supernatant, it is subsequent use to obtain silver sulfide nano particle.The 0.5mg silver sulfide nano particle is scattered in the n-hexane, splashes into the round-bottomed flask of 50mL, add octadecylamine 4mmol; The oil bath heating 10min that puts into 210 ℃ of constant temperature adds zinc dibutyl dithiocarbamate 0.1mmol, positive trioctylphosphine oxide (TOPO) 8mmol, positive stearylmercaptan 8mmol then to remove n-hexane, magnetic agitation reaction 30min; Reaction finishes to be cooled to room temperature, takes out solution to test tube, dilutes with n-hexane; Sonic oscillation 5min; Centrifugation 5min under the 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.The silver sulfide of preparing-zinc sulfide nano hetero-junctions length is 200nm, width 18nm, productive rate 82%.
Explain in conjunction with Fig. 1 to Fig. 3, the nano heterogeneous club shaped structure of becoming of silver sulfide-zinc sulfide semiconductor that uses the inventive method to obtain, its uniform form does not have and reunites; Short end (caput) is a silver sulfide, and long end (excellent body) is a zinc sulphide.
Pre-reaction material is the zinc dibutyl dithiocarbamate of single source form among the present invention, so can avoid owing to the too high inhomogeneities that causes product size of local concentration in the course of reaction.Among the present invention, through the control to pre-reaction material thermal decomposition process and solvent composition in high boiling mixed solvent, regulate nanocrystal nucleation and growth course, zinc sulphide at first is dissolved in the silver sulfide particle, separates out after the concentration that reaches capacity; Realized control through control, obtained the silver sulfide that the size homogeneous is adjustable, pattern is controlled-zinc sulfide nano hetero-junctions zinc sulfide crystal nucleation and growth course to the silver sulfide particle.
Claims (10)
1. the preparation method of silver sulfide-zinc sulfide semiconductor nano heterojunction may further comprise the steps:
Steps A: reaction precursor body dibutyl dithiocaarbamate silver decomposes in first mixed solvent and obtains the silver sulfide particle;
Step B: utilize the silver sulfide that obtains in the steps A to be catalyst; The intermediate product that zinc dibutyl dithiocarbamate is decomposed to form is dissolved in second mixed solvent that contains said silver sulfide particle; Under the effect of positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, grow the zinc sulfide nano rod, form silver sulfide-zinc sulfide semiconductor nano heterojunction from the silver sulfide particle.
2. preparation method according to claim 1 is characterized in that: first mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan in the said steps A, and said steps A is under 180 ℃ temperature, to carry out.
3. preparation method according to claim 2 is characterized in that: dibutyl dithiocaarbamate silver is 1: 100～1: 500 with the mol ratio of octadecylamine in the said steps A.
4. preparation method according to claim 2 is characterized in that: dibutyl dithiocaarbamate silver is 1: 50～1: 400 with the mol ratio of positive trioctylphosphine oxide (TOPO) in the said steps A.
5. preparation method according to claim 2 is characterized in that: dibutyl dithiocaarbamate silver is 1: 200～1: 800 with the mol ratio of positive stearylmercaptan in the said steps A.
6. preparation method according to claim 1 is characterized in that: second mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan among the said step B, and said step B carries out under 210 ℃ temperature.
7. preparation method according to claim 6 is characterized in that: the mol ratio of zinc dibutyl dithiocarbamate and octadecylamine is 1: 20～1: 320 among the said step B.
8. preparation method according to claim 6 is characterized in that: zinc dibutyl dithiocarbamate is 1: 20～1: 160 with the mol ratio of positive trioctylphosphine oxide (TOPO) among the said step B.
9. preparation method according to claim 6 is characterized in that: zinc dibutyl dithiocarbamate is 1: 40～1: 320 with the mol ratio of positive stearylmercaptan among the said step B.
10. according to any described preparation method in the claim 1 to 9, it is characterized in that the mol ratio of silver sulfide particle and said zinc dibutyl dithiocarbamate is 1: 1～1: 100 among the said step B.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103212426A (en) * | 2013-03-25 | 2013-07-24 | 温州大学 | Nano heterojunction and preparation method thereof |
| CN103641169A (en) * | 2013-11-12 | 2014-03-19 | 江苏大学 | Synthetic method of Bi2S3-MoS2 nanometer heterostructure |
| CN103771487A (en) * | 2013-12-26 | 2014-05-07 | 江苏大学 | Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave |
| CN107720827A (en) * | 2017-10-31 | 2018-02-23 | 合肥工业大学 | A kind of preparation method of ternary vulcanization zinc-manganese nano wire |
| CN113135595A (en) * | 2021-05-08 | 2021-07-20 | 合肥工业大学 | Preparation method of one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide |
| CN113184894A (en) * | 2021-05-08 | 2021-07-30 | 合肥工业大学 | One-dimensional heterogeneous nano material of silver sulfide and cobalt sulfide and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103212426A (en) * | 2013-03-25 | 2013-07-24 | 温州大学 | Nano heterojunction and preparation method thereof |
| CN103212426B (en) * | 2013-03-25 | 2015-09-23 | 温州大学 | A kind of nano heterojunction and preparation method thereof |
| CN103641169A (en) * | 2013-11-12 | 2014-03-19 | 江苏大学 | Synthetic method of Bi2S3-MoS2 nanometer heterostructure |
| CN103641169B (en) * | 2013-11-12 | 2015-09-02 | 江苏大学 | A kind of Bi 2s 3-MoS 2the synthetic method of nano-heterogeneous structure |
| CN103771487A (en) * | 2013-12-26 | 2014-05-07 | 江苏大学 | Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave |
| CN107720827A (en) * | 2017-10-31 | 2018-02-23 | 合肥工业大学 | A kind of preparation method of ternary vulcanization zinc-manganese nano wire |
| CN113135595A (en) * | 2021-05-08 | 2021-07-20 | 合肥工业大学 | Preparation method of one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide |
| CN113184894A (en) * | 2021-05-08 | 2021-07-30 | 合肥工业大学 | One-dimensional heterogeneous nano material of silver sulfide and cobalt sulfide and preparation method thereof |
| CN113135595B (en) * | 2021-05-08 | 2024-02-02 | 合肥工业大学 | Preparation method of one-dimensional heterogeneous nanomaterial of manganese sulfide and zinc sulfide |
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