CN102814185B - 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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- CN102814185B CN102814185B CN201110206243.7A CN201110206243A CN102814185B CN 102814185 B CN102814185 B CN 102814185B CN 201110206243 A CN201110206243 A CN 201110206243A CN 102814185 B CN102814185 B CN 102814185B
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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 nano material preparing technical field, specifically relate to a kind of synthetic method of silver sulfide-zinc sulfide nano hetero-junctions.
Background technology
Semiconductor sulfide nano-material has quantum size effect and skin effect, has the aspect performances such as excellent optical, electrical, magnetic, catalysis, has broad application prospects in industries such as electronics, biology, coating, pharmacy.
Heterostructure semiconductor nano material, 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, also because the combination of heterogeneity produces new characteristic.Nano heterojunction is different from 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 in conjunction with) is enhanced the performance that makes heterogeneous structure material.There is the semi-conducting material of nano-heterogeneous structure because its unrivaled excellent properties becomes one of most active content of current research, have very important theory and application prospect as chalcogenide heterogeneous structural nano material has been proved to be in fields such as semiconductor light emitting, photocatalysis and Novel Optoelectronic Devices.
In 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, is also therefore subject under study for action maximum attention.What in this area research at present, adopt is mainly that method of vapor-phase growing is prepared one dimension heterogeneous structural nano line, comprises radial heterostructure and axial heterojunction structure.Each constituent content repeatedly adjust gas phase in vapor phase growth process in, relies on the gas-liquid phase-solid phase mechanism (VLS mechanism) in vapor phase growth that two or more combination of components are formed to heterogeneous structural nano line in nano wire.But, the desired apparatus expensive of vapor phase method, high to vacuum requirement, preparation process is also comparatively loaded down with trivial details.The compare VLS mechanism of gas phase condition, under liquid-phase condition, prepare molten liquid-liquid phase-solid phase mechanism (SLS mechanism) that nano wire adopts and can show extra advantage, as nanowire size narrowly distributing, diameter is controlled, prepared by liquid phase low temperature system etc.
As provided a kind of sulfur group hetero-structure nano material and preparation method thereof in patent documentation CN102008966.Described nano-heterogeneous structure is bismuth sulfide and cadmium sulfide, and the mol ratio in He Ge source, bismuth source is 1: 1, and when it is applied to photocatalysis degradation organic contaminant, degradation efficiency significantly promotes.After UV-irradiation methyl red 20min under this nano-heterogeneous structure catalysis, methyl red 430nm characteristic peak remitted its fury is to 10% of initial intensity; And to reach same palliating degradation degree, and business titania powder need to about 80min, and the mixture of bismuth sulfide and cadmium sulfide approximately needs 60min.Described in 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 are all in valence band and the conduction band inside of cadmium sulfide, the electronics that in cadmium sulfide, illumination produces 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 there is effectively to separate raising photocatalysis efficiency in electron-hole pair.
Summary of the invention
The 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: precursors dibutyl dithiocaarbamate silver pyrolytic in the first mixed solvent obtains silver sulfide particle; Step B: utilizing the silver sulfide obtaining in steps A is catalyst, the intermediate product that zinc dibutyl dithiocarbamate pyrolytic is formed is dissolved in containing in the second mixed solvent of described silver sulfide particle, under the effect of positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, from silver sulfide particle, separate out zinc sulfide nano rod, form silver sulfide-zinc sulfide semiconductor nano heterojunction.
In preferred described steps A, the first mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, and described steps A is to carry out at the temperature of 180 ℃.In preferred described steps A, dibutyl dithiocaarbamate silver is 1: 100～1: 500 with the mol ratio of octadecylamine; 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.
In preferred described step B, the second mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, and described step B carries out at the temperature of 210 ℃.In preferred described step B, the mol ratio of zinc dibutyl dithiocarbamate and octadecylamine is 1: 20～1: 320; 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.
Preferably in described step B of the present invention, the mol ratio of silver sulfide particle and described zinc dibutyl dithiocarbamate is 1: 1～1: 100.
Be that the preferred concrete operation step of the present invention is, steps A: the round-bottomed flask that precursors dibutyl dithiocaarbamate silver 10～20mg (being 0.02～0.04mmol) is added to 50mL, add successively octadecylamine 4～10mmol, positive trioctylphosphine oxide (TOPO) 2～8mmol, positive stearylmercaptan 8～16mmol, flask is put into the oil bath of 180 ℃ of constant temperature, magnetic agitation reaction 5min, after reaction end is cooling, with dropper take out solution to test tube, gained precipitation is diluted with n-hexane, after sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom, abandoning supernatant, obtain silver sulfide nano particle for subsequent use, step B: 0.5～5.0mg silver sulfide nano particle is scattered in n-hexane, splash into the round-bottomed flask of 50mL, add octadecylamine 4～16mmol, put into the oil bath of 210 ℃ of constant temperature and heat 10min to remove n-hexane, then add zinc dibutyl dithiocarbamate 0.05～0.2mmol, positive trioctylphosphine oxide (TOPO) 4～8mmol, positive stearylmercaptan 8～16mmol, magnetic agitation reaction 30min, reaction finishes to be cooled to room temperature, take out solution to test tube, dilute with n-hexane, sonic oscillation 5min, centrifugation 5min under 8000rpm rotating speed, abandoning supernatant, nano heterojunction is sunken to container bottom.
Silver sulfide-zinc sulfide semiconductor nano heterojunction of the present invention can be used for efficient industrial catalyst; Can be used as the photocatalytic degradation catalyst material of harmful organic substance contaminant water environment gross contamination thing; Can be used as the making material of highly sensitive gas and biology sensor; Can be used as the luminescent material that ultraviolet laser is made.
The present invention has overcome completely in prior art semiconductor nano hetero-junctions preparation method and adopts the reaction condition complexity such as inert gas shielding, controls the shortcomings such as loaded down with trivial details; In the present invention, only need the conventional instrument and equipment in laboratory, as flask, agitator and oil bath pan etc., under normal pressure, can realize the nano heterogeneous junction configuration of silver sulfide-zinc sulfide semiconductor and structure control by the ratio that extends growth time or change mixed solvent; And in the present invention, the productive rate of silver sulfide-zinc sulfide semiconductor nano heterojunction can reach more than 80%.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of silver sulfide-zinc sulfide nano hetero-junctions in the embodiment of the present invention 1;
Fig. 2 is the high-resolution-ration transmission electric-lens figure of silver sulfide-zinc sulfide nano hetero-junctions in the embodiment of the present invention 1;
Fig. 3 is scanning transmission electron microscope (STEM) figure of silver sulfide-zinc sulfide nano hetero-junctions in the embodiment of the present invention 1.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.Below be only the preferred embodiment of the present invention, protection scope of the present invention is not limited to this, and any those skilled in the art is in technical scope disclosed by the invention, within can being easy to the change carried out or changing and be encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Embodiment 1:
Precursors dibutyl dithiocaarbamate silver 10mg is added to the round-bottomed flask of 50mL, add successively octadecylamine 6mmol, positive trioctylphosphine oxide (TOPO) 2mmol, positive stearylmercaptan 8mmol, flask is put into the oil bath of 180 ℃ of constant temperature, magnetic agitation reaction 5min, after reaction end is cooling, with dropper take out solution to test tube, dilute with n-hexane, after sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom, and abandoning supernatant obtains silver sulfide nano particle for subsequent use.0.5mg silver sulfide nano particle is scattered in n-hexane, splash into the round-bottomed flask of 50mL, add octadecylamine 4mmol, put into the oil bath of 210 ℃ of constant temperature and heat 10min to remove n-hexane, then add zinc dibutyl dithiocarbamate 0.05mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 8mmol, magnetic agitation reaction 30min, reaction finishes to be cooled to room temperature, take out solution to test tube, with n-hexane dilution, sonic oscillation 5min, centrifugation 5min under 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.Silver sulfide-zinc sulfide nano hetero-junctions length of preparing is 350nm, width 25nm, productive rate 88%.
Embodiment 2:
Precursors dibutyl dithiocaarbamate silver 12mg is added to the round-bottomed flask of 50mL, add successively octadecylamine 6mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 8mmol, flask is put into the oil bath of 180 ℃ of constant temperature, magnetic agitation reaction 5min, after reaction end is cooling, with dropper take out solution to test tube, dilute with n-hexane, after sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom, and abandoning supernatant obtains silver sulfide nano particle for subsequent use.1.0mg silver sulfide nano particle is scattered in n-hexane, splash into the round-bottomed flask of 50mL, add octadecylamine 8mmol, put into the oil bath of 210 ℃ of constant temperature and heat 10min to remove n-hexane, then add zinc dibutyl dithiocarbamate 0.1mmol, positive trioctylphosphine oxide (TOPO) 6mmol, positive stearylmercaptan 12mmol, magnetic agitation reaction 30min, reaction finishes to be cooled to room temperature, take out solution to test tube, with n-hexane dilution, sonic oscillation 5min, centrifugation 5min under 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.Silver sulfide-zinc sulfide nano hetero-junctions length of preparing is 300nm, width 25nm, productive rate 85%.
Embodiment 3:
Precursors dibutyl dithiocaarbamate silver 15mg is added to the round-bottomed flask of 50mL, add successively octadecylamine 8mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 16mmol, flask is put into the oil bath of 180 ℃ of constant temperature, magnetic agitation reaction 5min, after reaction end is cooling, with dropper take out solution to test tube, dilute with n-hexane, after sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom, and abandoning supernatant obtains silver sulfide nano particle for subsequent use.2.0mg silver sulfide nano particle is scattered in n-hexane, splash into the round-bottomed flask of 50mL, add octadecylamine 16mmol, put into the oil bath of 210 ℃ of constant temperature and heat 10min to remove n-hexane, then add zinc dibutyl dithiocarbamate 0.1mmol, positive trioctylphosphine oxide (TOPO) 6mmol, positive stearylmercaptan 10mmol, magnetic agitation reaction 30min, reaction finishes to be cooled to room temperature, take out solution to test tube, with n-hexane dilution, sonic oscillation 5min, centrifugation 5min under 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.Silver sulfide-zinc sulfide nano hetero-junctions length of preparing is 300nm, width 20nm, productive rate 85%.
Embodiment 4:
Precursors dibutyl dithiocaarbamate silver 20mg is added to the round-bottomed flask of 50mL, add successively octadecylamine 10mmol, positive trioctylphosphine oxide (TOPO) 8mmol, positive stearylmercaptan 12mmol, flask is put into the oil bath of 180 ℃ of constant temperature, magnetic agitation reaction 5min, after reaction end is cooling, with dropper take out solution to test tube, dilute with n-hexane, after sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom, and abandoning supernatant obtains silver sulfide nano particle for subsequent use.5.0mg silver sulfide nano particle is scattered in n-hexane, splash into the round-bottomed flask of 50mL, add octadecylamine 12mmol, put into the oil bath of 210 ℃ of constant temperature and heat 10min to remove n-hexane, then add zinc dibutyl dithiocarbamate 0.2mmol, positive trioctylphosphine oxide (TOPO) 8mmol, positive stearylmercaptan 16mmol, magnetic agitation reaction 30min, reaction finishes to be cooled to room temperature, take out solution to test tube, with n-hexane dilution, sonic oscillation 5min, centrifugation 5min under 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.Silver sulfide-zinc sulfide nano hetero-junctions length of preparing is 200nm, width 18nm, productive rate 88%.
Embodiment 5:
Precursors dibutyl dithiocaarbamate silver 12mg is added to the round-bottomed flask of 50mL, add successively octadecylamine 4mmol, positive trioctylphosphine oxide (TOPO) 4mmol, positive stearylmercaptan 8mmol, flask is put into the oil bath of 180 ℃ of constant temperature, magnetic agitation reaction 5min, after reaction end is cooling, with dropper take out solution to test tube, dilute with n-hexane, after sonic oscillation 10min, centrifugation 10min under the rotating speed of 12000rpm, product is sunken to container bottom, and abandoning supernatant obtains silver sulfide nano particle for subsequent use.0.5mg silver sulfide nano particle is scattered in n-hexane, splash into the round-bottomed flask of 50mL, add octadecylamine 4mmol, put into the oil bath of 210 ℃ of constant temperature and heat 10min to remove n-hexane, then add zinc dibutyl dithiocarbamate 0.1mmol, positive trioctylphosphine oxide (TOPO) 8mmol, positive stearylmercaptan 8mmol, magnetic agitation reaction 30min, reaction finishes to be cooled to room temperature, take out solution to test tube, with n-hexane dilution, sonic oscillation 5min, centrifugation 5min under 8000rpm rotating speed, nano heterojunction is sunken to container bottom, abandoning supernatant.Silver sulfide-zinc sulfide nano hetero-junctions length of preparing is 200nm, width 18nm, productive rate 82%.
Illustrate 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 form is even, without reuniting; Shorter one end (caput) is silver sulfide, and longer one end (excellent body) is zinc sulphide.
In the present invention, pre-reaction material is the zinc dibutyl dithiocarbamate of single source form, so can avoid due to the too high inhomogeneities that causes product size of local concentration in course of reaction.In the present invention, by the control to pre-reaction material thermal decomposition process and solvent composition in high boiling mixed solvent, regulate nanocrystal nucleation and growth course, first zinc sulphide be dissolved in silver sulfide particle, after the concentration that reaches capacity, separates out; By the control of silver sulfide particle has been realized to the control to zinc sulfide crystal nucleation and growth course, obtain silver sulfide-zinc sulfide nano hetero-junctions that size homogeneous is adjustable, pattern is controlled.
Claims (8)
1. a preparation method for silver sulfide-zinc sulfide semiconductor nano heterojunction, comprises the following steps:
Steps A: precursors dibutyl dithiocaarbamate silver decomposes and obtains silver sulfide particle in the first mixed solvent, described the first mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, steps A is to carry out at the temperature of 180 ℃;
Step B: utilizing the silver sulfide obtaining in steps A is catalyst, the intermediate product that zinc dibutyl dithiocarbamate is decomposed to form is dissolved in containing in the second mixed solvent of described silver sulfide particle, described the second mixed solvent is the mixing of octadecylamine, positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, under the effect of positive trioctylphosphine oxide (TOPO) and positive stearylmercaptan, grow zinc sulfide nano rod from silver sulfide particle, formation form is even, nothing is reunited, silver sulfide-zinc sulfide semiconductor nano heterojunction of club shaped structure, and its caput is that silver sulfide, rod are as zinc sulphide; And step B carries out at the temperature of 210 ℃.
2. preparation method according to claim 1, is characterized in that: in described steps A, dibutyl dithiocaarbamate silver is 1:100～1:500 with the mol ratio of octadecylamine.
3. preparation method according to claim 1, is characterized in that: in described steps A, dibutyl dithiocaarbamate silver is 1:50～1:400 with the mol ratio of positive trioctylphosphine oxide (TOPO).
4. preparation method according to claim 1, is characterized in that: in described steps A, dibutyl dithiocaarbamate silver is 1:200～1:800 with the mol ratio of positive stearylmercaptan.
5. preparation method according to claim 1, is characterized in that: in described step B, the mol ratio of zinc dibutyl dithiocarbamate and octadecylamine is 1:20～1:320.
6. preparation method according to claim 1, is characterized in that: in described step B, zinc dibutyl dithiocarbamate is 1:20～1:160 with the mol ratio of positive trioctylphosphine oxide (TOPO).
7. preparation method according to claim 1, is characterized in that: in described step B, zinc dibutyl dithiocarbamate is 1:40～1:320 with the mol ratio of positive stearylmercaptan.
8. according to the preparation method described in any one in claim 1 to 7, it is characterized in that in described step B, the mol ratio of silver sulfide particle and described zinc dibutyl dithiocarbamate is 1:1～1:100.
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| CN103212426B (en) * | 2013-03-25 | 2015-09-23 | 温州大学 | A kind of nano heterojunction and preparation method thereof |
| 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 |
| CN107720827B (en) * | 2017-10-31 | 2019-09-10 | 合肥工业大学 | A kind of preparation method of ternary vulcanization zinc-manganese nano wire |
| 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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| CN101074093A (en) * | 2006-05-19 | 2007-11-21 | 中国科学院理化技术研究所 | Series of elliptical metal sulfide grain, its production and use |
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| Controllable growth of semiconductor heterostructures mediated by bifunctional Ag2S nanocrystals as catalyst or source-host;Guoxing Zhu et al.;《American Chemical Society》;20101208;第133卷(第1期);第150页 * |
| Guoxing Zhu et al..Controllable growth of semiconductor heterostructures mediated by bifunctional Ag2S nanocrystals as catalyst or source-host.《American Chemical Society》.2010,第133卷(第1期),第150页. |
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