CN101345290A - Cadmium sulfide/organic semiconductor heterojunction nanowire and preparation method thereof - Google Patents
Cadmium sulfide/organic semiconductor heterojunction nanowire and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cadmium sulfide/organic semiconductor heterojunction nanometer wire and a preparation method thereof. The method of the invention is characterized in that electric chemical deposition is carried out for an alumina template under a power-on condition so as to obtain the cadmium sulfide nanometer wire; subsequently, the electric chemical deposition is carried out by using an electrolyte solution of conductive polymer compound and organic solution of electrolyte, thus obtaining the cadmium sulfide/organic semiconductor heterojunction nanometer wire. The nanometer wire has uniform appearance and clear interface, and can stably exist in the air. The heterojunction nanometer wire prepared by the method of the invention has wide potential application prospect in the nanometer-size photoelectric integration field and the nanometer electronic field such as field effect transistor, solar battery, photoelectric switch, photosensitive device, sensor, etc.
Description
Technical field
The present invention relates to a kind of cadmium sulfide/organic semiconductor heterojunction nanowire and preparation method thereof.
Background technology
Heterojunction is as the primary element in the electronics, important role (Sze, S.M.Physics of Semiconducting Devices.2ed. all arranged understanding other semiconductor device operation principles and hyundai electronics application; John wiley﹠amp; Sons:1981).The information technology of develop rapidly is more and more higher to the requirement of the miniaturization of electronic device and integrated level, and the individual devices size in the large scale integrated circuit has entered sub-micron even Nano grade.As realizing integrated prerequisite and the basis of nanoscale devices, how in the nanoscale scope, to construct nano-device, just become a difficult problem of needing solution badly.
The hybrid nano material can obtain each single component material and the not available high-performance of its body phase material, and become one of hot fields of material science research by the synergy of effective compound realization organic because of it.The inorganic material superior performance, but alternative scope is less, and character is fixed, and is difficult to regulation and control.And organic semiconducting materials is of a great variety, and critical natures such as molecular configuration and level structure can be regulated and control with synthetic flexibly by the design of molecule.So than traditional inorganic heterogeneous nano wire, the organic/inorganic heterojunction nano-wire combines the advantage of two component parts because of it: the electronic transmission performance that inorganic semiconductor material is good and stable; Organic semiconductor is regulated and control performance by chemical modification easily, some new physical phenomenon and character may occur, promptly helps deepening the research of organic and inorganic material intrinsic properties, helps developing the device (Moon, the C.Y. that make new advances again; Dalpian, G.M.; Zhang, Y.; Wei, S.H.; Huang, X.Y.; Li, J.Study of Phase Selectivityof Organic-Inorganic Hybrid Semiconductors Chem.Mater.2006,18,2805-2809.Halls, J.J.M.; Walsh, C.A.; Greenham, N.C.; Marseglia, E.A.; Friend, R.H.; Moratti, S.C.; Holmes, A.B.Efficient photodiodes from interpenetrating polymer networks Nature376,498-500.Gomez-Romero, P.Hybrid Organic-Inorganic Materials-In Search ofSynergic Activity, Adv.Mater.2001,13,163-174.).Yet the organic/inorganic heterojunction nano-wire is still blank so far from the research that is prepared into its various character.
Summary of the invention
The purpose of this invention is to provide a kind of cadmium sulfide/organic semiconductor heterojunction nanowire and preparation method thereof.
The method for preparing cadmium sulfide/organic semiconductor heterojunction nanowire provided by the invention comprises the steps:
1) be that the alumina formwork of platinum layer is fixed in the electrolysis tank as work electrode with the top layer, the dimethyl sulphoxide solution that will contain solubility cadmium salt and sulphur powder is as electrolyte solution, electrochemical deposition is carried out in energising, is that deposition obtains cadmium sulfide nano wires on the alumina formwork of platinum layer on the top layer;
2) top layer that deposits cadmium sulfide nano wires that step 1) is obtained is that the alumina formwork of platinum layer is as work electrode, the platinum filament conduct is to electrode, saturated calomel electrode is as reference electrode, electrolyte solution is conducting polymer compound and electrolytical organic solution, electrochemical deposition is carried out in energising, is that deposition obtains cadmium sulfide/organic semiconductor heterojunction nanowire on the alumina formwork of platinum layer on the top layer.
In the step 1) of said method, the solubility cadmium salt is caddy, cadmium nitrate or cadmium acetate, and the sulphur powder is sublimed sulfur or sedimentation sulphur; The concentration of the dimethyl sulphoxide solution of solubility cadmium salt is 0.055 mol, and the concentration of the dimethyl sulphoxide solution of sulphur powder is 0.19 mol.The temperature of electrochemical deposition is 110-130 ℃, and the time is 3-30min, and current density is 2.5-5 milliampere/square centimeter.
Step 2) in, the conducting polymer compound is pyrroles, thiophene, aniline or phenylene ethylene, and electrolyte is lithium perchlorate or tetrabutyl ammonium hexafluorophosphate, and the solvent in the organic solution is acetonitrile and/or toluene.In this electrolyte solution, the conducting polymer compound concentrations is the 0.1-0.5 mol, also can be 0.1-0.3 mol or 0.1-0.4 mol; Electrolytical concentration is the 0.1-0.3 mol.The temperature of electrochemical deposition is 20-40 ℃, and the time is 10-120min, also can be 10-60 minute, 10-80 minute or 10-100 minute; Current potential is constant in 0.85 volt (vs.SCE).
The cadmium sulfide/organic semiconductor heterojunction nanowire that utilizes above-mentioned preparation method to obtain; and the application of this cadmium sulfide/organic semiconductor heterojunction nanowire in the material of preparation field-effect transistor, solar cell, optoelectronic switch, light-sensitive device or transducer, also belong to protection scope of the present invention.
The object of the invention is to utilize business-like alumina formwork, by the different functional material of electro-deposition, can prepare pattern homogeneous based on different materials, interface heterojunction nano-wire clearly in a large number.This method not only can be used for preparing the organic/inorganic heterojunction nano-wire, equally also can be used for preparing inorganic/inorganic, organic/organic heterojunction nano wire.But this heterojunction nano-wire stable existence in air.The heterojunction nano-wire that adopts this method to prepare all has wide potential application foreground at nanoelectronic field, nanoscale photoelectricity integration fields such as field-effect transistor, solar cell, optoelectronic switch, light-sensitive device or transducers.
Description of drawings
ESEM (SEM) figure of the CdS-PPY heterojunction nano-wire that Fig. 1 prepares for the embodiment of the invention 1.
Transmission electron microscope (TEM) figure of the CdS-PPY heterojunction nano-wire that Fig. 2 prepares for the embodiment of the invention 1.
The Electronic Speculum figure of PTh-CdS nucleocapsid junction nanowire that Fig. 3 prepares for the embodiment of the invention 2 and PTh-CdS head to head configuration nano wire.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the present invention is not limited to following examples.
Embodiment 1, preparation CdS-PPY heterojunction nano-wire
Preparation CdS-PPY heterojunction nano-wire method provided by the invention comprises the steps:
A side evaporation (or sputter) that at first with the aperture is the alumina formwork of 100 nanometers is gone up metal platinum (Pt) as conductive layer, then this alumina formwork is fixed in the electrolysis tank as work electrode.
1) will contain 0.055 mol (M) caddy (CdCl
2) and dimethyl sulfoxide (DMSO) (DMSO) solution of 0.19M sedimentation sulphur be electrolyte, under 130 ℃ temperature (between 110-130 ℃ arbitrary temperature all can), constant current density is 2.5 milliamperes of/square centimeter (mA/cm
2) carry out electrochemical deposition, prepare cadmium sulfide (CdS) nano wire.The length of CdS can be controlled (not waiting from 10-30 minute) by sedimentation time.After deposition finishes, adopt hot DMSO, acetone, acetonitrile equal solvent flushing alumina formwork surface successively.
2) continue the alumina formwork that deposits the CdS nano wire for preparing with step 1) as work electrode, platinum filament is as to electrode, and saturated calomel electrode (SCE) is as reference electrode, and electropolymerization prepares PPY (polypyrrole) part in three-electrode system.Electropolymerization is containing 0.1M pyrroles and 0.1M (0.1-0.3M all can) lithium perchlorate (LiClO
4) acetonitrile solution in carry out, temperature is 20 ℃ (20-40 ℃ all can), keeps current potential constant in 0.85 volt (V) (vs.SCE) 1 hour, promptly obtains the CdS-PPY heterojunction nano-wire on the alumina formwork surface.In the sodium hydroxide solution of 3M, optionally dissolve alumina formwork, and precipitate four times, obtain the CdS-PPY heterojunction nano-wire of surface cleaning with the sample that deionized water wash obtains.
Utilize SEM that structures of samples is observed, this SEM sample prepares as follows: with alumina formwork all after the dissolving, centrifugally leave and take precipitation and with deionized water wash 3-4 time, then with ethanol with sample dispersion, and drip on the silicon chip of cleaning.After treating the alcohol solvent volatilization totally on the silicon chip, the silicon chip that will have sample is bonded on the sample stage with conducting resinl to be tested.Above-mentioned ESEM (SEM) test result as shown in Figure 1, wherein, Figure 1A is the cross section sem photograph that is filled with the alumina formwork of CdS-PPY heterojunction nano-wire; Figure 1B is the sem photograph of single CdS-PPY heterojunction nano-wire; Fig. 1 C is the element mapping of single CdS-PPY heterojunction nano-wire.As seen from the figure, the CdS-PPY heterojunction nano-wire for preparing gained with this method has very high filling rate, and pattern homogeneous, interface are clear, and average diameter is about 200-400 nanometer (nm), and length is 10-20 micron (μ m).
It is under 15 kilovolts of (kV) accelerating voltages that the first vegetarian noodles of X-ray energy loss spectrum (EDS) distributes, and beam bombardment sample surfaces and get, the first vegetarian noodles of carbon (C) element and cadmium (Cd) distribute, and to prove conclusively the CdS-PPY heterojunction nano-wire be head to head structure.
The TEM sample prepares according to following steps: the CdS-PPY heterojunction nano-wire was dispersed in the ethanol after ultrasonic 2-3 minute, gets homodisperse suspension 10 microlitres (μ L), slowly drop on the copper mesh.Above-mentioned transmission electron microscope (TEM) test result as shown in Figure 2, wherein, Fig. 2 A is the low power transmission electron microscope picture of CdS-PPY heterojunction nano-wire; Fig. 2 B is the transmission electron microscope picture that CdS-PPY amplifies at the interface, and as seen from the figure, the organic/inorganic junction interface that CdS-PPY forms is in conjunction with tight, and the interface is clear.
Embodiment 2, preparation PTh-CdS nuclear shell structure nano line
There is the AAO template of conduction Pt layer to be fixed in the electrolysis tank according to the method evaporation among the embodiment 1, as work electrode.
1) at first, as to electrode, saturated calomel electrode (SCE) is as reference electrode with platinum filament, and electropolymerization prepares PTh (polythiophene) part in three-electrode system.Electropolymerization carries out in the acetonitrile solution of thiophene that contains 0.1-0.3M and 0.1M tetrabutyl ammonium hexafluorophosphate, temperature is 30 ℃ (20-40 ℃ all can), keeps current potential constant in a constant value (the 1.85 volt more commonly used) 10-60min of 1.85-2.0 volt (V) in (vs.SCE).
2) continue the alumina formwork that deposits the PTh nano wire for preparing with step 1) as work electrode, platinum filament is to electrode, is containing 0.055 mol (M) caddy (CdCl
2) and dimethyl sulfoxide (DMSO) (DMSO) solution of 0.19M sulphur powder be electrolyte, under 130 ℃ temperature, constant current density is 2.5 milliamperes of/square centimeter (mA/cm
2) carry out electrochemical deposition, prepare cadmium sulfide (CdS) nano wire part.The length of CdS can be controlled (not waiting from 10-30 minute) by sedimentation time.After deposition finishes, still as embodiment 1 usefulness in each solvent clean the template surface that contains PTh-CdS nuclear shell structure nano line successively.In the sodium hydroxide solution of 3M, optionally dissolve alumina formwork, and precipitate four times, obtain the PTh-CdS nuclear shell structure nano line of surface cleaning with the sample that deionized water wash obtains.
Embodiment 3, preparation PTh-CdS head to head configuration nano wire
Method step described in preparation PTh-CdS head to head configuration nano wire method provided by the invention and the embodiment 2 is identical.Only in preparation process, by changing step 2) middle electrochemical deposition CdS current density size partly, just can prepare PTh-CdS head to head configuration nano wire.Also promptly containing 0.055 mol (M) caddy (CdCl
2) and dimethyl sulfoxide (DMSO) (DMSO) solution of 0.19M sedimentation sulphur be electrolyte, under 130 ℃ temperature, constant current density is 5 milliamperes of/square centimeter (mA/cm
2) carry out electrochemical deposition.Deposit 3 minutes and can obtain PTh-CdS head to head configuration nano wire.
Utilize SEM, TEM that structures of samples is characterized, sample preparation methods is identical with embodiment 1.The PTh-CdS nuclear shell structure nano line that use the inventive method prepares and the Electronic Speculum test result of PTh-CdS head to head configuration nano wire are as shown in Figure 3.Wherein, Fig. 3 A is the front scan Electronic Speculum figure of PTh-CdS nuclear shell structure nano line; Fig. 3 B is the transmission electron microscope picture of two PTh-CdS nuclear shell structure nano lines; Fig. 3 C is the positive surface sweeping Electronic Speculum figure of PTh-CdS head to head configuration nano wire.Fig. 3 D, 3E are respectively the surface sweeping Electronic Speculum figure and the projection Electronic Speculum figure of single PTh-CdS head to head configuration nano wire.As seen from the figure, employing this method prepares the PTh-CdS nuclear shell structure nano line of gained and PTh-CdS head to head configuration nano thread structure is clear and definite, the pattern homogeneous, and average diameter is consistent with the template duct, is 200-400 nanometer (nm), adjustable length.
Claims (9)
1, a kind of cadmium sulfide/organic semiconductor heterojunction nanowire is prepared as follows and obtains:
1) be that the alumina formwork of platinum layer is fixed in the electrolysis tank as work electrode with the top layer, the dimethyl sulphoxide solution that will contain solubility cadmium salt and sulphur powder is as electrolyte solution, electrochemical deposition is carried out in energising, is that deposition obtains cadmium sulfide nano wires on the alumina formwork of platinum layer on described top layer;
2) top layer that deposits cadmium sulfide nano wires that described step 1) is obtained is that the alumina formwork of platinum layer is as work electrode, the platinum filament conduct is to electrode, saturated calomel electrode is as reference electrode, electrolyte solution is conducting polymer compound and electrolytical organic solution, electrochemical deposition is carried out in energising, is that deposition obtains cadmium sulfide/organic semiconductor heterojunction nanowire on the alumina formwork of platinum layer on described top layer.
2, nano wire according to claim 1 is characterized in that: in the described step 1), the solubility cadmium salt is caddy, cadmium nitrate or cadmium acetate, and the sulphur powder is sublimed sulfur or sedimentation sulphur;
Described step 2) in, the conducting polymer compound is pyrroles, thiophene, aniline or phenylene ethylene, and electrolyte is lithium perchlorate or tetrabutyl ammonium hexafluorophosphate, and the solvent in the organic solution is acetonitrile and/or toluene.
3, nano wire according to claim 1 and 2 is characterized in that: in the described step 1), the concentration of the dimethyl sulphoxide solution of solubility cadmium salt is 0.055 mol, and the concentration of the dimethyl sulphoxide solution of sulphur powder is 0.19 mol;
Described step 2) in, in the described electrolyte solution, the conducting polymer compound concentrations is the 0.1-0.5 mol, and electrolytical concentration is the 0.1-0.3 mol.
4, nano wire according to claim 1 and 2 is characterized in that: in the described step 1), the temperature of electrochemical deposition is 110-130 ℃, and the time is 3-30 minute, and current density is 2.5-5 milliampere/square centimeter;
Described step 2) in, the temperature of electrochemical deposition is 20-40 ℃, and the time is 10-120 minute, and current potential is constant in 0.85 volt.
5, a kind of method for preparing cadmium sulfide/organic semiconductor heterojunction nanowire comprises the steps:
1) be that the alumina formwork of platinum layer is fixed in the electrolysis tank as work electrode with the top layer, the dimethyl sulphoxide solution that will contain solubility cadmium salt and sulphur powder is as electrolyte solution, electrochemical deposition is carried out in energising, is that deposition obtains cadmium sulfide nano wires on the alumina formwork of platinum layer on described top layer;
2) top layer that deposits cadmium sulfide nano wires that described step 1) is obtained is that the alumina formwork of platinum layer is as work electrode, the platinum filament conduct is to electrode, saturated calomel electrode is as reference electrode, electrolyte solution is conducting polymer compound and electrolytical organic solution, electrochemical deposition is carried out in energising, is that deposition obtains cadmium sulfide/organic semiconductor heterojunction nanowire on the alumina formwork of platinum layer on described top layer.
6, method according to claim 5 is characterized in that: in the described step 1), the solubility cadmium salt is caddy, cadmium nitrate or cadmium acetate, and the sulphur powder is sublimed sulfur or sedimentation sulphur;
Described step 2) in, the conducting polymer compound is pyrroles, thiophene, aniline or phenylene ethylene, and electrolyte is lithium perchlorate or tetrabutyl ammonium hexafluorophosphate, and the solvent in the organic solution is acetonitrile and/or toluene.
7, according to claim 5 or 6 described methods, it is characterized in that: in the described step 1), the concentration of the dimethyl sulphoxide solution of solubility cadmium salt is 0.055 mol, and the concentration of the dimethyl sulphoxide solution of sulphur powder is 0.19 mol;
Described step 2) in, in the described electrolyte solution, the conducting polymer compound concentrations is the 0.1-0.5 mol, and electrolytical concentration is the 0.1-0.3 mol.
8, according to claim 5 or 6 described methods, it is characterized in that: in the described step 1), the temperature of electrochemical deposition is 110-130 ℃, and the time is 3-30 minute, and current density is 2.5-5 milliampere/square centimeter;
Described step 2) in, the temperature of electrochemical deposition is 20-40 ℃, and the time is 10-120 minute, and current potential is constant in 0.85 volt.
9, the application of the arbitrary described cadmium sulfide/organic semiconductor heterojunction nanowire of claim 1-4 in the material of preparation field-effect transistor, solar cell, optoelectronic switch, light-sensitive device or transducer.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102050426A (en) * | 2009-11-10 | 2011-05-11 | 北京邮电大学 | Method for preparing heterogeneous nanowire |
| CN102148332A (en) * | 2010-11-26 | 2011-08-10 | 北京化工大学 | Preparation method of semiconductor nano-wire-based organic/inorganic composite solar cell |
| CN103641169A (en) * | 2013-11-12 | 2014-03-19 | 江苏大学 | Synthetic method of Bi2S3-MoS2 nanometer heterostructure |
| CN103755927A (en) * | 2013-12-30 | 2014-04-30 | 北京化工大学 | Preparation method of cadmium sulfide/poly 3-hexyl thiophene/carbon nanotube composite material |
| CN108269698A (en) * | 2018-02-06 | 2018-07-10 | 太原理工大学 | A kind of electrochemical preparation method of metal sulfide and its application |
| CN110499489A (en) * | 2019-07-23 | 2019-11-26 | 电子科技大学 | A kind of preparation process of semiconductor/metal heterojunction nano-wire array material |
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2008
- 2008-09-05 CN CN 200810119395 patent/CN101345290A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050426A (en) * | 2009-11-10 | 2011-05-11 | 北京邮电大学 | Method for preparing heterogeneous nanowire |
| CN102050426B (en) * | 2009-11-10 | 2013-06-12 | 北京邮电大学 | Method for preparing heterogeneous nanowire |
| CN102148332A (en) * | 2010-11-26 | 2011-08-10 | 北京化工大学 | Preparation method of semiconductor nano-wire-based organic/inorganic composite solar cell |
| 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 |
| CN103755927A (en) * | 2013-12-30 | 2014-04-30 | 北京化工大学 | Preparation method of cadmium sulfide/poly 3-hexyl thiophene/carbon nanotube composite material |
| CN108269698A (en) * | 2018-02-06 | 2018-07-10 | 太原理工大学 | A kind of electrochemical preparation method of metal sulfide and its application |
| CN110499489A (en) * | 2019-07-23 | 2019-11-26 | 电子科技大学 | A kind of preparation process of semiconductor/metal heterojunction nano-wire array material |
| CN110499489B (en) * | 2019-07-23 | 2021-06-01 | 电子科技大学 | Preparation process of semiconductor/metal heterojunction nanowire array material |
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