CN101752211A - Method for preparing nano-wire containing inorganic/organic heterojunction - Google Patents
Method for preparing nano-wire containing inorganic/organic heterojunction Download PDFInfo
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- CN101752211A CN101752211A CN 200810227886 CN200810227886A CN101752211A CN 101752211 A CN101752211 A CN 101752211A CN 200810227886 CN200810227886 CN 200810227886 CN 200810227886 A CN200810227886 A CN 200810227886A CN 101752211 A CN101752211 A CN 101752211A
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Abstract
The invention provides a method for preparing a nano-wire containing inorganic/organic heterojunction, comprising the following steps: a. an electrochemical deposition liquid of an inorganic compound semiconductor and an electrophoretic deposition liquid of an organic semiconductor are firstly prepared; b. the electrochemical deposition is carried out by taking a porous template coated with a metal film as a working electrode, and a template partially filled with inorganic semiconductor nano-wires is obtained; and c. the template filled with the inorganic semiconductor nano-wires is cleaned and dried, then the template is placed in the electrophoretic deposition liquid of the organic semiconductor, the organic semiconductor is electrophoretically deposited in a hole of the template under the action of electric-field intensity of 5V/cm-100V/cm, and the nano-wire containing the inorganic/organic heterojunction is obtained. By adopting the preparation method, the selection range of the organic nano-wire is extended. The method has simple operation, is easily combined with the existing semiconductor processing technology and realizes the scale preparation of the devices.
Description
Technical field
The present invention relates to contain the preparation method of inorganic/organic heterojunction nano wire.
Background technology
Heterojunction is being played the part of an important role in the conventional electrical device, it can be designed to various forms such as pn, pnp, npn, pin or pip as required, thereby brings into play various Core Feature effects.Since the eighties of last century the nineties, rise along with nanosecond science and technology, the nano wire that contains heterojunction more and more causes people's extensive concern, and these nano wires that contain heterojunction will play an important role in fields such as electronics, photoelectron, transducer, energy conversion.
Up to the present, the relevant both at home and abroad patent application that contains the heterojunction nano-wire preparation mainly concentrates on and contains inorganic/inorganic heterogeneous nano wire.In application for a patent for invention " manufacture method of nanostructure and nano wire reaches the device by its manufacturing " literary composition that on August 1st, 2007, disclosed publication number was CN101009214, the preparation method that several preparations contain heterojunction structure nanometer wire is disclosed, a kind of method wherein is dissolving first gas reactant in catalyst liquid, grow first section, in described catalyst liquid, dissolve second gas reactant, second section of growing different then again with the composition of described first section connection.
The report that relevant preparation contains organic-inorganic heterogeneous nano wire is fewer, " American Chemical Society's magazine (J.Am.Chem.Soc) " discloses one piece and has been entitled as " the article of the organic/inorganic P-N junction nanowire of photocontrol (Light-Controlled Organic/InorganicP-N Junction Nanowires); and enclosed a kind of method for preparing inorganic/organic heterojunction nano wire in the supplementary material of this article; inorganic nanowires wherein and organic nano line all generate by being electrochemically-deposited in the porous alumina formwork; inorganic fragment wherein is a cadmium sulfide, and organic fragment is a polypyrrole on 130 phase 9198-9199 pages or leaves in 2008.Wherein oxidative polymerization takes place by pyrrole monomer and obtains in polypyrrole in electrochemical deposition process.In this piece article, Special attention will be given to the preparation method and the performance test of single nano-wire.
Summary of the invention
The purpose of this invention is to provide the method that a kind of preparation contains inorganic/organic heterojunction nano wire, in the method, the use combined together of electrochemical deposition and electrophoretic deposition.
In this article, " electrochemical deposition " is defined as material in the solution by deposit the process that generates novel substance in electrode surface generation redox reaction; " electrophoretic deposition " is defined as outside under the effect of electric field, and the charged particle in the solution (as molecule) is directed to be moved, and in the process of electrode surface deposition, in this course, charged particle is not in electrode surface generation redox reaction; " inorganic compound semiconductor " herein is defined as the inorganic compound with semiconductor property that is made of two kinds and two or more element; " organic semiconductor " is defined as the organic compound with semiconductor property." inorganic semiconductor electrochemical deposition liquid " refers to electrochemical deposition inorganic semiconductor desired material is dissolved in formed solution in the solvent; " organic semiconductor electrophoretic deposition liquid " refers to the solution that contains organic semiconductor molecule that is used for electrophoretic deposition, the organic molecule that deposits need have electric charge, if the neutral of this organic molecule own, can be by in solution, adding suitable material, as add acid and make organic molecule protonated, and make it be with electric charge; Perhaps by the method for chemical modification, make this minute subband lotus group that powers on, satisfy the requirement of electrophoresis.
The method of one aspect of the present invention provides a kind of preparation to contain inorganic/organic heterojunction nano wire, this method may further comprise the steps:
A. at first prepare inorganic compound semiconductor electrochemical deposition liquid and organic semiconductor electrophoretic deposition liquid, contain 1 in the described organic semiconductor electrophoretic deposition liquid) not modified small molecule organic semiconductor compound, make the protonated acid of this compound and can dissolve the solvent of above-mentioned two kinds of compounds, perhaps 2) modified small molecule organic semiconductor compound and can dissolve the solvent of this compound, perhaps 3) macromolecule organic semiconductor compound and can dissolve or disperse the solvent of this compound;
B. the foraminous die plate with metal-plated membrane is a work electrode, carries out electrochemical deposition in the inorganic semiconductor electrochemical deposition liquid, obtains the partially filled template that inorganic semiconductor nanowires is arranged;
C. the partially filled clean and drying of template that inorganic semiconductor nanowires is arranged that step b is obtained, again this template is placed the organic semiconductor electrophoretic deposition liquid, under the effect of 5V/cm-100V/cm electric field strength, electrophoretic deposition organic semiconductor compound in the hole of this template obtains containing inorganic/organic heterojunction nano wire.In this step, both can remove template and obtain discrete nano wire; Also can not remove template, the template that will contain inorganic/organic heterojunction nano wire is done as a whole, is used for next step device configuration.
The deposition of inorganic nanowires in template realizes that by electrochemical deposition method this is identical with prior art among the present invention.Yet, the organic nano line is that method by electrophoretic deposition forms among the present invention, the redox reaction that in the process of this deposition, does not have the generating electrodes surface, be fit to deposition micromolecule and synthetic in advance macromolecule organic semiconductor compound, described organic small molecular semiconductor compound can be that the process modification also can be not modified.The preparation that prior art provided is inorganic/and there is certain limitation in the method for the organic fragment of organic heterojunction nano wire, it be by in the oxidation reaction of electrode surface by the on-the-spot synthetic organic polymer semiconducting compound of small molecule monomer, be not suitable for depositing and synthesize good organic polymer semiconducting compound, also be not suitable for depositing through modifying or not modified small molecule organic semiconductor compound by other method.Therefore, the present invention utilizes electrophoresis method, has expanded in inorganic/organic heterojunction nano wire the range of choice as the organic fragment nano-material.
Preferably, described step c is further comprising the steps of:
D. the partially filled clean and drying of template that inorganic semiconductor nanowires is arranged that step b is obtained, again dried template is placed first kind of organic semiconductor electrophoretic deposition liquid, under the effect of 5V/cm-100V/cm electric field strength, to first section organic semiconductor compound of this template deposition;
E. again this template is placed the electrophoretic deposition liquid of another organic molecule, under the effect of 5V/cm-100V/cm electric field strength, deposit second kind of organic nano line fragment;
F. repeating step e obtains containing inorganic/organic heterojunction nano wire.The organic nano line part of the inorganic/organic heterojunction nano wire that obtains in this way can comprise the different organic nano line of multilayer.
Preferably, in described step b, use the method for constant current electrochemical deposition, constant voltage electrochemical deposition or pulse voltage electrochemical deposition in the foraminous die plate of metal-plated membrane, to deposit the inorganic semiconductor nano wire.The size of deposition voltage and electric current depends on the material that will deposit.
Preferably, not modified small molecule organic semiconductor compound described in the step a is phthalocyanine or porphyrin compound, making the protonated acid of not modified small molecule organic semiconductor compound is trifluoroacetic acid, and the described solvent that can dissolve above-mentioned two kinds of compounds is carrene or chloroform.The effect that makes the protonated acid of not modified small molecule organic semiconductor compound is to make phthalocyanine and porphyrin compound be with electric charge by protonated, thereby makes electrophoresis process become possibility.
Preferably, not modified small molecule organic semiconductor compound or the modified concentration of small molecule organic semiconductor compound in the organic semiconductor electrophoretic deposition liquid are 0.1mM-1mM among the step a.
Preferably, making the protonated concentration of acid in the organic semiconductor electrophoretic deposition liquid of not modified small molecule organic semiconductor compound in described step a is 0.1M-1M.
Preferably, the inorganic compound semiconductor of inorganic compound semiconductor for obtaining among the step a with electrochemical deposition method.
Preferred inorganic compound semiconductor is an oxide semiconductor, sulfide semiconductor, selenide semiconductor or tellurides as semiconductor.
Preferably, in described step a, modified small molecule organic semiconductor compound is to make electric charge group on the small molecule organic semiconductor compound band by chemical modification.The purpose of chemical modification is to avoid adding in the organic semiconductor electrophoretic deposition liquid making the protonated acid of this compound.
Preferably, described macromolecule organic semiconductor compound is polythiophene or polyaniline compound through chemical modification.Chemical modification makes on the macromolecule organic semiconductor compound band as chemical modification groups such as alkane chains, increasing its solubility in solvent, or makes it when increasing solubility, is with as sulfonic group, and electric charge groups such as carboxyl are beneficial to electrophoretic deposition.The strand of conducting polymer is rigidity comparatively, generally needs chemical modification, otherwise does not dissolve or be dispersed in the solvent.
Preferably, the foraminous die plate of described metal-plated membrane is the anodised aluminium foraminous die plate of metal-plated membrane or is grown in anodised aluminium foraminous die plate on the silicon base.The anodised aluminium foraminous die plate of metal-plated membrane is metal film/AAO structure, and the anodised aluminium foraminous die plate that is grown on the silicon base is silicon/metal film/AAO structure.
The method of beneficial effect of the present invention is that preparation provided by the invention contains inorganic/organic heterojunction nano wire is simple, with low cost, is easy to large-scale production.There is certain limitation in the method for the preparation that prior art provided contains inorganic/organic heterojunction nano wire: the preparation method of its organic nano line fragment be only applicable to by in the oxidation reaction of electrode surface by the on-the-spot synthetic high polymer semiconductor of small molecule monomer, be not suitable for depositing the small molecule organic semiconductor compound, also be not suitable for depositing synthetic in advance good macromolecule organic semiconductor compound.These have the micromolecule or the macromolecule organic semiconductor compound of special electricity and optical property, can't obtain with the method for electrochemistry polymerized in-situ, must be synthetic in advance with other modes.Here, electrophoresis method provides micromolecule that will synthesize in advance and macromolecule organic semiconductor to be assembled into approach in the heterojunction nano-wire, has expanded the range of choice of organic fragment material.Simultaneously, utilize electrophoresis method, can be as required, deposit multilayer organic molecule fragment, these fragments can constitute micromolecule/micromolecule interface, also can constitute micromolecule/macromolecule interfacial, this be existing method can't accomplish.In addition, electrochemical deposition involved in the present invention and electrophoresis method, can combine with ripe now semiconducter process, realize that required device is integrated, for example, utilize the anodised aluminium foraminous die plate (silicon/metal film/AAO structure) that is grown on the silicon base, inorganic/organic heterojunction nano wire can be integrated on the silicon base, for next step device manufacturing lays the first stone, these devices comprise opto-electronic conversion and photoelectric detector or the like.
Description of drawings
Fig. 1 represents to prepare the step that the present invention contains inorganic-organic heterojunction nano wire, wherein 1-hole; The aluminum oxide porous template of 2-metal-plated membrane; The 3-metal film; 4-inorganic semiconductor nano wire fragment; 5-organic semiconductor nano wire fragment.
Fig. 2 represents that embodiment 1 removes the Bi that contains after the template
2Te
3The photograph of the nano wire of/CuPc heterojunction.
Embodiment
Embodiment 1
Te powder, Bi powder are dissolved in the 1M nitric acid, are configured to solution A, wherein the concentration of Te element is 0.013M in the solution, and the concentration of Bi element is 0.01M; CuPc (the English CuPc that is called for short), trifluoroacetic acid are dissolved in the dichloromethane solvent, make solution B, wherein the concentration of CuPc is 0.5mM, and the concentration of trifluoroacetic acid is 1M.At first at one side (the English AAO template that is called for short) the plated with gold film of aluminum oxide porous template, the diameter of the nano-pore of template is 200 nanometers, and thickness is 70 microns.The AAO template is placed the three-electrode system of A solution, under constant potential V=-0.15V (with respect to saturated calomel electrode) condition, in the AAO template, deposit Bi earlier
2Te
3The nano wire segment will deposit Bi
2Te
3The AAO template of nano wire fragment is taken out from solution, washs this template with distilled water and ethanol, it is dried in 60 ℃ baking oven again; Template after will drying again places B solution electrophoretic deposition CuPc organic semiconductor compound, and electric field strength is controlled at 20V/cm.After reaction is finished, remove the AAO template, can be with 1000 times of observation by light microscope to containing Bi
2Te
3The nano wire of/CuPc heterojunction.Accompanying drawing 2 has shown a such example, and wherein the light/dark balance of arrow indication nano wire partly is CuPc, and aterrimus partly is Bi
2Te
3
Te powder, Bi powder are dissolved in the 1M nitric acid, are configured to solution A, wherein the concentration of Te element is 0.013M in the solution, and the concentration of Bi element is 0.01M; Porphyrin and trifluoroacetic acid are dissolved in the chloroform solvent, make solution B.At first the AAO template one side plated with gold film, the diameter of nano-pore is 200 nanometers, thickness is 70 microns.The AAO template is placed the three-electrode system of A solution, under constant potential V=-0.15V (with respect to saturated calomel electrode) condition, in the AAO template, deposit Bi earlier
2Te
3The nano wire segment is taken out the AAO template that has deposited Bi2Te3 nano wire fragment from solution, wash this template with distilled water and ethanol, it is dried in 60 ℃ baking oven again; Template after will drying again places B solution electrophoretic deposition porphyrin organic semiconductor compound, and electric field strength is controlled at 40V/cm.Can obtain Bi
2Te
3/ porphyrin nano linear array.
Claims (10)
1. one kind prepares the method that contains inorganic/organic heterojunction nano wire, and this method may further comprise the steps:
A. at first prepare inorganic compound semiconductor electrochemical deposition liquid and organic semiconductor electrophoretic deposition liquid, contain 1 in the described organic semiconductor electrophoretic deposition liquid) not modified small molecule organic semiconductor compound, make the protonated acid of this compound and can dissolve the solvent of above-mentioned two kinds of compounds, perhaps 2) modified small molecule organic semiconductor compound and can dissolve the solvent of this compound, perhaps 3) macromolecule organic semiconductor compound and can dissolve or disperse the solvent of this compound;
B. the foraminous die plate with metal-plated membrane is a work electrode, carries out electrochemical deposition in the inorganic semiconductor electrochemical deposition liquid, obtains the partially filled template that inorganic semiconductor nanowires is arranged;
C. the partially filled clean and drying of template that inorganic semiconductor nanowires is arranged that step b is obtained, again this template is placed the organic semiconductor electrophoretic deposition liquid, under the effect of 5V/cm-100V/cm electric field strength, electrophoretic deposition organic semiconductor compound in the hole of this template obtains containing inorganic/organic heterojunction nano wire.
2. method according to claim 1 may further comprise the steps in described step c:
D. the partially filled clean and drying of template that inorganic semiconductor nanowires is arranged that step b is obtained, again dried template is placed first kind of organic semiconductor electrophoretic deposition liquid, under the effect of 5V/cm-100V/cm electric field strength, to first section organic semiconductor compound of this template deposition;
E. again this template is placed the electrophoretic deposition liquid of another organic molecule, under the effect of 5V/cm-100V/cm electric field strength, deposit second kind of organic nano line fragment;
F. repeating step e obtains containing inorganic/organic heterojunction nano wire.
3. method according to claim 1 and 2 wherein in described step b, uses the method for constant current electrochemical deposition, constant voltage electrochemical deposition or pulse voltage electrochemical deposition to deposit the inorganic semiconductor nano wire in the foraminous die plate of metal-plated membrane.
4. according to each described method among the claim 1-3, wherein the not modified small molecule organic semiconductor compound described in the step a is phthalocyanine or porphyrin compound, making the protonated acid of not modified small molecule organic semiconductor compound is trifluoroacetic acid, and the described solvent that can dissolve above-mentioned two kinds of compounds is carrene or chloroform.
5. according to each described method among the claim 1-4, wherein not modified small molecule organic semiconductor compound or the modified concentration of small molecule organic semiconductor compound in the organic semiconductor electrophoretic deposition liquid are 0.1mM-1mM among the step a.
6. according to each described method among the claim 1-5, making the protonated concentration of acid in the organic semiconductor electrophoretic deposition liquid of not modified small molecule organic semiconductor compound among the wherein said step a is 0.1M-1M.
7. according to each described method among the claim 1-6, wherein the inorganic compound semiconductor described in the step a is the inorganic compound semiconductor that obtains with electrochemical deposition method, preferred oxides semiconductor, sulfide semiconductor, selenide semiconductor or tellurides as semiconductor.
8. according to each described method among the claim 1-7, wherein in described step a, modified small molecule organic semiconductor compound is to make electric charge group on the small molecule organic semiconductor compound band by chemical modification.
9. according to each described method among the claim 1-8, wherein said macromolecule organic semiconductor compound is polythiophene or polyaniline compound through chemical modification.
10. according to each described method among the claim 1-9, the foraminous die plate of wherein said metal-plated membrane is the anodised aluminium foraminous die plate of metal-plated membrane or is grown in anodised aluminium foraminous die plate on the silicon base.
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Cited By (6)
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| CN102642809A (en) * | 2012-04-27 | 2012-08-22 | 中国科学院理化技术研究所 | Organic nanowire/metal nano particle composite nano material and preparation method thereof |
| CN103503134A (en) * | 2011-05-17 | 2014-01-08 | 麦克马斯特大学 | Light emitting diodes and substrates |
| CN103503134B (en) * | 2011-05-17 | 2016-11-30 | 麦克马斯特大学 | Light emitting diode and substrate |
| CN108456908A (en) * | 2018-02-08 | 2018-08-28 | 北京航空航天大学 | A kind of preparation and application of the porphyrin based on self assembly/alumina composite nanochannel film |
| CN109841736A (en) * | 2018-11-21 | 2019-06-04 | 华东理工大学 | One kind accurately constructing organic heterojunction resistive memory and its application based on electrochemical method |
| 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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| US6465132B1 (en) * | 1999-07-22 | 2002-10-15 | Agere Systems Guardian Corp. | Article comprising small diameter nanowires and method for making the same |
| CN101009214B (en) * | 2001-03-30 | 2010-05-19 | 加利福尼亚大学董事会 | Methods of fabricating nanostructures and nanowires and devices fabricated therefrom |
| CN100473422C (en) * | 2006-12-31 | 2009-04-01 | 厦门大学 | Preparation method of nanometer ordered structure biomaterial membranous layer based on super hydro philic/hydro phobic characteristic template |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103503134A (en) * | 2011-05-17 | 2014-01-08 | 麦克马斯特大学 | Light emitting diodes and substrates |
| US9257601B2 (en) | 2011-05-17 | 2016-02-09 | Mcmaster University | Light emitting diodes and substrates |
| CN103503134B (en) * | 2011-05-17 | 2016-11-30 | 麦克马斯特大学 | Light emitting diode and substrate |
| CN102642809A (en) * | 2012-04-27 | 2012-08-22 | 中国科学院理化技术研究所 | Organic nanowire/metal nano particle composite nano material and preparation method thereof |
| CN108456908A (en) * | 2018-02-08 | 2018-08-28 | 北京航空航天大学 | A kind of preparation and application of the porphyrin based on self assembly/alumina composite nanochannel film |
| CN108456908B (en) * | 2018-02-08 | 2019-08-27 | 北京航空航天大学 | A kind of preparation and application of the porphyrin based on self assembly/alumina composite nanochannel film |
| CN109841736A (en) * | 2018-11-21 | 2019-06-04 | 华东理工大学 | One kind accurately constructing organic heterojunction resistive memory and its application based on electrochemical method |
| 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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