CN103943778A - Method for preparing cross nanofiber P-N heterojunction array - Google Patents

Method for preparing cross nanofiber P-N heterojunction array Download PDF

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CN103943778A
CN103943778A CN201410140100.4A CN201410140100A CN103943778A CN 103943778 A CN103943778 A CN 103943778A CN 201410140100 A CN201410140100 A CN 201410140100A CN 103943778 A CN103943778 A CN 103943778A
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nanofiber
spinning
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zno
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CN103943778B (en
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龙云泽
陈帅
盛琛皓
韩文鹏
董瑞华
张红娣
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Qingdao University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
    • H10K10/20—Organic diodes
    • H10K10/29—Diodes comprising organic-inorganic heterojunctions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

Abstract

The invention belongs to the technical field of cross nanofiber preparation, and relates to a method for preparing a cross nanofiber P-N heterojunction array. The method includes the steps of firstly, depositing a layer of P type or N type nanofiber array with the controllable fiber number and the controllable interval on a collector of a three-dimensional adjustable low-voltage near-field in-situ electrostatic spinning device; secondly, rotating the collector by a certain angle; thirdly, depositing a layer of N type or P type orderly-arrayed nanofiber array through the three-dimensional adjustable low-voltage near-field in-situ electrostatic spinning device, and obtaining the cross nanofiber P-N heterojunction array on the collector. The method is simple, scientific and reliable in theory, high in efficiency, accurate in accuracy control, beneficial to large-scale production and environmentally friendly.

Description

A kind of preparation method of intersecting nanofiber P-N heterojunction array
Technical field:
The invention belongs to and intersect nanofiber preparing technical field, a kind of particularly method of the fiber of assemble nanometer accurately and fast chi structure P-N heterojunction array, particularly a kind of preparation method of intersecting nanofiber P-N heterojunction array.
Background technology:
The application of nanometer technology in electronic device is one of micro-nano electronics focus of becoming gradually current nanosecond science and technology research, and according to bibliographical information, scientific research personnel has for example prepared, based on zero-dimension nano particle (single organic molecule, quantum dot, C at present 60), the multiple nano-device (for example diode, triode, sensor) of 1-dimention nano fiber (for example single-root carbon nano-tube, organic or inorganic semiconductor nano fiber/nanotube), two-dimensional nano film (for example Graphene), particularly 1-dimention nano fiber/nanotube is the smallest dimension structure of effectively transmission charge, the role who simultaneously takes on wire and device cell.Because P-N knot is the basis of constructing complex semiconductor devices, except the electronic device building based on single nanofiber and homogeneous material nanofiber array, scientific research personnel is also devoted to assemble the nanofiber P-N heterojunction that different materials forms, nanofiber P-N heterojunction mainly contains three kinds: the one, and axial arrangement, the one end that is nanofiber is P type, and the other end is N-type; The 2nd, radial structure, i.e. P(or N) coated outside of type nanofiber one deck N-type (or P) semiconductor, forms coaxial composite nano fiber; The 3rd, chi structure, P type and N-type nanofiber intersect to form.With the heterogeneous example of becoming of nanofiber chi structure P-N; dissimilar nanofiber forms chi structure often can show the not available unique electrical of homogeneous material, optics and chemical property; the for example Lieber of Harvard University seminar [Nature409,66 (2001); Science291,851 (2001); Science294,1313 (2001)] utilize the technology such as fluid NW-TFT, electric field NW-TFT to assemble multiple chi structure P-N heterojunction nano-wire (P type Si nano wire from bottom to top, N-type InP, GaN, CdS and CdSe nano wire) device and circuit, for example nano luminescent diode [Small1,142 (2005)], intersection nano-wire field effect transistor, nanometer gate, nanocomputer [www.pnas.org/cgi/doi/10.1073/pnas.1323818111] etc.; Except common inorganic semiconductor nano wire, also can build chi structure P-N heterojunction electronic logic circuit [Advanced Materials21,4234 (2009)] with organic crystal nano wire.Although nanofiber chi structure P-N heterojunction is more easily processed into nano luminescent diode, rectifier diode, the single nano-device such as field-effect transistor, and form simple logic electronics circuit (for example AND gate than being easier to assembling, OR-gate, inverter etc.), aspect complicated nano electron device, more there iing application prospect, but because single nanofiber chi structure P-N heterojunction device also has suitable distance from practical nanoelectronic circuits, how by extensive single P-N heterojunction nano-device, accurately, the ordered fabrication practical function circuit that gets up is still a challenge.At present the method for assemble nanometer fiber chi structure P-N heterojunction comprises that microfluid NW-TFT, electric field or magnetic field assists assembling, L B film technology, microprobe and optical tweezer technology, and these assemble methods exist the problem that packaging efficiency is low, can not accurately control.In addition, Chinese patent (patent No.: ZL201010184093.X) discloses a kind of directed electrochemical deposition method original position and has prepared conductive polymer nanometer line chi structure heterojunction, and the method efficiency is lower, is difficult to scale preparation.
Electrostatic spinning be a kind of simple effectively, utilize the technology of even, the continuous superfine fibre of the fairly large preparation of electrostatic field, by conventional electrostatic device for spinning is improved, can regulate and control the appearance structure of the electrospinning fibre of preparation, for example, the centrifugal electrostatic spinning apparatus (patent No.: ZL201010184068.1) that applicant proposes and two framework are collected electrostatic spinning apparatus (patent No.: ZL201110137420.0) and can be prepared the electrospinning fibres such as orderly arrangement architecture, chi structure, spiral winding structure.Although above-mentioned improved electric spinning equipment can rapid-assembling chi structure fiber, due to distant (several centimetres to tens centimetres) of spinneret and collecting board, distance between radical, the parallel fibers of the deposition position of nanofiber on collecting board, deposit fiber, the angle etc. of nanofiber of intersecting can't accurately be controlled.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, seek design a kind of method of utilizing three-dimensional adjustable low-voltage near field original position electrostatic spinning technique to prepare accurately and fast intersection nanofiber P-N heterojunction array is provided, the nanofiber chi structure heterojunction of can assemble in situ organic-organic, organic-inorganic, inorganic-inorganic multiple material, promotes the development of the nanofiber heterojunction nano-devices such as conducting polymer, organic crystal, metal and inorganic semiconductor and electronic logic circuit.
To achieve these goals, the present invention realizes in the adjustable low-voltage near field original position of three-dimensional electrostatic spinning apparatus, and its concrete preparation process is:
(1), ZnO spinning precursor solution preparation: by 8.5 grams of absolute ethyl alcohols and at room temperature mix and blend 2-4 hour of 1.5 grams of polyvinylpyrrolidones (PVP), obtain the transparent 15wt%PVP solution of homogeneous; Again 1.0 grams of zinc acetates, 2.0 grams of absolute ethyl alcohols, 0.2 gram of distilled water are mixed and heated to 60-80 DEG C of stirring and within 8-12 minute, obtain mixed solution, after solid dissolves completely, mixed solution is all transferred in 15wt% polyvinylpyrrolidone (PVP) solution having prepared, at room temperature stir and within 50-70 minute, make two kinds of solution fully mix, obtain ZnO spinning precursor solution;
(2), electrospinning ZnO nano fiber array: the ZnO presoma nanofiber array of electrospinning one deck ordered arrangement on collector, the distance of adjusting spinning head and collector is 1-2 millimeter, the speed that moves horizontally of collector is 50-100 cel, spinning voltage is 1-2 kilovolt, and the speed of flow control pump is micro-l/h of degree 50-100; Then collector is removed to organic principle in heat treatment 3-4 hour at 600-700 DEG C, on collector, obtain ZnO nano fiber array;
(3), PEDOT spinning precursor solution preparation: be 2.8wt%PEDOT/PSS(poly-(3 by 1.0 grams of PVP powder, 3.0 gram weight percentages, 4-dioxoethyl thiophene)-polystyrolsulfon acid) the aqueous solution and 2 grams of absolute ethyl alcohols mix, then add 0.2 gram of dimethyl sulfoxide (DMSO), at room temperature magnetic agitation 4-6 hour, solution is mixed, obtain the PEDOT spinning precursor solution of homogeneous;
(4), electrospinning PEDOT-ZnO intersection nanofiber heterojunction array: the collector rotation 0-180 degree that will deposit ZnO nano fiber array, and then on collector the PEDOT nanofiber of electrospinning one deck ordered arrangement, electrospinning condition is identical with step (2), obtains PEDOT-ZnO intersection nanofiber P-N heterojunction array.
The agent structure of the adjustable low-voltage near field original position of the three-dimensional electrostatic spinning apparatus the present invention relates to comprises flow control pump, spinning head, high voltage source, computer and collector; Spinning head is electrically connected with the positive pole of flow control pump and high voltage source respectively, the flow velocity of precursor solution in flow control pump control spinning head, and high voltage source provides spinning voltage for spinning head; Collector is arranged on 0.5-5 millimeter place, spinning head below, and collector is connected with the negative electricity of computer and high voltage source respectively, the motion of computer control collector, and collector adopts SiO 2/ Si substrate.
The present invention compared with prior art has following characteristics and advantage: the one, and electrostatic spinning process, by computer control, ensures the deposition accurately and fast of electrospinning fibre and number and the spacing of deposit fiber; The 2nd, electrospinning fibre can be chosen multiple P type and n type material is assembled, and can build as required organic-organic, organic-inorganic and inorganic-inorganic heterogeneous, ensures flexibility and the diversity of P-N intersection heterojunction; The 3rd, can make arbitrarily as required the chi structure P-N heterojunction array device of n × m, form addressable transducer or simple logic electronics circuit; Its preparation method is simple, and principle science is reliable, and efficiency is high, and precision precise control, is easy to large-scale production, environmental friendliness.
Brief description of the drawings:
Fig. 1 is the agent structure principle schematic of the adjustable low-voltage near field original position of the three-dimensional electrostatic spinning apparatus that the present invention relates to.
Fig. 2 is the flow process principle schematic that the present invention prepares intersection nanofiber P-N heterojunction array.
Embodiment:
Also be described further by reference to the accompanying drawings below by embodiment.
Embodiment:
The present embodiment adopts three-dimensional adjustable low-voltage near field original position electrostatic spinning apparatus to realize the preparation of intersection nanofiber P-N heterojunction array, with conducting polymer PEDOT(poly-3,4-dioxoethyl thiophene, p-type organic semiconductor) and ZnO(n type metal oxide inorganic semiconductor) be raw material preparation intersection nanofiber P-N heterojunction array, its concrete preparation process is:
(1), ZnO spinning precursor solution preparation: by 8.5 grams of absolute ethyl alcohols and at room temperature mix and blend 2-4 hour of 1.5 grams of polyvinylpyrrolidones (PVP), obtain the transparent 15wt%PVP solution of homogeneous; Again 1.0 grams of zinc acetates, 2.0 grams of absolute ethyl alcohols, 0.2 gram of distilled water are mixed and heated to 60-80 DEG C of stirring and within 8-12 minute, obtain mixed solution, after dissolving completely, solid mixed solution is all transferred in the 15wt%PVP solution having prepared, at room temperature stir and within 50-70 minute, make two kinds of solution fully mix, obtain ZnO spinning precursor solution;
(2), electrospinning ZnO nano fiber array: the ZnO presoma nanofiber array of electrospinning one deck ordered arrangement on collector, the distance of adjusting spinning head and collector is 1-2 millimeter, the speed that moves horizontally of collector is 50-100 cel, spinning voltage is 1-2 kilovolt, and the speed of flow control pump is micro-l/h of degree 50-100; Then collector is removed to organic principle in heat treatment 3-4 hour at 600-700 DEG C, on collector, obtain pure ZnO nano fiber array;
(3), PEDOT(poly-(3,4-dioxoethyl thiophene)) preparation of spinning precursor solution: be 2.8wt%PEDOT/PSS(poly-(3 by 1.0 grams of PVP powder, 3.0 gram weight percentages, 4-dioxoethyl thiophene)-polystyrolsulfon acid) the aqueous solution and 2 grams of absolute ethyl alcohols mix, then add 0.2 gram of dimethyl sulfoxide (DMSO), at room temperature magnetic agitation 4-6 hour, solution is mixed, obtain the PEDOT spinning precursor solution of homogeneous;
(4), electrospinning PEDOT-ZnO intersection nanofiber heterojunction array: will deposit the collector 90-degree rotation of ZnO nano fiber array, and then on collector the PEDOT nanofiber of electrospinning one deck ordered arrangement, electrospinning condition is identical with step (2), obtains PEDOT-ZnO intersection nanofiber P-N heterojunction array.
The agent structure of the adjustable low-voltage near field original position of the three-dimensional electrostatic spinning apparatus that the present embodiment relates to comprises flow control pump 1, spinning head 2, high voltage source 3, computer 4 and collector 5; Spinning head 2 is electrically connected with the positive pole of flow control pump 1 and high voltage source 3 respectively, and flow control pump 1 is controlled the flow velocity of spinning head 2 interior precursor solutions, and high voltage source 3 provides spinning voltage for spinning head 2; Collector 5 is arranged on spinning head 2 0.5-5 millimeter places, below, and collector 5 is connected with the negative electricity of computer 4 and high voltage source 3 respectively, and computer 4 is controlled the motion of collector 5, and collector 5 adopts SiO 2/ Si substrate.
The present embodiment adopts said method also can assemble accurately and fast other organic-inorganic, inorganic-inorganic and organic-organic nanofibers chi structure heterojunction array, for example PEDOT-TiO 2, PEDOT-BaTiO 3, P-type conduction polyaniline or polypyrrole-N-type ZnO, TiO 2or BaTiO 3and P type ZnO-N-type TiO 2or BaTiO 3.
PEDOT-ZnO intersection nanofiber P-N the heterojunction array of the present embodiment to preparation carries out microelectrode processing and performance measurement, the method that the nanofiber heterojunction array microelectrode that intersects is processed mainly contains two kinds: the one, first on collector, make metal microelectrode array, then with low-voltage near field original position electrostatic spinning apparatus accurate deposition intersection nanofiber between microelectrode; The 2nd, first on collector, deposit and intersect nanofiber array, and then make metal microelectrode with micro-processing technology; On this basis, can make single chi structure P-N heterojunction device, directly measure and study electricity, photoelectricity and the sensing capabilities of single chi structure P-N heterojunction device; In addition, can make the chi structure P-N heterojunction array of n × m, for example diode and transistor array form addressable transducer or simple logic electronics circuit.

Claims (2)

1. intersect the preparation method of nanofiber P-N heterojunction array, it is characterized in that realizing in the adjustable low-voltage near field original position of three-dimensional electrostatic spinning apparatus, its concrete preparation process is:
(1), ZnO spinning precursor solution preparation: by 8.5 grams of absolute ethyl alcohols and 1.5 grams of at room temperature mix and blend 2-4 hour of polyvinylpyrrolidone, obtain the transparent 15wt% polyvinylpyrrolidonesolution solution of homogeneous; Again 1.0 grams of zinc acetates, 2.0 grams of absolute ethyl alcohols, 0.2 gram of distilled water are mixed and heated to 60-80 DEG C of stirring and within 8-12 minute, obtain mixed solution, after dissolving completely, solid mixed solution is all transferred in the 15wt% polyvinylpyrrolidonesolution solution having prepared, at room temperature stir and within 50-70 minute, make two kinds of solution fully mix, obtain ZnO spinning precursor solution;
(2), electrospinning ZnO nano fiber array: the ZnO presoma nanofiber array of electrospinning one deck ordered arrangement on collector, the distance of adjusting spinning head and collector is 1-2 millimeter, the speed that moves horizontally of collector is 50-100 cel, spinning voltage is 1-2 kilovolt, and the speed of flow control pump is micro-l/h of degree 50-100; Then collector is removed to organic principle in heat treatment 3-4 hour at 600-700 DEG C, on collector, obtain ZnO nano fiber array;
(3), PEDOT spinning precursor solution preparation: by poly-(3 of 1.0 grams of polyvinylpyrrolidonepowder powder, 3.0 grams of 2.8wt%, 4-dioxoethyl thiophene)-polystyrolsulfon acid the aqueous solution and 2 grams of absolute ethyl alcohols mixing, then add 0.2 gram of dimethyl sulfoxide (DMSO), at room temperature magnetic agitation 4-6 hour, solution is mixed, obtain the PEDOT spinning precursor solution of homogeneous;
(4), electrospinning PEDOT-ZnO intersection nanofiber heterojunction array: the collector rotation 0-180 degree that will deposit ZnO nano fiber array, and then on collector the PEDOT nanofiber of electrospinning one deck ordered arrangement, electrospinning condition is identical with step (2), obtains PEDOT-ZnO intersection nanofiber P-N heterojunction array.
2. the preparation method of intersection nanofiber P-N heterojunction array according to claim 1, is characterized in that the agent structure of the adjustable low-voltage near field original position of the three-dimensional relating to electrostatic spinning apparatus comprises flow control pump, spinning head, high voltage source, computer and collector; Spinning head is electrically connected with the positive pole of flow control pump and high voltage source respectively, the flow velocity of precursor solution in flow control pump control spinning head, and high voltage source provides spinning voltage for spinning head; Collector is arranged on 0.5-5 millimeter place, spinning head below, and collector is connected with the negative electricity of computer and high voltage source respectively, the motion of computer control collector, and collector adopts SiO 2/ Si substrate.
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US10792658B2 (en) 2014-12-08 2020-10-06 Berkeley Lights, Inc. Lateral/vertical transistor structures and process of making and using same
CN104638019B (en) * 2015-02-02 2017-07-25 青岛大学 A kind of zinc oxide nano fiber homogeneity p n junction devices and preparation method thereof
CN104638019A (en) * 2015-02-02 2015-05-20 青岛大学 Zinc oxide nanofiber homogeneous p-n junction device and preparation method thereof
CN104966781A (en) * 2015-05-04 2015-10-07 青岛大学 Perovskite nanometer fiber film solar cell and preparation method thereof
CN104966781B (en) * 2015-05-04 2018-04-17 青岛大学 A kind of perovskite nanofiber film solar cell and preparation method thereof
CN105350112A (en) * 2015-12-07 2016-02-24 哈尔滨工业大学 Preparation method of polythiophene-type high-molecular/inorganic semi-conductor bulk-heterojunction nano-fiber
CN105702772A (en) * 2016-04-07 2016-06-22 姜凯 One-dimensional array nanowires based ultraviolet light detector
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CN107068864A (en) * 2017-04-14 2017-08-18 武汉华星光电技术有限公司 The preparation method of OTFT
CN110699764A (en) * 2019-10-30 2020-01-17 大连理工大学 Device for preparing controllable arrangement nano fibers based on NPN type triode
CN114047231A (en) * 2021-11-04 2022-02-15 湖州师范学院 Diode type heterojunction gas sensor chip and preparation method thereof
CN114047231B (en) * 2021-11-04 2024-02-27 湖州师范学院 Diode type heterojunction gas sensor chip and preparation method thereof
CN115140704A (en) * 2022-09-05 2022-10-04 北京仿生界面科学未来技术研究院 Method for preparing cross-stacked heterostructure array

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