CN103441216A - Ultraviolet light detector based on titanium dioxide nanometer bowl array and manufacturing method thereof - Google Patents

Ultraviolet light detector based on titanium dioxide nanometer bowl array and manufacturing method thereof Download PDF

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CN103441216A
CN103441216A CN2013103848802A CN201310384880A CN103441216A CN 103441216 A CN103441216 A CN 103441216A CN 2013103848802 A CN2013103848802 A CN 2013103848802A CN 201310384880 A CN201310384880 A CN 201310384880A CN 103441216 A CN103441216 A CN 103441216A
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ultraviolet light
film
light detector
bowl array
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阮圣平
孟凡旭
周敬然
刘彩霞
温善鹏
董玮
张歆东
郭文滨
沈亮
李质奇
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Jilin University
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Abstract

The invention provides an ultraviolet light detector based on a titanium dioxide nanometer bowl array and a manufacturing method of the ultraviolet light detector and belongs to the technical field of organic photoelectric devices. The manufacturing method comprises the following steps that firstly, the titanium dioxide nanometer bowl array serving as an electron acceptor is generated on conducting glass according to the sol-gel method and the PS ball template method; secondly, a PVK film serving as an electron donor is manufactured on the titanium dioxide nanometer bowl array according to the solution spin coating method; thirdly, a tungsten trioxide film serving as a hole transporting layer is manufactured on an active layer according to the vacuum vapour deposition method; finally, a metal film serving as a top electrode is manufactured on the tungsten trioxide film according to the vacuum vapour deposition method. The organic and inorganic hybridized ultraviolet light detector has the advantages of being simple in manufacturing method and low in cost, enabling the large-area film to be formed and having the obvious spectrum selection character.

Description

A kind of based on TiO 2ultraviolet light detector of nano bowl array and preparation method thereof
Technical field
The invention belongs to the organic electro-optic device technical field, be specifically related to a kind of Polyvinyl carbazole (PVK) as electron donor, titanium dioxide (TiO 2) nano bowl (nanobowls) array is as organic inorganic hybridization ultraviolet light detector of electron acceptor and preparation method thereof.
Background technology
Ultraviolet detector all has a wide range of applications at aspects such as national defense and military, ultraviolet astronomy, combustion enginnering, Missile Plume detection, ultraviolet alarm, biological cell canceration detection and the monitorings of turbine engine combustion efficiency, has become one of emphasis problem of many advanced countries research and development in the world.And the wide bandgap semiconductor base ultraviolet light detector has obtained in the photodetection field paying attention to widely and development at full speed due to advantages such as volume are little, efficiency is high, cost is low, low in energy consumption.
Semi-conducting material for ultraviolet light detector has much at present, mainly concentrates in the wide bandgap semiconductor materials such as carborundum (SiC), gallium nitride (GaN) and zinc oxide (ZnO).But it should be noted that, the spectral response range of most of ultraviolet light detector based on semiconductor material with wide forbidden band is wider, can't meet the demand of some special applications, as the detection of biological or chemical harmful substance in air, these harmful substances can give off the ultraviolet light of specific wavelength usually.In addition, the making of these devices needs the complicated like this technique of metalloid organic chemistry vapor phase deposition (MOCVD) or molecular beam epitaxy (MBE) usually, causes the device production cost higher.
Because the absorption spectrum of organic material can be regulated effectively by controlling molecular structure, the organic/inorganic semiconductor hybrid is together with the advantages of organic and inorganic semiconductor material, for the ultraviolet light detector that realizes having spectral selection provides relatively easy and research means cheaply.The PVK(Polyvinyl carbazole) be a kind of organic semiconducting materials with higher hole mobility, at 310～360nm wave band, there is very strong absorption.And TiO 2as a kind of inorganic N-type semiconductor material with wide forbidden band, it is cheap, has extraordinary weatherability, physics and chemistry stability, good photoelectric characteristic.By PVK and TiO 2combine and make the heterojunction of hybrid, utilize the mutual superposition of bi-material absorption spectrum, can develop the ultraviolet light detector with spectrum-selectivity characteristic.
In addition, by inorganic semiconductor material and the organic material of introducing low-dimensional, carry out hydridization, can increase the organic/inorganic contact interface, directed carrier transport path is provided, improve separation and the transmission of photogenerated charge, improve the performance of hydridization device.And the spectrum-selectivity characteristic that the special optical character (as the reflex for special wavelength) that the periodic structure of himself high-sequential has can be also ultraviolet light detector produces positive role.Therefore, by the TiO that PVK and polystyrene (PS) bead template synthesis are gone out 2the spectral selection ultraviolet light detector that nano bowl array hydridization is prepared has unique application prospect.
Summary of the invention
The object of the present invention is to provide a kind of PVK as electron donor, TiO 2the nano bowl array is as the organic inorganic hybridization ultraviolet light detector of electron acceptor and the preparation method of this ultraviolet light detector.
The present invention adopts PVK as electron donor material, TiO 2the nano bowl array is as electron acceptor material, and the double layer heterojunction that bi-material is made to hybrid, as active layer, is made ultraviolet light detector.By tin indium oxide (ITO), PVK, TiO 2the interaction of each layer film optical characteristics of nano bowl array, realize the spectrum-selectivity characteristic of ultraviolet light detector.
Ultraviolet light detector of the present invention is characterized in that: from the light incident direction, be followed successively by the ito glass substrate, as the triangular crystal lattice that is of electron acceptor, arrange closelypacked TiO 2nano bowl array (PS bead template and sol-gal process preparation), PVK film (preparation of solution spin-coating method), as the tungstic acid (WO of hole transmission layer 3) film (vacuum vapour deposition preparation), as the metallic film of top electrode (metal can be silver-colored Ag, aluminium Al, golden Au etc., the vacuum vapour deposition preparation).
Further, arrange closelypacked TiO for being triangular crystal lattice 2the nano bowl array, the internal diameter of bowl shaped structure unit is 360～390nm, spine is highly 50～80nm, spine's thickness is 90～120nm, bottom thickness is 30～60nm, the length of adjacent two bowl shaped structure unit circle center line connectings (being the lattice constant of triangular crystal lattice) is 420～440nm, and the thickness of PVK film is 100～150nm, WO 3the thickness of film is 10～15nm, and the thickness of metallic film is 50～60nm.
Of the present invention based on TiO 2the preparation process of the organic inorganic hybridization ultraviolet light detector of nano bowl array is as follows:
[1] ito glass is used acetone, isopropyl alcohol, deionized water ultrasonic cleaning successively, then dries;
[2] at room temperature, the mixed solution that the hydrochloric acid that is 0.28mol/L by 20～40mL ethanol, 10～20mL deionized water, 2～5mL concentration is made into dropwise splashes in the solution that contains 10～20mL butyl titanate, 50～60mL ethanol, 5～10mL acetylacetone,2,4-pentanedione, and with vigorous stirring 2～4 hours, and then make TiO 2colloidal sol;
[3] by TiO 2colloidal sol is spin-coated on ito glass with the rotating speed of 3000～5000rpm, then puts into Muffle furnace, and under 450～500 ℃ of conditions, sintering is 2～4 hours, forms Detitanium-ore-type TiO after sintering on ito glass 2nanocrystalline thin film (nc-TiO 2), thickness is 30～60nm; Wherein, sintering temperature is during lower than 450 ℃, TiO 2colloidal sol can not be transformed into TiO fully 2nanocrystal, during higher than 500 ℃, TiO 2the crystal formation of nanocrystal starts to change to rutile-type from Detitanium-ore-type.TiO 2the spin coating revolution of colloidal sol is higher, and the film thickness made is thinner.Experimental result shows, the spin coating revolution is between 3000～5000rpm the time, and the device performance made changes little.
[4] the PS bead that is 450nm by diameter (can obtain by purchase) be take (volume ratio of water and ethanol is 1:1～3) in the mixed solution of the water-soluble and ethanol of 3～5% mass ratio, and with microsyringe, this mixed solution slowly is expelled to the surface of water, it is freely disperseed, until the PS bead is paved with the whole water surface with individual layer; Then the surface that the lauryl sodium sulfate that is 1～3% by several mass ratioes (SDS) aqueous solution drips to water reduces the surface tension of water, the self assembly of individual layer bead is formed be triangular crystal lattice to arrange close-packed structure; Finally place 24 hours, make the bead sedimentation suspended in water, whole process all completes in enclosed environment;
[5] by the TiO sintered 2film inserts the previous step self assembly with the angle inclination of 30～40 degree to be had in the aqueous solution of PS bead, and the PS bead single thin film of self assembly on the water surface is slowly picked up, and then, under nitrogen protection, dries one hour, makes PS bead template for 70～90 ℃.Again will be with the TiO of PS bead template 2film vertically inserts TiO 2in colloidal sol 30 seconds～1 minute, make the Interglobular space of PS by TiO 2colloidal sol is filled full; Finally slowly propose and put into Muffle furnace, under 450～500 ℃ of conditions, sintering is 2～3 hours, and the PS bead is sintered carbonization and removes, and originally fills the TiO in space between bead 2colloidal sol is sintered into the TiO of ridged 2crystal, with following TiO 2crystal film is combined, thereby forms TiO 2the nano bowl array;
[6] the PVK chloroformic solution that is 10～15mg/mL by concentration is spin-coated on TiO with the rotating speed of 800～1000rpm 2on the nano bowl array, then put it into vacuum drying oven, dry under 90～110 ℃ 15～30 minutes, thereby obtain the PVK active layer film that thickness is 100～150nm;
The ito glass that [7] will have an active layer film is transferred in thermal evaporation system (the organic gas molecule in space depositing system of SD400B type multi-source temperature control), evaporation hole transmission layer and metal electrode in turn on the active layer film; Vapor deposition source is respectively WO 3powder, Ag, Al or Au powder, all can obtain by purchase, thereby prepare of the present invention based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array.
The accompanying drawing explanation
Fig. 1: the structural representation of device of the present invention;
Fig. 2: the present invention prepare based on TiO 2the light of the organic inorganic hybridization ultraviolet light detector of nano bowl array, dark current density characteristic curve;
Fig. 3: TiO prepared by the present invention 2the XRD figure of nano bowl array and SEM figure;
Fig. 3 (a) is TiO 2the XRD figure of nano bowl array;
Fig. 3 (b) is TiO 2the SEM figure of nano bowl array;
Fig. 4: TiO prepared by the present invention 2the schematic cross-section of nano bowl unit and based on TiO 2the section S EM figure of the organic inorganic hybridization ultraviolet light detector of nano bowl array;
Fig. 4 (a) is TiO 2the schematic cross-section of nano bowl unit;
Fig. 4 (b) is based on TiO 2the section S EM figure of the organic inorganic hybridization ultraviolet light detector of nano bowl array;
Fig. 5: PVK, TiO 2absorption spectrum and the transmitted spectrum of ITO;
Fig. 6: the present invention prepare based on TiO 2the spectral response characteristic curve of the organic inorganic hybridization ultraviolet light detector of nano bowl array under-5V bias voltage;
Fig. 7: TiO 2the reflectance spectrum of nano bowl array front and back.
As shown in Figure 1, device is by transparent cathode (ito glass) 1, TiO 2 nano bowl array 2, PVK film 3, WO 3 hole transmission layer 4, metal electrode 5 forms.Wherein transparent cathode 1 is used for conduction electron; TiO 2thereby nano bowl array 2 is used for absorbing photon and produces electron hole pair conduction electron; Thereby PVK film 3 is used for absorbing photon and produces exciton conduction hole; Hole transmission layer 4 be used for block electrons, collect hole, metal electrode 5 conduction holes.
As shown in Figure 2, unglazed, according under condition, the current density of device under-5V bias voltage is 7.97 μ A/cm 2; And be 144 μ W/cm in intensity 2the wavelength UV-irradiation that is 330nm under, the current density of device under-5V bias voltage is 1.17mA/cm 2.Calculating thus the light dark current ratio of device under-5V bias voltage is 147.
As shown in Figure 3, the TiO that prepared by the present invention 2the XRD figure of nano bowl array and SEM figure.Fig. 3 (a) and Fig. 3 (b) are respectively TiO prepared by the present invention 2the XRD figure of nano bowl array and SEM figure.From Fig. 3 (a), can find out, the crystal formation of sample is Detitanium-ore-type; Can find out TiO from Fig. 3 (b) 2the nano bowl diameter is about 375nm, is triangular crystal lattice and arranges.
As shown in Figure 4, the TiO that prepared by the present invention 2the schematic cross-section of nano bowl unit and based on TiO 2the section S EM figure of the organic inorganic hybridization ultraviolet light detector of nano bowl array.Fig. 4 (a) and Fig. 4 (b) are respectively TiO prepared by the present invention 2the schematic cross-section of nano bowl unit and based on TiO 2the section S EM figure of the organic inorganic hybridization ultraviolet light detector of nano bowl array.Can find out TiO from Fig. 4 (a) 2the nano bowl unit is by being highly that the bottom that h, the thickness spine that is d and thickness are D forms, and the internal diameter of nano bowl unit is r; From Fig. 4 (b), can find out, the thickness of ito thin film is about 150nm, TiO 2nano bowl array internal diameter r is about 375nm, and the height h of spine is about 50nm, and thickness d is about 100nm, and the bottom thickness D of bowl is about 50nm, and the thickness of PVK film is about 150nm, WO 3the thickness of/Ag film is about 70nm.
As shown in Figure 5, when wavelength is less than 320nm, the transmitance of ito glass sharply descends; The absorption band of PVK is 310～360nm, and at 330nm and 345nm two places, absworption peak is arranged respectively; And TiO 2the ABSORPTION EDGE of nano bowl array is positioned at 375nm.The interaction of three kinds of film light spectral properties just, make ultraviolet light detector prepared by the present invention have spectrum-selectivity characteristic.
As shown in Figure 6, the present invention prepare based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array has embodied obvious spectrum-selectivity characteristic, under-5V bias voltage, the responsiveness of device (R) peak value appears at the 330nm place, and half-peak breadth (FWHM) is 38.5nm, and ultraviolet-visible injects and is about 60 than (R330nm/R450nm).
As shown in Figure 7, due to TiO 2there is reflection peak in the back side of nano bowl array at the 375nm place, and this can contribute to the long wave cut-off function limit of device spectral response.For TiO 2, there is a little reflection peak in the front of nano bowl array at the 330nm place, the ultraviolet light that this reflection peak can help the PVK recycling to reflect through metal electrode, and the peak value to the device spectral response at the 330nm place contributes.
Embodiment
Embodiment 1:
[1] ito glass is used acetone, isopropyl alcohol, deionized water ultrasonic cleaning successively, then dries;
[2] at room temperature, the mixed solution that the hydrochloric acid that is 0.28mol/L by 30mL ethanol, 10mL deionized water, 2mL concentration is made into dropwise splashes in the solution that contains 10mL butyl titanate, 60mL ethanol, 5mL acetylacetone,2,4-pentanedione, and with vigorous stirring 2 hours, and then make TiO 2colloidal sol;
[3] by TiO 2colloidal sol is spin-coated on ito glass with the rotating speed of 3000rpm, then puts into Muffle furnace, and under 450 ℃ of conditions, sintering is 2 hours, forms Detitanium-ore-type TiO after sintering on ito glass 2nanocrystalline thin film (nc-TiO 2), thickness is 50nm;
[4] at first, the PS bead be take to (volume ratio of water and ethanol is 1:2) in the mixed solution of the water-soluble and ethanol of 5% mass ratio, and with microsyringe, this mixed solution slowly is expelled to the surface of water, it is freely disperseed, until be paved with the whole water surface with individual layer.Then the surface that the lauryl sodium sulfate that is 2% by several mass ratioes (SDS) aqueous solution drips to water reduces the surface tension of water, the individual layer bead is arranged compact.Finally place 24 hours, make the bead sedimentation suspended in water, whole process all completes in enclosed environment;
[5] by the TiO sintered 2film inserts the previous step self assembly with the angle inclination of 30 degree to be had in the aqueous solution of PS bead, and the PS bead single thin film of self assembly on the water surface is slowly picked up, and then, under nitrogen protection, dries one hour, makes PS bead template for 90 ℃.Again will be with the TiO of PS bead template 2film vertically inserts TiO 2in colloidal sol 30 seconds, finally slowly propose and put into Muffle furnace, under 450 ℃ of conditions, sintering is 2 hours, thereby obtains TiO2 nano bowl array;
[6] the PVK chloroformic solution that is 10mg/mL by concentration is spin-coated on TiO2 nano bowl array with the rotating speed of 800rpm, then puts it into vacuum drying oven, dries 30 minutes under 100 ℃, thereby obtains the PVK film that thickness is 150nm;
[7] by substrate-transfer to thermal evaporation system (the organic gas molecule in space depositing system of SD400B type multi-source temperature control), evaporation WO successively 3(10nm)/Ag(60nm) layer, as hole transmission layer and the anode of device, the WO of 10nm 3the evaporation rate of the Ag of layer and 50nm is respectively 0.03nm/s and 0.15nm/s.
The effective area of the battery prepared in above-described embodiment is 6mm 2.Measurement is to carry out under the 500W xenon lamp irradiation of producing in Beijing Chang Tuo Science and Technology Ltd., and use monochromator, continuously change the optical wavelength be radiated on device, the 10nm of take measures as one, at 450nm, in the 250nm scope, the spectral response of device is tested, the ultraviolet light irradiation meter that light intensity is produced with Beijing Normal University is measured.The I-V curve is measured with Keithley2601.All measurements are all carried out under atmospheric environment.
Above said content, be only the specific embodiment of the present invention, can not limit scope of the invention process with it, and the impartial changes and improvements of generally carrying out according to patent claim of the present invention, all should still belong to the scope that patent of the present invention contains.

Claims (8)

1. one kind based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array is characterized in that: from the light incident direction, successively by Conducting Glass, as the triangular crystal lattice that is of electron acceptor, arrange closelypacked TiO 2the nano bowl array, as the PVK film of electron donor, as the WO of hole transmission layer 3film and forming as the metallic film of top electrode.
2. as claimed in claim 1 a kind of based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array is characterized in that: be triangular crystal lattice and arrange closelypacked TiO 2the internal diameter of the bowl shaped structure unit of nano bowl array is 360～390nm, and spine is highly 50～80nm, and spine's thickness is 90～120nm, bottom thickness is 30～60nm, the length of adjacent two bowl shaped structure unit circle center line connectings is 420～440nm, and the thickness of PVK film is 100～150nm, WO 3the thickness of film is 10～15nm, and the thickness of metallic film is 50～60nm.
3. as claimed in claim 1 a kind of based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array is characterized in that: the metal of metallic film is Ag, Al or Au.
4. as claimed in claim 1 a kind of based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array is characterized in that: electro-conductive glass is ito glass.
5. claimed in claim 1 a kind of based on TiO 2the preparation method of the organic inorganic hybridization ultraviolet light detector of nano bowl array, its step is as follows:
1) electro-conductive glass is used acetone, isopropyl alcohol and deionized water ultrasonic cleaning successively, then dries;
2) prepare TiO 2colloidal sol;
3) by TiO 2colloidal sol is spin-coated on electro-conductive glass with the rotating speed of 3000～5000rpm, then puts into Muffle furnace, and under 450～500 ℃ of conditions, sintering is 2 hours, forms Detitanium-ore-type TiO after sintering on electro-conductive glass 2nanocrystalline thin film;
4) be at the aqueous solution surface self-organization PS bead single thin film that triangular crystal lattice is arranged close-packed structure;
5) will form TiO 2the electro-conductive glass of nanocrystalline thin film inserts above-mentioned self assembly with the angle inclination of 30～40 degree to be had in the aqueous solution of PS bead single thin film; the PS bead single thin film of self assembly on the water surface is slowly picked up; then under nitrogen protection, dry 1 hour for 70～90 ℃, thereby at TiO 2pS bead template is made on the nanocrystalline thin film surface; Again will be with the TiO of PS bead template 2nanocrystalline thin film vertically inserts TiO 2in colloidal sol 30 seconds～1 minute, finally slowly propose and put into Muffle furnace, under 450～500 ℃ of conditions, sintering is 2～3 hours, thereby forms TiO on electro-conductive glass 2the nano bowl array;
6) the PVK chloroformic solution that is 10～15mg/mL by concentration is spin-coated on TiO with the rotating speed of 800～1000rpm 2on the nano bowl array, then put it into vacuum drying oven, dry under 90～110 ℃ 15～30 minutes, thereby obtain PVK active layer film;
The electro-conductive glass that 7) will have an active layer film is transferred in thermal evaporation system, evaporation hole transmission layer and metal electrode in turn on the active layer film, thus prepare based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array.
6. as claimed in claim 5 a kind of based on TiO 2the preparation method of the organic inorganic hybridization ultraviolet light detector of nano bowl array is characterized in that: be triangular crystal lattice and arrange closelypacked TiO 2the internal diameter of the bowl shaped structure unit of nano bowl array is 360～390nm, and spine is highly 50～80nm, and spine's thickness is 90～120nm, bottom thickness is 30～60nm, the length of adjacent two bowl shaped structure unit circle center line connectings is 420～440nm, and the thickness of PVK film is 100～150nm, WO 3the thickness of film is 10～15nm, and the thickness of metallic film is 50～60nm.
7. as claimed in claim 5 a kind of based on TiO 2the organic inorganic hybridization ultraviolet light detector preparation method of nano bowl array, it is characterized in that: step 2) be at room temperature, the mixed solution that the hydrochloric acid that is 0.28mol/l by 20～40ml ethanol, 10～20ml deionized water, 2～5ml concentration is made into dropwise splashes in the solution that contains 10～20ml butyl titanate, 50～60ml ethanol, 5～10ml acetylacetone,2,4-pentanedione, and with vigorous stirring 2～4 hours, and then make TiO 2colloidal sol.
8. as claimed in claim 5 a kind of based on TiO 2the organic inorganic hybridization ultraviolet light detector preparation method of nano bowl array, it is characterized in that: in the mixed solution of the PS bead that step 4) is is 450nm by diameter and ethanol water-soluble with 3～5% mass ratio, the volume ratio of water and ethanol is 1:1～3, and with microsyringe, this mixed solution slowly is expelled to the surface of water, it is freely disperseed, until the PS bead is paved with the whole water surface; Then the surface that the lauryl sodium sulfate aqueous solution that is 1～3% by several mass ratioes drips to water reduces the surface tension of water, the individual layer bead is arranged compact; Finally place 24 hours, make the bead sedimentation suspended in water, self assembly forms and is the PS bead single thin film that triangular crystal lattice is arranged close-packed structure, and whole process all completes in enclosed environment.
CN201310384880.2A 2013-08-29 2013-08-29 A kind of based on TiO 2ultraviolet light detector of nano bowl array and preparation method thereof Expired - Fee Related CN103441216B (en)

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CN105304747A (en) * 2015-09-15 2016-02-03 湖北大学 Self-driven photodetector based on ZnO nanorod/CH3NH3PbI3/MoO3 structure and preparation method thereof
CN105529404A (en) * 2015-12-21 2016-04-27 吉林大学 Organic solar cell with two-dimensional nano-bowl array light trapping structure and preparation method of organic solar cell
CN113594370A (en) * 2021-07-16 2021-11-02 华中科技大学 CsPbCl with omnibearing imaging function3Spherical ultraviolet detector and preparation method thereof

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN105304747A (en) * 2015-09-15 2016-02-03 湖北大学 Self-driven photodetector based on ZnO nanorod/CH3NH3PbI3/MoO3 structure and preparation method thereof
CN105529404A (en) * 2015-12-21 2016-04-27 吉林大学 Organic solar cell with two-dimensional nano-bowl array light trapping structure and preparation method of organic solar cell
CN105529404B (en) * 2015-12-21 2018-02-23 吉林大学 A kind of organic solar batteries with two-dimensional nano bowl array light trapping structure and preparation method thereof
CN113594370A (en) * 2021-07-16 2021-11-02 华中科技大学 CsPbCl with omnibearing imaging function3Spherical ultraviolet detector and preparation method thereof

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