CN103441216B - A kind of based on TiO 2ultraviolet light detector of nano bowl array and preparation method thereof - Google Patents

A kind of based on TiO 2ultraviolet light detector of nano bowl array and preparation method thereof Download PDF

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CN103441216B
CN103441216B CN201310384880.2A CN201310384880A CN103441216B CN 103441216 B CN103441216 B CN 103441216B CN 201310384880 A CN201310384880 A CN 201310384880A CN 103441216 B CN103441216 B CN 103441216B
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tio
film
nano bowl
light detector
ultraviolet light
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CN103441216A (en
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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

A kind of based on TiO 2ultraviolet light detector of nano bowl array and preparation method thereof, belongs to organic electro-optic device technical field.First employing sol-gal process and PS ball template method grow the TiO as electron acceptor on electro-conductive glass 2nano bowl array, then adopt solution spin coating method at TiO 2pVK film as electron donor prepared by nano bowl array, then employing vacuum vapour deposition prepares the WO as hole transmission layer on active layer 3film, finally adopts vacuum vapour deposition at WO 3metallic film as top electrode prepared by film.It is simple that organic inorganic hybridization ultraviolet light detector prepared by the present invention has preparation method, with low cost, can the feature of large area film forming, and have obvious spectrum-selectivity characteristic.

Description

A kind of based on TiO 2ultraviolet light detector of nano bowl array and preparation method thereof
Technical field
The invention belongs to 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 the organic inorganic hybridization ultraviolet light detector and preparation method thereof of electron acceptor.
Background technology
Ultraviolet detector all has a wide range of applications in national defense and military, ultraviolet astronomy, combustion enginnering, Missile Plume detection, UV warming, biological cell canceration detection and the monitoring of turbine engine combustion efficiency etc., has become one of emphasis problem of many advanced countries research and development in the world.And wide bandgap semiconductor base ultraviolet light detector is due to advantages such as volume are little, efficiency is high, cost is low, low in energy consumption, obtains in photodetection field and pay attention to widely and development at full speed.
Semi-conducting material at present for ultraviolet light detector has a lot, mainly concentrates in the semiconductor material with wide forbidden band such as carborundum (SiC), gallium nitride (GaN) and zinc oxide (ZnO).But it should be noted that, major part is wider based on the spectral response range of the ultraviolet light detector of semiconductor material with wide forbidden band, cannot 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 metalloid organic chemistry vapor phase deposition (MOCVD) or the so complicated technique of molecular beam epitaxy (MBE) usually, causes device production cost higher.
Because the absorption spectrum of organic material can regulate effectively by controlling molecular structure, organic/inorganic semiconductor hybrid is by organic together with the advantages of inorganic semiconductor material, and the ultraviolet light detector for realization with spectral selection provides research means that is relatively easy and low cost.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 the inorganic N-type semiconductor material with wide forbidden band of one, 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, the ultraviolet light detector with spectrum-selectivity characteristic can be developed.
In addition, carry out hydridization by the inorganic semiconductor material and organic material introducing low-dimensional, organic/inorganic contact interface can be increased, directed carrier transport path is provided, improve separation and the transmission of photogenerated charge, improve the performance of hydridization device.And the special optical character that the periodic structure of himself high-sequential has (reflex as special wavelength) also can produce positive role for the spectrum-selectivity characteristic of ultraviolet light detector.Therefore, the TiO by 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 organic inorganic hybridization ultraviolet light detector of nano bowl array as electron acceptor and the preparation method of this ultraviolet light detector.
The present invention adopts PVK as electron donor material, TiO 2bi-material, as electron acceptor material, is made the double layer heterojunction of hybrid as active layer by nano bowl array, makes ultraviolet light detector.By tin indium oxide (ITO), PVK, TiO 2the interaction of each layer film optical characteristics of nano bowl array, realizes the spectrum-selectivity characteristic of ultraviolet light detector.
Ultraviolet light detector of the present invention, is characterized in that: be followed successively by ito glass substrate from light incident direction, arrange closelypacked TiO as electron acceptor in triangular crystal lattice 2nano bowl array (PS bead template and sol-gal process preparation), PVK film (preparation of solution spin-coating method), tungstic acid (WO as hole transmission layer 3) film (vacuum vapour deposition preparation), metallic film (metal can be silver-colored Ag, aluminium Al, golden Au etc., vacuum vapour deposition prepare) as top electrode.
Further, closelypacked TiO is arranged in triangular crystal lattice 2nano 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 (i.e. the lattice constant of triangular crystal lattice) of adjacent two bowl shaped structure unit circle center line connectings is the thickness of 420 ~ 440nm, 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 uses acetone, isopropyl alcohol, deionized water ultrasonic cleaning successively, then dries;
[2] at room temperature, be that the mixed solution that the hydrochloric acid of 0.28mol/L is made into dropwise instills in the solution containing 10 ~ 20mL butyl titanate, 50 ~ 60mL ethanol, 5 ~ 10mL acetylacetone,2,4-pentanedione by 20 ~ 40mL ethanol, 10 ~ 20mL deionized water, 2 ~ 5mL concentration, and with vigorous stirring 2 ~ 4 hours, and then obtained 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, sinters 2 ~ 4 hours, form Detitanium-ore-type TiO after sintering on ito glass under 450 ~ 500 DEG C of conditions 2nanocrystalline thin film (nc-TiO 2), thickness is 30 ~ 60nm; Wherein, when sintering temperature is lower than 450 DEG C, TiO 2colloidal sol can not be transformed into TiO fully 2nanocrystal, during higher than 500 DEG C, TiO 2the crystal formation of nanocrystal starts to change from Detitanium-ore-type to rutile-type.TiO 2the spin coating revolution of colloidal sol is higher, and obtained film thickness is thinner.Experimental result shows, when spin coating revolution is between 3000 ~ 5000rpm, obtained device performance change is little.
[4] by diameter be the water-soluble and ethanol of PS bead (obtaining by the buying) mass ratio with 3 ~ 5% of 450nm mixed solution in (volume ratio of water and ethanol is 1:1 ~ 3), and with microsyringe, this mixed solution is slowly expelled to the surface of water, it is made freely to disperse, until PS bead is paved with the whole water surface with individual layer; Then by several mass ratioes be 1 ~ 3% lauryl sodium sulfate (SDS) aqueous solution drip to the surface of water to reduce the surface tension of water, make the self assembly of individual layer bead formed in triangular crystal lattice arrangement close-packed structure; Finally place 24 hours, make the bead sedimentation suspended in water, whole process all completes in enclosed environment;
[5] TiO will sintered 2film inserts previous step self assembly with the angular slope of 30 ~ 40 degree to be had in the aqueous solution of PS bead, is slowly picked up by the PS bead single thin film of self assembly on the water surface, then under nitrogen protection, dries one hour, makes PS bead template for 70 ~ 90 DEG C.Again by the TiO with PS bead template 2film normal 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 DEG C of conditions, sintering 2 ~ 3 hours, 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 TiO below 2crystal film is combined, thus forms TiO 2nano bowl array;
[6] be that the PVK chloroformic solution of 10 ~ 15mg/mL is spin-coated on TiO with the rotating speed of 800 ~ 1000rpm by concentration 2on nano bowl array, then put it into vacuum drying oven, dry 15 ~ 30 minutes at 90 ~ 110 DEG C, thus obtain the PVK active layer film that thickness is 100 ~ 150nm;
[7] ito glass with active layer film is transferred in thermal evaporation system (SD400B type multi-source temperature control organic vapors molecule deposition system), evaporation hole transmission layer and metal electrode in turn on active layer film; Vapor deposition source is respectively WO 3powder, Ag, Al or Au powder, all obtain by buying, thus prepare of the present invention based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array.
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 2xRD figure and the SEM figure of nano bowl array;
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 organic inorganic hybridization ultraviolet light detector under-5V bias voltage of nano bowl array;
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 2nano bowl array 2, PVK film 3, WO 3hole transmission layer 4, metal electrode 5 forms.Wherein transparent cathode 1 is used for conduction electron; TiO 2nano bowl array 2 is used for absorb photons thus produce electron hole pair conduction electron; PVK film 3 is used for absorb photons thus produce exciton conduction hole; Hole transmission layer 4 be used for block electrons, collect hole, metal electrode 5 conduction hole.
As shown in Figure 2, under non-illuminated conditions, the current density of device under-5V bias voltage is 7.97 μ A/cm 2; And be 144 μ W/cm in intensity 2wavelength be under the UV-irradiation of 330nm, the current density of device under-5V bias voltage is 1.17mA/cm 2.Calculating the light dark current ratio of device under-5V bias voltage is thus 147.
As shown in Figure 3, the TiO for preparing of the present invention 2xRD figure and the SEM figure of nano bowl array.Fig. 3 (a) and Fig. 3 (b) is respectively TiO prepared by the present invention 2xRD figure and the SEM figure of nano bowl array.As can be seen from Fig. 3 (a), the crystal formation of sample is Detitanium-ore-type; As can be seen from Fig. 3 (b), TiO 2nano bowl diameter is about 375nm, arranges in triangular crystal lattice.
As shown in Figure 4, the TiO for preparing of 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) is 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.As can be seen from Fig. 4 (a), TiO 2nano bowl unit by be highly h, the bottom of thickness to be the spine of d and thickness be D forms, the internal diameter of nano bowl unit is r; As can be seen from Fig. 4 (b), the thickness of ito thin film is about 150nm, TiO 2nano bowl array internal diameter r is about 375nm, and spine height h 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 declines; The absorption band of PVK is 310 ~ 360nm, and has absworption peak at 330nm and 345nm two place 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, ultraviolet light detector prepared by the present invention is provided with 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, responsiveness (R) peak value of device appears at 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 at 375nm place in the back side of nano bowl array, this can contribute to the long wave cut-off function limit of device spectral response.For TiO 2the front of nano bowl array, at the reflection peak that 330nm place existence one is little, this reflection peak can help PVK to reuse the ultraviolet light reflected through metal electrode, contributes at the peak value at 330nm place to device spectral response.
Embodiment
Embodiment 1:
[1] ito glass uses acetone, isopropyl alcohol, deionized water ultrasonic cleaning successively, then dries;
[2] at room temperature, be that the mixed solution that the hydrochloric acid of 0.28mol/L is made into dropwise instills in the solution containing 10mL butyl titanate, 60mL ethanol, 5mL acetylacetone,2,4-pentanedione by 30mL ethanol, 10mL deionized water, 2mL concentration, and with vigorous stirring 2 hours, and then obtained 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, sinters 2 hours, form Detitanium-ore-type TiO after sintering on ito glass under 450 DEG C of conditions 2nanocrystalline thin film (nc-TiO 2), thickness is 50nm;
[4] first, by PS bead with 5% the water-soluble and ethanol of mass ratio mixed solution in (volume ratio of water and ethanol is for 1:2), and with microsyringe, this mixed solution is slowly expelled to the surface of water, make it freely disperse, until be paved with the whole water surface with individual layer.Then by several mass ratioes be 2% lauryl sodium sulfate (SDS) aqueous solution drip to the surface of water to reduce the surface tension of water, make individual layer bead arrange compact.Finally place 24 hours, make the bead sedimentation suspended in water, whole process all completes in enclosed environment;
[5] TiO will sintered 2film inserts previous step self assembly with the angular slope of 30 degree to be had in the aqueous solution of PS bead, is slowly picked up by the PS bead single thin film of self assembly on the water surface, then under nitrogen protection, dries one hour, makes PS bead template for 90 DEG C.Again by the TiO with PS bead template 2film normal inserts TiO 2in colloidal sol 30 seconds, finally slowly propose and put into Muffle furnace, under 450 DEG C of conditions, sintering 2 hours, thus obtain TiO2 nano bowl array;
[6] be that the PVK chloroformic solution of 10mg/mL is spin-coated on TiO2 nano bowl array with the rotating speed of 800rpm by concentration, then put it into vacuum drying oven, dry 30 minutes at 100 DEG C, thus obtain the PVK film that thickness is 150nm;
[7] by substrate-transfer to thermal evaporation system (SD400B type multi-source temperature control organic vapors molecule deposition system), 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 carries out under the 500W xenon lamp produced in Beijing Chang Tuo Science and Technology Ltd. irradiates, and use monochromator, continuously change the optical wavelength be radiated on device, be one with 10nm to measure, test the spectral response of device in 450nm to 250nm scope, the intensity of light is measured with the ultraviolet light irradiation meter that Beijing Normal University produces.I-V curve Keithley2601 measures.All measurements are all carried out under atmospheric environment.
Above said content, is only the specific embodiment of the present invention, can not limit scope of the invention process with it, generally according to the impartial changes and improvements that patent claim of the present invention is carried out, still all should belong to the scope that patent of the present invention contains.

Claims (7)

1. one kind based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array, is characterized in that: from light incident direction, successively by Conducting Glass, arrange closelypacked TiO as electron acceptor in triangular crystal lattice 2nano bowl array, as the PVK film of electron donor, the WO as hole transmission layer 3film and forming as the metallic film of top electrode; Closelypacked TiO is arranged in triangular crystal lattice 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 the thickness of 420 ~ 440nm, PVK film is 100 ~ 150nm, WO 3the thickness of film is 10 ~ 15nm, and the thickness of metallic film is 50 ~ 60nm.
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: the metal of metallic film is Ag, Al or Au.
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: electro-conductive glass is ito glass.
4. one according to claim 1 is 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 uses acetone, isopropyl alcohol and deionized water ultrasonic cleaning successively, then dries;
2) TiO is prepared 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, sinters 2 hours, form Detitanium-ore-type TiO after sintering on electro-conductive glass under 450 ~ 500 DEG C of conditions 2nanocrystalline thin film;
4) aqueous solution surface self-organization be triangular crystal lattice arrangement close-packed structure PS bead single thin film;
5) TiO will be formed 2the electro-conductive glass of nanocrystalline thin film inserts above-mentioned self assembly with the angular slope 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 DEG C, thus at TiO 2pS bead template is made on nanocrystalline thin film surface; Again by the TiO with 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 DEG C of conditions, sintering 2 ~ 3 hours, thus form TiO on electro-conductive glass 2nano bowl array;
6) be that the PVK chloroformic solution of 10 ~ 15mg/mL is spin-coated on TiO with the rotating speed of 800 ~ 1000rpm by concentration 2on nano bowl array, then put it into vacuum drying oven, dry 15 ~ 30 minutes at 90 ~ 110 DEG C, thus obtain PVK active layer film;
7) electro-conductive glass with active layer film is transferred in thermal evaporation system, evaporation hole transmission layer and metal electrode in turn on active layer film, thus prepares based on TiO 2the organic inorganic hybridization ultraviolet light detector of nano bowl array.
5. as claimed in claim 4 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: arrange closelypacked TiO in triangular crystal lattice 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 the thickness of 420 ~ 440nm, PVK film is 100 ~ 150nm, WO 3the thickness of film is 10 ~ 15nm, and the thickness of metallic film is 50 ~ 60nm.
6. as claimed in claim 4 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, be that the mixed solution that the hydrochloric acid of 0.28mol/l is made into dropwise instills in the solution containing 10 ~ 20ml butyl titanate, 50 ~ 60ml ethanol, 5 ~ 10ml acetylacetone,2,4-pentanedione by 20 ~ 40ml ethanol, 10 ~ 20ml deionized water, 2 ~ 5ml concentration, and with vigorous stirring 2 ~ 4 hours, and then obtained TiO 2colloidal sol.
7. as claimed in claim 4 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 4) be by diameter be 450nm PS bead with 3 ~ 5% the water-soluble and ethanol of mass ratio mixed solution in, the volume ratio of water and ethanol is 1:1 ~ 3, and with microsyringe, this mixed solution is slowly expelled to the surface of water, it is made freely to disperse, until PS bead is paved with the whole water surface; Then by several mass ratioes be 1 ~ 3% lauryl sodium sulfate aqueous solution drip to the surface of water to reduce the surface tension of water, make individual layer bead arrange compact; Finally place 24 hours, make the bead sedimentation suspended in water, self assembly forms the PS bead single thin film of the arrangement close-packed structure in triangular crystal lattice, and whole process all completes in enclosed environment.
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