CN103545397B - Thin film ultraviolet detector and preparation method thereof and application - Google Patents

Thin film ultraviolet detector and preparation method thereof and application Download PDF

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CN103545397B
CN103545397B CN201310521558.XA CN201310521558A CN103545397B CN 103545397 B CN103545397 B CN 103545397B CN 201310521558 A CN201310521558 A CN 201310521558A CN 103545397 B CN103545397 B CN 103545397B
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thin film
photoconductive detector
zinc oxide
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CN103545397A (en
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靳志文
王吉政
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Institute of Chemistry CAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
    • H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by at least one potential-jump barrier or surface barrier, e.g. phototransistors
    • H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
    • H01L31/102—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier or surface barrier
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264—Inorganic materials
    • H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1828—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a kind of thin film ultraviolet detector and preparation method thereof and application.This thin film photoconductive detector, comprises the electrode layer of substrate and patterning thereon, between the positive pole and negative pole of the electrode layer of described patterning, have light-sensitive layer, and described light-sensitive layer comprises zinc oxide film and nanogold particle layer.This detector combines the low conductive layer of large-area Lacking oxygen layer that the high mobility of zinc oxide and gold nano grain and Zinc Oxide Interface are formed, high mobility result in short electron transit time, the low conductive layer of large-area Lacking oxygen result in the life-span of long photoexciton, when illumination is mapped on device, material extinction produces very fast and a large amount of being collected by electrode of charge carrier and produces very large G value, thus improves detector sensitivity.Ultra-thin active layer material simultaneously used by device to the absorption of visible ray and scattering low especially, its light transmission is also splendid.Therefore, this thin film ultraviolet detector has important using value.

Description

Thin film ultraviolet detector and preparation method thereof and application
Technical field
The present invention relates to a kind of thin film ultraviolet detector and preparation method thereof and application.
Background technology
At present, known ultraviolet light detector structure is made up of the light-sensitive layer of two horizontal electrodes and centre.Photoconductive device is connected into loop and adds a bias field, when incident light contacts with detector, the light-sensitive layer of detector inside produces electron hole pair, electron hole pair is separated and is collected by electrode and forms photoelectric current under the effect of electric field, characterized intensity and the size of light by the intensity of photoelectric current, can be used for carrying out the directions such as light detection, image imaging or bio-sensing.Therefore device is quite important to the susceptibility of light, and we characterize such Species sensitivity by two important parameters usually: responsiveness R and optical gain G.R represents a ratio of the photoelectric current of generation and the luminous intensity of introducing, and what G represented is that device often absorbs the inner electric charge flow through of a photonic device.
These two values can represent with formula below:
G represents optical gain:
G = ( μ n + μ p ) τE L = τ ( 1 t n + 1 t p ) - - - ( 1 )
R represents responsiveness (AW -1):
R = EQE λq hc G = I Light - I Dark P ill - - - ( 2 )
The parameter of other three no less importants can represent with formula below:
P represents signal to noise ratio:
P = I Light - I Dark I Dark - - - ( 3 )
D* represents sensitivity (in units of jones):
D * = R S 2 qI dark - - - ( 4 )
LDR represents linear dynamic range (in units of dB):
LDR = 20 log ( J Light J Dark ) - - - ( 5 )
(EQE is outer quantum effect, and λ is lambda1-wavelength, and h is Planck's constant, and c is the light velocity, and q is the quantity of electric charge, and L is device channel length (two interelectrode distance), and E is additional electric field strength, μ nelectron mobility, μ pbe hole mobility, τ is the life-span of photoexciton, t nelectron transit time, t pthe hole transit time, P illincident optical power, I lightphotoelectric current, I darkbe dark current, S is exposure area, J light1mW/cm 2time density of photocurrent, J darkdark current density).
Thin film ultraviolet detector can be applied in civilian and national defence, such as can be attached on glass, on display screen or on other photoelectric devices.For desirable thin film ultraviolet detector, basic requires: the G that (1) is large, R, D* and LDR value; (2) good linear relationship can be presented with incident light; (3) high incident light transmitance; (4) simple structure; (5) preparation technology of low price; (6) low-temperature operation.The forbidden band of wide bandgap semiconductor can only absorb ultraviolet light and through visible ray.Wherein the energy gap of zinc oxide is 3.2eV, and it is again a kind of environmental friendliness shaped material simultaneously.And be used for zinc oxide realizing ultraviolet light detector and also there are following two important reasons: (1), by simply various method to realize high mobility, in various different substrate, high mobility can reduce electron transit time; (2) oxygen can be adsorbed on zinc oxide surface and cause very large Lacking oxygen, and form the low conductive layer of one deck, the existence of this one deck can cause photogenerated charge to be difficult to compound, increases the life-span of photoexciton.These two reasons all can cause large G value, thus improve the performance of device.
The past period, the research about this respect is directed to the mobility how improving material, the nearly 1.5AW of R of acquisition -1.Its sensitivity is nowhere near, because zinc oxide surface is long-pending too little.At present, the thin-film device that nanostructure is composited mainly is paid close attention in most research, because such nanostructure has very large specific area, thus creates large Lacking oxygen conductive formation.The R value of the thin-film device such as utilizing Zinc oxide nanoparticle to make is up to 61AW -1, the R value of the device utilizing Electrospun zinc oxide nanowire to make is up to 790AW -1.But various nanostructure causes carrier transport distance longer between two electrodes and reduces mobility.Simultaneously this nanostructure create large light scattering and have impact on visible ray through.Therefore, the transparent zinc oxide thin film ultraviolet detector utilizing simple method to prepare high R and G value is at present a large challenge.
Summary of the invention
The present invention, in order to overcome the shortcoming of the low and printing opacity rate variance of existing thin film photoconductive detector performance, provides that a kind of structure is simple, preparation method is easy, have the Uv Photoconductivity Properties detector of very high optical gain and responsiveness.
Another object of the present invention is to provide the preparation method of above-mentioned thin film ultraviolet detector.
Another object of the present invention is to provide the purposes of above-mentioned thin film ultraviolet detector.
The present invention is achieved through the following technical solutions:
A kind of thin film photoconductive detector, it is characterized in that, described detector comprises the electrode layer of substrate and patterning thereon, between the positive pole and negative pole of the electrode layer of described patterning, have light-sensitive layer, and described light-sensitive layer comprises zinc oxide film and nanogold particle layer.
According to the present invention, described zinc oxide film is positioned on substrate, and described nanogold particle layer is positioned on described zinc oxide film.
According to the present invention, the thickness of described zinc oxide film is 3-30nm, preferred 4-20nm, such as 5nm.
According to the present invention, described gold nano grain is distributed on zinc-oxide film, preferably dispersed, and the diameter of described gold nano grain is preferably 2-50nm domain size distribution, is more preferably the domain size distribution of 2-4nm.
According to the present invention, described substrate can be rigid basement or flexible substrates, and described rigid basement is such as glass or silicon, and described flexible substrates can be at least one be selected from polyimides and polyester film.
According to the present invention, the relative molecular weight of described polyimides is preferably 10000-100000g/mol, more preferably 20000-60000g/mol, such as 45000g/mol; The relative molecular weight of described polyester is preferably 10000-100000g/mol, more preferably 20000-80000g/mol, such as 70000g/mol.
According to the present invention, material preferred autoxidation indium tin (ITO) of described electrode layer, mixes at least one in the tin oxide (FTO) of fluorine or aluminium electrode, is preferably ITO electrode.The electrode layer of described patterning is made up of the anode layer and negative electrode layer being positioned at same layer, and the level interval of described anode layer and negative electrode layer is 10-1000 μm, is preferably 30-500 μm, is more preferably 50 μm.The thickness of electrode layer is 30-200nm, is preferably 50-150nm, is more preferably 50nm.
According to the present invention, described thin film photoconductive detector is transparent thin film photoconductive detector.
According to the present invention, described thin film photoconductive detector is made up of following layer: the electrode layer of substrate, patterning and light-sensitive layer.Electrode layer and the light-sensitive layer of described patterning are all deposited in substrate, and described light-sensitive layer is between the positive pole and negative pole of the electrode layer of described patterning.Described light-sensitive layer comprises zinc oxide film and nanogold particle layer.Described zinc oxide film is deposited in substrate, and described nanogold particle is deposited upon on described zinc oxide film.Present invention also offers a kind of method preparing described thin film photoconductive detector, comprise the steps:
1) in the described substrate with the electrode of patterning, zinc oxide film is prepared;
2) on described zinc oxide film, prepare gold nano grain layer, obtain described detector.
According to the present invention, in the above-mentioned methods, the method preparing described zinc oxide film and gold nano grain layer is solution spin-coating method.
According to the present invention, in described spin-coating method, the concentration of the burnett's solution used is 1-10mg/ml, such as 6mg/ml; The speed of spin coating is 500-10000rpm, such as 3000rpm; The concentration of the gold nano grain solution used is 0.1-1mg/ml, such as 0.5mg/ml; The speed of spin coating is 500-10000rpm, such as 6000rpm.
According to the present invention, before the step 1) of above-mentioned preparation method, also first the substrate of the electrode with patterning can be done following preliminary treatment: by described substrate priority deionized water, acetone and isopropyl alcohol cleaning, then dry.
According to the present invention, the method preparing electrode layer is conventional method, such as, in optional vacuum vapour deposition and sputtering method any one;
In described sputtering method, the vacuum degree of sputtering is 10 -4-10 -5pa, is preferably 1 × 10 -4pa.
In described vacuum vapour deposition, the vacuum degree of electrode evaporation layer is 10 -4-10 -5pa, is preferably 1 × 10 -4pa.
Present invention also offers the purposes of described detector, it can be used for preparing photodetector, image image device or biology sensor,
Present invention also offers a kind of photodetector, it comprises detector of the present invention.
Present invention also offers a kind of image image device, it comprises detector of the present invention.
Present invention also offers a kind of biology sensor, it comprises detector of the present invention.
Uv Photoconductivity Properties detector of the present invention, structure is simple, and preparation method is easy, and has very high optical gain and responsiveness.This detector combines the low conductive layer of large-area Lacking oxygen that the high mobility of zinc oxide and gold nano grain and Zinc Oxide Interface are formed, high mobility result in short electron transit time, the low conductive layer of large-area Lacking oxygen result in the life-span of long photoexciton, so when illumination is mapped on device, material extinction produces very fast and a large amount of being collected by electrode thus have very large G and R value of charge carrier.Therefore this photoconductive detector has very large optical gain, thus improves the responsiveness of photoconductive detector to light, and then improves the sensitivity of thin film photoconductive device.Therefore detector of the present invention has important using value.
Accompanying drawing explanation
Fig. 1 a is the structural representation of the thin film ultraviolet detector part of embodiment 1.
Fig. 1 b is the cross-sectional scans Electronic Speculum figure of the thin film ultraviolet detector part of embodiment 1.
Fig. 2 a is the SEM image of zinc-oxide film.
Fig. 2 b is the XPS Analysis figure of zinc-oxide film.
Fig. 2 c is the transmission electron microscope picture of gold nano grain.
Fig. 2 d is the XRD figure of gold nano grain.
Fig. 3 a is the transfer curve figure of gold nano grain and zinc oxide composite membrane.
Fig. 3 b is the photoresponse of device and the relation of wavelength.
Fig. 3 c is device at the I-V curve chart of light and dark place.
Fig. 3 d is that gold nano grain and electrode channel length are on the impact of the photoresponse situation of device.
Fig. 4 a is the repeatability of device to the switching characteristic of light.
Fig. 4 b is the result of calculation of G and R of device.
Fig. 4 c is the result of calculation of the D* of device.
Fig. 4 d is that the photogenerated current of device is linear with light intensity.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.Described method is conventional method if no special instructions.Described raw material all can obtain from open commercial sources if no special instructions.
ZnOxH 2o, 97% purchased from Sigma-Aldrich company, and production code member is 475319;
Ammonium hydroxide is purchased from Sigma-Aldrich company, and production code member is 320145;
Embodiment 1
1) by ZnOxH 2o is dissolved in ammonium hydroxide the solution obtaining 6mg/ml concentration, 3000rpm spin coating 60s thickness be 3mm with in the substrate of glass 5 of ITO electrode 3 and the 180 DEG C of 1h that anneal, obtain the carrier blocking layers 4 that thickness is 5nm in triplicate.
Forming the material absorbing ultraviolet light and carrier blocking layers is zinc oxide, and 1 represents incident light;
2) gold nano grain adopts two phase process synthesis.By the HAuCl of 0.63g 4xH 2o is soluble in water, and is dissolved in 160ml paraxylene by 3g tetra-octyl group ammonium bromide.Mixed for two solution and stir standing.Collect organic phase continuation stirring and add 0.8ml mercaptan.By 0.76gNaBH 4be dissolved in 50ml water also slowly adding in above-mentioned organic phase in ice-water bath, continue stirring 2 hours.The gold nano grain domain size distribution finally obtained is at 2 – 4nm.
3) on the zinc-oxide film of step 1) gained, the very thin gold nano grain layer 2 of one deck is prepared in spin coating.Concrete steps comprise: gold nano grain is dissolved in carrene the solution obtaining 0.5mg/ml concentration, 6000rpm spin coating 60s the 180 DEG C of 24h of annealing obtain gold nano grain layers 2.
Be the structural representation of this transparent membrane ultraviolet detector device as shown in Figure 1a.
Be the cross-sectional scans Electronic Speculum figure of this transparent membrane ultraviolet detector device as shown in Figure 1 b.
During test, the electrode 3 of this detector is connected with external circuit.Testing light source used is tungsten halogen lamp white light source, and intensity can change, and the light intensity of monochromatic source used is 10.6 μ W/cm 2.All light intensity are calibrated by irradiatometer before testing.The substrate that the test of mobility is used is Si/SiO 2, wherein Si is N-shaped heavy doping, SiO 2thick 300nm, electric capacity is 10nF.
As the SEM image that Fig. 2 a is zinc-oxide film.
As the XPS Analysis figure that Fig. 2 b is zinc-oxide film.
From Fig. 2 a and 2b, the zinc-oxide film obtained is little druse composition, can produce very large surface area, learn that the composition material of film is zinc oxide by XPS Analysis.
If Fig. 2 c is the transmission electron microscope picture of gold nano grain.
As the XRD figure that Fig. 2 d is gold nano grain.
From Fig. 2 c and 2d, gold nano grain domain size distribution is at 2 – 4nm.
Fig. 3 a is the transfer curve figure of gold nano grain and zinc oxide composite membrane.Give the electron mobility 1.78cm that it is high 2.V -1.s -1.
If Fig. 3 b is the photoresponse of device and the relation of wavelength.
As the I-V curve chart that Fig. 3 c is device in light and dark place.
Be that gold nano grain and electrode channel length are on the impact of the photoresponse situation of device as shown in Figure 3 d.
As shown in Figure 3, the detector made with gold nano grain and zinc oxide composite membrane has good photoresponse and the selectivity to optical wavelength.The large-area Lacking oxygen layer that gold nano grain and Zinc Oxide Interface can be formed can increase the life-span of photoexciton.Simultaneously along with shortening channel length can reduce the transit time of electronics.These two aspects can improve the performance of described device greatly.
If Fig. 4 a is the repeatability of device to the switching characteristic of light.
If Fig. 4 b is the optical gain (G) of device and the result of calculation of responsiveness (R).
Be the result of calculation of the sensitivity (D*) of device as Fig. 4 c.
If Fig. 4 d is that the photogenerated current of device is linear with light intensity.
As shown in Figure 4, the ultraviolet light detector made from gold nano grain and zinc oxide composite membrane has excellent performance, and photogenerated current is linear with light intensity, and calculating gained LDR is 60dB, can meet application completely.

Claims (21)

1. a thin film photoconductive detector, it comprises the electrode layer of substrate and patterning thereon, between the positive pole and negative pole of the electrode layer of described patterning, there is light-sensitive layer, described light-sensitive layer comprises zinc oxide film and gold nano grain layer, and described zinc oxide film is positioned on substrate, described gold nano grain layer is positioned on described zinc oxide film.
2. thin film photoconductive detector according to claim 1, the thickness of described zinc oxide film is 3-30nm.
3. thin film photoconductive detector according to claim 2, the thickness of described zinc oxide film is 4-20nm.
4. thin film photoconductive detector according to claim 2, the thickness of described zinc oxide film is 5nm.
5. thin film photoconductive detector according to claim 1, described gold nano grain is distributed on zinc-oxide film, and the diameter of described gold nano grain is 2-50nm domain size distribution.
6. thin film photoconductive detector according to claim 5, wherein, the diameter of described gold nano grain is the domain size distribution of 2-4nm.
7. the thin film photoconductive detector according to any one of claim 1-6, the material of described electrode layer is selected from tin indium oxide (ITO), mixes at least one in the tin oxide (FTO) of fluorine or aluminium electrode.
8. the thin film photoconductive detector according to any one of claim 1-6, wherein, the level interval between the positive pole of the electrode layer of described patterning and negative pole is 10-1000 μm.
9. thin film photoconductive detector according to claim 8, wherein, the level interval between the positive pole of the electrode layer of described patterning and negative pole is 30-500 μm.
10. thin film photoconductive detector according to claim 8, wherein, the level interval between the positive pole of the electrode layer of described patterning and negative pole is 50 μm.
11. thin film photoconductive detector according to any one of claim 1-6, the thickness of described electrode layer is 30-200nm.
12. thin film photoconductive detector according to claim 11, the thickness of described electrode layer is 50-150nm.
13. thin film photoconductive detector according to claim 12, the thickness of described electrode layer is 50nm.
14. thin film photoconductive detector according to any one of claim 1-6, described substrate is rigid basement or flexible substrates, and described rigid basement is glass or silicon, and described flexible substrates is selected from least one in polyimides and polyester film.
15. thin film photoconductive detector according to claim 14, the relative molecular mass of wherein said polyimides is 10000-100000g/mol; The relative molecular mass of described polyester is 10000-100000g/mol.
16. thin film photoconductive detector according to claim 15, the relative molecular mass of described polyimides is 45000g/mol; The relative molecular mass of described polyester is 70000g/mol.
17. 1 kinds of methods preparing the thin film photoconductive detector described in any one of claim 1-16, comprise the steps:
1) in the described substrate with the electrode of patterning, zinc oxide film is prepared;
2) on described zinc oxide film, prepare gold nano grain layer, obtain described detector;
Wherein, the method preparing described zinc oxide film and gold nano grain layer is solution spin-coating method.
The purposes of the thin film photoconductive detector described in 18. any one of claim 1-16, it is for the preparation of photodetector, image image device or biology sensor.
19. 1 kinds of photodetectors, it comprises the thin film photoconductive detector described in any one of claim 1-16.
20. 1 kinds of image image devices, it comprises the thin film photoconductive detector described in any one of claim 1-16.
21. 1 kinds of biology sensors, it comprises the thin film photoconductive detector described in any one of claim 1-16.
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