CN106252455B - It is a kind of to drive Se/ZnO heterojunction ultraviolet photodetectors and preparation method thereof certainly - Google Patents
It is a kind of to drive Se/ZnO heterojunction ultraviolet photodetectors and preparation method thereof certainly Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000004528 spin coating Methods 0.000 claims abstract description 9
- 239000011669 selenium Substances 0.000 claims description 42
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 18
- 239000010453 quartz Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 13
- 229910052711 selenium Inorganic materials 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 150000003751 zinc Chemical class 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000012736 aqueous medium Substances 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000006193 liquid solution Substances 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- -1 zinc salt compound Chemical class 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 14
- 238000000137 annealing Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract 1
- 239000002120 nanofilm Substances 0.000 abstract 1
- 238000002207 thermal evaporation Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 79
- 239000011787 zinc oxide Substances 0.000 description 39
- 239000004065 semiconductor Substances 0.000 description 7
- 238000005286 illumination Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 235000013904 zinc acetate Nutrition 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
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- 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 potential barriers, e.g. phototransistors
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- H01L31/102—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier
- H01L31/109—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier the potential barrier being of the PN heterojunction type
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Abstract
It is specially a kind of from driving Se/ZnO heterojunction ultraviolet photodetectors and preparation method thereof the invention belongs to photoelectric device technical field.The method that the present invention uses spin coating high annealing, is prepared the thickness of large area between 50 200nm, the good ZnO nano particle film of crystallinity；Then the method for using thermal evaporation transfer deposits Se films of a layer thickness at 12 μm in ZnO nano film；Then Se/ZnO heterojunction bilayers films will be obtained and be built into photodetector.Se/ZnO heterojunction photoelectric detectors have work under zero-bias from drive characteristic, the response time of good ultraviolet selective and Millisecond.The device solves traditional disadvantage slow based on ZnO UV photodetector response speeds, and preparation process is simple, can be applied in ultraviolet light detection and its related field.
Description
Technical field
The invention belongs to photoelectric device technical fields, and in particular to a kind of from driving Se/ZnO heterojunction ultraviolet photodetections
The preparation method of device.
Background technology
UV photodetector is a kind of important optoelectronic sensor and in optical communication, fire alarm, bioid credit
It is widely used in the numerous areas such as analysis and aerospace.Zinc oxide（ZnO）It is that one kind being widely used in ultraviolet detector
N-shaped semiconductor material with wide forbidden band.In recent years, a variety of to be based on nano structure of zinc oxide（Nano wire（Y. Zheng, L.
Cheng, M. Yuan, Z. Wang, Nanoscale, 2014, 6, 7842.）, nanobelt（Y. Yang, W. Guo,
J. Qi, Appl. Phys. Lett., 2010, 97, 223113.）, nano particle etc.（Y. Jin, J. Wang, B.
Sun , Nano Lett., 2008, 8, 1649.））UV photodetector have received widespread attention and study.So
And based on the UV photodetector of nano structure of zinc oxide due to the process of the oxygen adsorption and desorption before and after illumination, device
Response speed it is usually relatively slow, the response time needs the several seconds（Z. Jin, Q. Zhou, Y. Chen, Y. Li,Adv. Mater., 2016, 28, 3697.）.In addition to this, the metal-semiconductor-metal based on nano zinc oxide material (MSM) is tied
The semiconductor photo detector of structure usually requires additional bias and carrys out driving element work, this causes device dark current higher and work(
It consumes larger.
In order to improve response speed, power consumption and the brightness electric current ratio based on the ultraviolet broadcasting and TV detectors of ZnO, semiconductor is built
Photovoltaic detector is a kind of ideal selection.Photovoltaic type semiconductor photo detector is a kind of important optoelectronic sensor,
Its outstanding advantages is not need external power supply, directly generates nonequilibrium carrier by light radiation, is detected by photogenerated current
Luminous intensity.Photovoltaic detector based on semiconductor p-n heterojunction can effectively reduce the dark current of device, improve brightness electricity
Stream ratio.Meanwhile rational p-type material being selected to can effectively improve the response speed based on ZnO nano-structure UV photodetector
Degree.Selenium（Se）As a kind of intrinsic p-type semiconductor material, there are many excellent physical properties, such as：Low melting point, high electricity
Conductance, high intrinsic carrier concentration etc..Most of all, the photodetector based on selenium material has response speed quickly.
Existing report shows that the response time of selenium nano-belt optical detector is only about 2 ms.（L.B. Luo, X.B. Yang,
F.X. Liang, L. Wang, Crystengcomm, 2012, 14, 1942.）Therefore, Se/ZnO p-n hetero-junctions is constructed
Photodetector can effectively improve whole device performance.
Invention content
The purpose of the present invention is to provide it is a kind of it is simple for process, easy to operate, there is excellent ultraviolet detector performance, have
Quick response and Se/ZnO heterojunction photoelectric detectors and preparation method thereof from drive characteristic.
The present invention, which provides, has good crystallinity Se/ZnO bilayer film preparation methods.
Provided by the invention novel from the preparation method for driving Se/ZnO heterojunction ultraviolet photodetectors, specific steps are such as
Under：
（1）It is prepared by ZnO nano particle precursor liquid solution.It is dissolution of raw material in aqueous medium using zinc salt, weak acid, passes through weak acid
The effective hydrolysis for reducing zinc salt.It is stirring evenly and then adding into suitable polyvinylpyrrolidone（PVP）, to improve precursor solution
Viscosity, be configured to stablize and modest viscosity precursor solution；
The zinc salt is the zinc salt compound containing the crystallization water or without the crystallization water, preferably zinc acetate, zinc nitrate etc..It is described
Preferred acetic acid of weak acid etc.；
（2）It is prepared by ZnO nano particle film.By the spin coating under 3000 ~ 5000 revs/min of rotating speed of above-mentioned precursor solution
Uniform film is obtained on the surface of quartz substrate, spin coating rotating speed determines that rotating speed is slower according to required film thickness, and film is thick
Degree is thicker.Film is placed in Muffle furnace later, heating rate is 1 ~ 5 DEG C/min, until 450-800 DEG C, 1.5-3 h are calcined,
It decomposes the organic matter PVP in precursor solution under hot conditions, obtains the good ZnO nano membrana granulosa of crystallinity；
（3）The preparation of Se films.A certain amount of selenium powder is placed in quartz boat to and is positioned over the center of 1 m tube furnaces, away from
From being disposed vertically the above-mentioned quartz plate for having ZnO nano particle film at 30 ~ 35 cm of selenium powder, and the half of quartz plate is blocked；
Under the conditions of the nitrogen or argon gas of 200 ~ 300 sccm flow velocitys, tube furnace central temperature is added from room temperature in 30 ~ 120 min
Heat keeps the temperature 180 ~ 300 min to 300 ~ 330 DEG C under the temperature condition；In insulating process, nitrogen or argon gas are protected always
It holds constant rate and flows to quartz plate from selenium source, it will be on the selenium steam-transfer to ZnO nano particle film that evaporated；It has kept the temperature
Cheng Hou makes central temperature from maximum temperature cooled to room temperature, is obtained on the ZnO nano particle film surface not being blocked
The good selenium film of even and crystallinity, as ZnO/Se films；
（4）Detector is constructed.On the quartz plate of above-mentioned obtained ZnO/Se films, respectively be blocked and not by
The indium electrode that the ZnO film both ends pressing diameter blocked is about 0.3 ~ 1 mm, forms heterojunction photoelectric detector.
In the present invention, step（2）Described in ZnO nano particle film thickness be 50-200 nm.
In the present invention, step（3）Described in Se film thicknesses be 1-2 μm.
Se/ZnO heterojunction ultraviolet photodetectors prepared by the present invention, core cell are that thickness is 50-200 nm
The p-n heterojunction that ZnO particle film is formed with 1-2 μm of Se film.
New ultra-violet photodetector part proposed by the present invention has following features：
（1）With from drive characteristic, i.e., it can also be realized without external bias and generate stable electric current in the case where detecting illumination
Output；
（2）With excellent fast-response energy, under the light source irradiation of pulse laser, rise time and fall time
Within 20 ms, improved close to 4 orders of magnitude compared to pure ZnO nano membrana granulosa；
（3）With high brightness electric current ratio, under ultraviolet light, brightness electric current ratio is up to 104；
（4）It is less than the ultraviolet light Response to selection of 400 nm with wavelength, ultraviolet light response one is less than to the response of visible light
It is more than a magnitude.
Description of the drawings
Fig. 1 is Se/ZnO heterojunction photoelectric device structural schematic diagrams.
Fig. 2 is the microcosmic scanning electron microscope pattern in Se/ZnO bilayer films surface and section.
Fig. 3 is device 300-600 nm spectrum responses.
Fig. 4 is that device electric current under 370nm illumination changes over time curve in the case where switching illumination.
Fig. 5 is quick response curve of the device under pulsed laser irradiation.
Specific implementation mode
Below by specific embodiment, the content further illustrated the present invention, to be best understood from present disclosure and
Unrestricted protection scope of the present invention.
Se/ZnO heterojunction photoelectric devices performance characterization produced by the present invention is as follows：
The microstructure of Se/ZnO bilayer films by Zeiss companies Sigma field emission scanning electron microscopes（FESEM）It observes
It arrives.
The photoelectric properties of Se/ZnO heterojunction photoelectric devices are surveyed by the 4200-SCS semiconductor characterisation instrument of Keithley companies
.
Each test all carries out at ambient conditions, unless otherwise indicated.
It is prepared by embodiment 1, ZnO nano particle film
Take 1 g zinc acetates and 1 g polyvinylpyrrolidones（PVP）It is added in 10 ml deionized waters, mixed solution is stirred
2 h make PVP be completely dissolved and the acetic acid of 0.1 ml are slowly added dropwise in whipping process.Then the precursor solution that will be prepared
It is added drop-wise in clean quartz substrate, and spin-coating film on spin coating instrument, spin coating process is divided into two steps, respectively 500 rev/min of 5 s
With 4000 rev/min of 30 s.Then the film after spin coating is placed in muffle furnace at 550 DEG C in annealing 150 min removal films
Organic matter, obtain the good ZnO film of crystallinity.
Step is repeated above operation, similar product can be obtained by changing zinc acetate into zinc nitrate.
Step is repeated above operation, between second step rotating speed is arranged to 3500-5000 revs/min in spin coating process, can be obtained
The different ZnO film of thickness.
Step is repeated above operation, annealing temperature setting can be obtained into similar product between 500-700 DEG C.
Step is repeated above operation, annealing time setting can be obtained into similar product between 90-360 min.
Embodiment 2, the Se film preparations of ZnO film surface
It is the center that 99.95% selenium powder is placed in 1m tube furnaces in quartz boat to take 1g purity, at selenium powder 30cm
It is disposed vertically the quartz plate for the ZnO nano particle film that half is blocked.55 under the condition of nitrogen gas of 300 sccm flow velocitys
Tube furnace central temperature is heated to 300 DEG C from room temperature in min, and keeps the temperature 180 min under the temperature condition.In insulating process
Nitrogen remains constant rate from the selenium steam-transfer to growth substrate that selenium source flows to quartz plate will evaporate.Heat preservation
After the completion, central temperature is from maximum temperature cooled to room temperature.It can be grown on the ZnO nano particle film surface not being blocked
One layer of uniform and good Se film of crystallinity.
Step is repeated above operation, there will be the quartz plate of ZnO film to be positioned over away from 35 cm of selenium powder, while flow velocity being reduced
To 250 sccm, similar product can be obtained.
Step is repeated above operation, holding temperature is increased to 330 DEG C, and simultaneously reduce soaking time to 180
Min can obtain similar product.
Step is repeated above operation, holding temperature is only increased to 330 DEG C, the thicker Se films of thickness can be obtained.
Step is repeated above operation, soaking time is only reduced to the Se films that can obtain thinner thickness to 180 min.
Step is repeated above operation, changes nitrogen into argon gas, similar product can be obtained.
Embodiment 3, the test of Se/ZnO heterojunction photoelectric device photoelectric properties
On the quartz plate of obtained ZnO/Se films, pressed respectively at the ZnO film both ends for being blocked and not being blocked
The indium electrode that diameter is about 0.5 mm forms heterojunction photoelectric detector and with photoelectricity test system test performance.0
V does not have under illumination condition, and the dark current of device is about 1 pA, in the case where wavelength is the ultraviolet light of 370 nm, the output of device
Electric current is about 10 nA, and brightness electric current ratio reaches 104.Device equally has response speed quickly, and in 0.5 s, electric current can be with
Decline 3 magnitudes, rises nearly 4 magnitudes.Under the irradiation of pulse laser, rising and falling time be respectively 0.69 ms and
13.5 ms.In addition, device also has good ultraviolet selective, the responsiveness of ultraviolet light is about 10 times of visible light.
Claims (5)
1. a kind of from the preparation method for driving Se/ZnO heterojunction ultraviolet photodetectors, which is characterized in that be as follows：
（1）It is prepared by ZnO nano particle precursor liquid solution
It is dissolution of raw material in aqueous medium using zinc salt, weak acid, is stirring evenly and then adding into suitable polyvinylpyrrolidone（PVP）,
It is configured to stablize the precursor solution with modest viscosity；
The zinc salt is the zinc salt compound containing the crystallization water or without the crystallization water；
（2）It is prepared by ZnO nano particle film
Above-mentioned precursor solution is spin-coated on to the surface of quartz substrate under 3000 ~ 5000 revs/min of rotating speed, is obtained uniform
Film, spin coating rotating speed are determined according to required film thickness；Film is placed in Muffle furnace later, with heating rate be 1 ~ 5 DEG C/
Min is warming up to 450-800 DEG C, calcines 1.5-3 h, so that the organic matter PVP in precursor solution is decomposed, it is good to obtain crystallinity
ZnO nano particle film；
（3）The preparation of Se films
A certain amount of selenium powder is placed in quartz boat to and is positioned over the center of 1 m tube furnaces, is being hung down at 30 ~ 35 cm of selenium powder
The above-mentioned quartz substrate for having ZnO nano particle film is directly placed, and the half of quartz substrate is blocked；In 200 ~ 300 sccm
Under the conditions of the nitrogen or argon gas of flow velocity, tube furnace central temperature is heated to 300 ~ 330 from room temperature in 30 ~ 120 min
DEG C, and 180 ~ 300 min are kept the temperature under the temperature condition；In insulating process, nitrogen or argon gas remain constant rate
Quartz substrate is flowed to from selenium source, it will be on the selenium steam-transfer to ZnO nano particle film that evaporated；After the completion of heat preservation, in making
Heart temperature is obtained uniformly and is crystallized from maximum temperature cooled to room temperature, on the ZnO nano particle film surface not being blocked
Spend good selenium film, as ZnO/Se films；
（4）Detector is constructed
In the quartz substrate of above-mentioned obtained ZnO/Se films, respectively at the ZnO film both ends for being blocked He not being blocked
The indium electrode that diameter is 0.3 ~ 1 mm is pressed, heterojunction photoelectric detector is formed.
2. preparation method according to claim 1, which is characterized in that step（1）Described in zinc salt be selected from zinc acetate or nitre
Sour zinc；The weak acid is acetic acid.
3. preparation method according to claim 1, which is characterized in that step（2）Described in ZnO nano particle film thickness
For 50-200 nm.
4. preparation method according to claim 1, which is characterized in that step（3）Described in Se film thicknesses be 1-2 μm.
5. a kind of driving Se/ZnO heterojunction ultraviolet photodetections certainly being prepared by preparation method described in claim 1
Device, core cell are the p-n heterojunctions that the ZnO nano particle film that thickness is 50-200 nm is formed with 1-2 μm of Se film.
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