CN107579138B - A kind of full-inorganic perovskite Schottky photodetector and preparation method thereof - Google Patents
A kind of full-inorganic perovskite Schottky photodetector and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of full-inorganic perovskite Schottky photodetectors and preparation method thereof.The detector is by Si/SiO2Substrate, ITO or so electrode, perovskite micro wire composition.Using two-step method fabricated in situ CsPbBr on substrate3Perovskite micro wire, i.e., first synthesize PbI2Micro wire, CsPbBr is then obtained by way of ion exchange in CsBr methanol solution3Perovskite micro wire.Schottky junction is formed using ITO electrode and perovskite, realizes the quickly excellent photosensitive detection performance of ultraviolet-visible.Micro wire is made of nano particle and has porous structure, it can be achieved that Multiple Scattering to light, obtained detector have the characteristics that responsiveness height, high sensitivity, response restore fast.
Description
Technical field
The invention belongs to nano material preparations and photoelectron to use field, relate generally to a kind of full-inorganic CsPbBr3Calcium titanium
Ultraviolet-visible Schottky type photodetector of mine multi-pore micron line and preparation method thereof.
Technical background
In recent years, photoelectron scientific development is very rapid, and wherein photodetector can directly turn optical signal as one kind
The device for changing electric signal into has obtained the very big concern of scientific research personnel, and various types of photodetector layers go out not poor.Quotient at present
The detector of industry is mainly silicon-based detector, but silicon-based detector spectral selection is poor, often to cooperate optical filter to realize
Spectral selection detection, this increases its cost of manufacture, and structure is sufficiently complex, is unfavorable for its further development.So finding
A kind of low in cost, production is simple, spectral selection is good material becomes the research hotspot of scientific research personnel.
Studying more perovskite material in recent years, band gap is adjustable, absorptivity is good, carrier mobility since it possesses
Height can use the features such as inexpensive solwution method preparation, be expected to replace silicon materials, become next-generation photoelectron material.Currently based on calcium
The photodetector of titanium ore material has been achieved for many important research achievements.Such as Paul Meredith seminar report
A kind of perovskite photodetector for the high spectral selectivity not needing optical filter, causes great repercussion in the world,
Its achievement is published on Nature Photonics (Qianqian Lin, Ardalan Armin, Paul L.Burn and
Paul Meredith.Filterless narrowband visible photodetectors.Nature Photonics,
2015,175), and related patents are achieved.And the detection that the standby perovskite photodetector of Yang Yang project team system obtains
High sensitivity is up to 1014Jones, linear dynamic range reach excellent properties (the Letian Dou, Yang (Micheal) of 100dB
Yang, Jingbi You, Ziruo Hong, Wei-Hsuan Chang, Gang Li, Yang Yang.Solution-
processed hybrid perovskite photodetectors with high detectivity.Nature
Communication 2014,5:5404.), therefore perovskite photodetector has very big development prospect.But it is above-mentioned to be based on
Its structure of the photodetector of perovskite material is all that hetero-junctions or PIN structural, hetero-junctions complex manufacturing technology, and performance are held
Vulnerable to effect of the interface, for example cause very big leakage current, simultaneously because the limitation of hetero-junctions itself, responsiveness also up for
It further increases, and above-mentioned perovskite used is all organic inorganic hybridization perovskite-like, wherein organic molecule is in high temperature and humidity
And it is all unstable in air, therefore there is also very big challenges for its practice.In order to improve the performance of device, low dimensional structures
Perovskite detector be to select well.For example someone is with traditional nano impression (Honglei Wang, Ross
Haroldson, Balasubramaniam Balachandran, Alex Zakhidov, Sandeep Sohal, Julia
Y.Chan, Anvar Zakhidov and Walter Hu.Nanoimprinted Perovskite Nanograting
Photodetector with Improved Efficiency.ACS NANO) or template (Jiangang Feng, Xiaoxu
Yan, Yun Liu, Hanfei Gao, Yuchen Wu, Bin Su and Lei Jiang.Crystallographically
Aligned Perovskite Structures for High-Performance Polarization-Sensitive
Photodetectors.Advanced Materials 2017,1605993) obtain the perovskite array of high quality, property
It can be greatly improved, but these methods require harshness to growth conditions, need to accomplish accurately to control.So finding one kind
The simple and stable perovskite photodetector of structure, manufacture craft is the side of the emphasis that researcher pays close attention at present and effort
To.In this respect, a series of important achievement is had been achieved for recently.Such as it is a kind of based on the full-inorganic calcium titanium synthesized at room temperature
The Au/CsPbBr of mine quantum dot (QDs) preparation3The photodetector of QDs/Au structure makes its property by Au plasma enhancing
Can be greatly improved (Yuhui Dong, Yu Gu, Yousheng Zou, Jizhong Song, Leimeng with stability
Xu, Jianhai Li, Jie Xue, Xiaoming Li, and Haibo Zeng.Improving All-Inorganic
Perovskite Photodetectors by Preferred Orientation and Plasmonic Effect.Small
2016.).It then has been reported that again and successfully synthesizes two-dimentional CsPbBr3Ultrathin nanometer piece (NPs), and it is prepared for Au/CsPbBr3NPs/
Peak response degree has been increased to 34A/W (Xuhai Liu, Dejian Yu, Fei Cao, Xiaoming by the detector of Au structure
Li, Jianping Ji, Jun Chen, Xiufeng Song, and Haibo Zeng.Low-Voltage
Photodetectors with High Responsivity Based on Solution-Processed Micrometer-
Scale All-Inorganic Perovskite Nanoplatelets.Small 2017.).But above-mentioned detector is main
It is based on Au and CsPbBr3Ohmic contact type detector, under higher applied voltage, dark current can become very big, this is right
The influence of detector performance is fairly obvious, so dark current is greatly a key factor for restricting detector development, is in addition limited
In the size of quantum dot and nanometer sheet, certain requirement is proposed to the size of channel.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of structure is special and simply perovskite-based Xiao of preparation process
Special base contact-type ultraviolet-visible photodetector and preparation method thereof.The detector has good spy in ultraviolet-visible wave band
Survey ability, and there is preferable thermal stability.
A kind of preparation method of full-inorganic perovskite micro wire, includes the following steps:
Step (1) configures PbI2/ DMF (dimethylformamide) mixed solution, PbI2: the mass ratio of DMF is 1:7~1:
12, it is then stirred at 60~90 DEG C, makes PbI2It is completely dissolved, a certain amount of deionized water is then added, forms it into supersaturation
Solution is stood at room temperature, makes PbI2Recrystallization is precipitated, and obtains PbI2The suspension of micro wire；
Step (2), with sol evenning machine by PbI obtained by step (1)2The suspension of micro wire is spun on substrate, is then immersed in
It is sufficiently reacted into CsBr methanol solution, growth obtains CsPbBr3Perovskite micro wire.
Preferably, PbI obtained by step (1)2Micron linear diameter is 2~5 μm, and length is 30~60 μm.
Preferably, PbI in step (1)2: the mass ratio of DMF is 1:9.5.
Preferably, the concentration of the CsBr methanol solution used in step (2) is 3~10mg/ml.
Preferably, by PbI in step (2)2After the suspension of micro wire is spun on substrate, anneal at 70~100 DEG C
10~30min, then immerse in CsBr methanol solution.
Preferably, resulting CsPbBr3Micro wire is made of nano particle and has porous structure.
A kind of preparation method of full-inorganic perovskite Schottky photodetector, includes the following steps:
Step a, substrate clean and to be dried with nitrogen；
Step b, preparation is in the ITO electrode of tiled configuration on the substrate obtained by step a；
Step c, using the preparation method of above-mentioned full-inorganic perovskite micro wire, by PbI2The suspension of micro wire is spun to
On the resulting substrate of step b, continue the preparation method using above-mentioned full-inorganic perovskite micro wire, in the resulting substrate of step b
On grow CsPbBr3Perovskite micro wire；
Step d, by gained CsPbBr3Perovskite micro wire is made annealing treatment, and full-inorganic perovskite Schottky light is obtained
Electric explorer ITO/CsPbBr3/ITO。
Preferably, the ITO electrode of the tiled configuration includes left electrode and right electrode, between the left electrode and right electrode
Channel distance should be less than gained PbI2Micro wire and CsPbBr3The length of micro wire, to form Schottky junction structure.
Preferably, the substrate is Si/SiO2, SiO2With a thickness of 280nm.
Preferably, annealing temperature described in step d is 50~250 DEG C, and the time is 10~30min.
A kind of full-inorganic perovskite Schottky photodetector, is prepared using the above method.
The present invention successfully synthesizes one-dimensional full-inorganic CsPbBr by simple two steps solwution method3Perovskite micro wire, it is micro-
It is to be made of many nano-perovskite particles in rice noodles, there is the features such as large specific surface area, porous, this is conducive to the multiple of light
Scattering and absorption.Based on these features, we are prepared for a kind of ITO/CsPbBr3The detector of/ITO structure, CsPbBr3With ITO
Show as Schottky contacts.Since there are Schottky barriers between perovskite and electrode, so dark current very little, is pico-ampere level, because
And this detector has the characteristics that responsiveness height, high sensitivity, response recovery time are fast.Additionally, due to being full-inorganic material system
Standby, which also has preferable thermal stability.Our growth conditions adjustable extent is big simultaneously, protects without inert gas
Shield, technique very simple.This has established certain basis to the development of perovskite-based detector.
Compared with the prior art, the invention has the characteristics that:
1, it is prepared using whole soln method, is not necessarily to inert gas shielding, operating procedure is simple, and it is at low cost, it is suitable for mass production；
2, prepared perovskite-based detector is schottky junction, has cracking response resume speed, there is very big answer
Use potentiality；
3, it is made of perovskite nano particle inside micro wire, and there are a large amount of hole, conducive to absorption to light and more
Secondary scattering.
4, CsPbBr3Micro wire has good thermal stability, is conducive to the photo and thermal stability for improving device；
5, device investigative range is ultraviolet-visible wave band (300~550nm), is rung in 520nm with highest under -5V bias
Response 18.8A/W, 300nm responsiveness is 7.8A/W；
6, there is very low dark current, therefore detectivity is very high, close to 1013Jones.
Detailed description of the invention
Fig. 1 is the device junction composition of perovskite micron line detector, in which: 1, Si/SiO2Substrate；2, ITO left electrodes；3,
The right electrode of ITO；4, CsPbBr3Micro wire；
Fig. 2 is the voltage-current curve of perovskite photodetector prepared by embodiment 1；
Fig. 3 is the spectral response curve of perovskite photodetector prepared by embodiment 1；
Fig. 4 is the voltage-current curve of perovskite photodetector prepared by embodiment 2；
Fig. 5 is the spectral response curve of perovskite photodetector prepared by embodiment 2；
Fig. 6 is the voltage-current curve of the perovskite photodetector prepared by embodiment 3 is annealed at 50 DEG C；
Fig. 7 is the voltage-current curve of the perovskite photodetector prepared by embodiment 3 is annealed at 250 DEG C；
Fig. 8 is that the perovskite photodetector prepared by embodiment 4 is annealed at 50 DEG C is bent in 50 DEG C of voltage-to-current
Line；
Fig. 9 is the voltage-current curve of the perovskite photodetector prepared by embodiment 4 is annealed at 250 DEG C.
Specific embodiment
The main preparation step of full-inorganic perovskite Schottky photodetector of the invention is as follows:
The cleaning of substrate, in the present invention, Si/SiO can be used in substrate2Or glass substrate, it mainly adopts in the present embodiment
Use Si/SiO2Substrate.Substrate is cut into the size (1cm × 1cm) being sized for first, then successively uses deionized water, third
Ketone, dehydrated alcohol, deionized water are cleaned by ultrasonic 10min in ultrasonic cleaning instrument respectively, then with being dried with nitrogen, obtain clean
Substrate.
Photoetching and magnetron sputtering technique are mainly used in the preparation of the ITO electrode of tiled configuration.
(1) photoresist is uniformly spin-coated on clean Si/SiO with sol evenning machine first by photoetching2On substrate, condition is
600 revs/min low speed rotation 6 seconds, then with 2000 revs/min high speed rotation 15 seconds；The substrate of spin coating photoresist is in 100 DEG C of front bakings
1min；Then it is exposed using mask plate；Development after exposed, the proportion of developer solution are tetramethyl aqua ammonia: deionization
Water=1:10, developing time are 60 seconds, are then rinsed 15 seconds in deionized water；Substrate after rinsed dries after 100 DEG C
1min。
(2) it sputters, it is intracavitary that the good substrate of photoetching is transferred to magnetron sputtered vacuum, and place ITO target, target purity >
99.99%, background vacuum is better than 1 × 10-3Pa when sputtering, argon flow 12 standard ml/min, and 70 DEG C of underlayer temperature, sputtering
The substrate for having sputtered ITO electrode is immersed ultrasound 5min in acetone, by remaining photoresist by power 100W, sputtering time 10min
It completely removes, obtained ITO electrode is in 200 DEG C of annealing 30min, and channel distance is electric for 10 microns of ITO between obtaining left and right electrode
Pole.
The growth of perovskite weighs a certain amount of PbI in the balance2It is added in a certain amount of DMF (dimethylformamide),
In 60~90 DEG C of stirrings sufficiently dissolution, it is then slowly added into a certain amount of deionized water, it can be found that solution becomes cloudy, it is then clear
Clearly, then standing 10~12h at room temperature can be obtained PbI2Micro wire suspension, at 2~5 microns, length exists diameter
30~60 microns, surface is smooth, very smooth.10 microlitres of PbI are taken with dropper2Micro wire suspension is spun to ITO electrode
On substrate, then in 100 DEG C of annealing 10min, then sample is put into certain density CsBr methanol solution and is reacted, can be obtained
Full-inorganic perovskite Schottky photodetector containing full-inorganic perovskite micro wire is inside full-inorganic perovskite micro wire
It is made of a large amount of nano particles.
The test of device, in order to illustrate the performance of perovskite detector of the invention, we are tested using photodetector
System has carried out a series of electrical measurements to device, mainly includes voltage-current curve under monochromatic light, current versus time curve, light
Compose response curve.
The present invention is further described below with reference to embodiment, the description be intended merely to better illustrate the present invention rather than
It is limited.The present invention is not limited to particular example as described herein and embodiments.Technology in any this field
Personnel are easy to be further improved without departing from the spirit and scope of the present invention and perfect, both fall within the present invention
Protection scope.
Embodiment 1:
1, substrate cleaning: with above-mentioned cleaning process to Si/SiO2Substrate is cleaned.
2, the preparation of ITO electrode: as the above method prepares ITO electrode using photoetching and sputtering technology.
3, perovskite micro wire growth: configuration PbI2/ DMF mixed solution, PbI2: the mass ratio of DMF is 1:9.5, at 80 DEG C
Stirring is allowed to be completely dissolved, and a certain amount of deionized water is then added, forms it into supersaturated solution, then at room temperature
Stand 10h.PbI2Since recrystallization is precipitated, PbI is obtained2The suspension of micro wire simultaneously can long-term preservation；Gained is contained with sol evenning machine
There is PbI2The suspension of micro wire is spun on the substrate of ITO electrode, through 100 DEG C of annealing 10min, makes PbI2Preferably crystallization,
It places the substrate into and is reacted under room temperature in the CsBr methanol solution of 3mg/ml 1 hour.It takes out substrate to be cleaned with isopropanol, be used in combination
Nitrogen dries up isopropanol.Obtained sample is annealed at 50 DEG C, time 10min.Obtain ITO/CsPbBr3/ ITO knot
The full-inorganic perovskite Schottky photodetector of structure, as shown in Figure 1, wherein 1, Si/SiO2Substrate；2, ITO left electrodes；3,
The right electrode of ITO；4, CsPbBr3Micro wire rough surface can be observed in micro wire, is made of many nano particles.
4, test: obtained sample is placed on probe station, left and right electrode adds scanning voltage, obtains dark current and difference
Photoelectric current under wavelength, as shown in Figure 2, it is seen that it mainly generates photoelectric current in ultraviolet and visible waveband.By formula:
Wherein R is responsiveness, JphFor density of photocurrent, LlightFor light intensity, its spectral response curve, such as Fig. 3 can be calculated,
The perovskite detection implement body probing wave that the present embodiment can be obtained is grown in 300~550nm, and under the bias of -5V, 520nm is obtained
Peak response degree 18.86A/W is 7.83A/W in the ultraviolet band responsiveness of 300nm.
Embodiment 2
1, the cleaning of substrate: with embodiment 1.
2, the preparation of ITO electrode: with embodiment 1.
3, perovskite micro wire growth: configuration PbI2/ DMF mixed solution, PbI2: the mass ratio of DMF is 1:7, in 70 DEG C of items
Stirring is allowed to be completely dissolved under part, and a certain amount of deionized water is then added, forms it into supersaturated solution, then in room temperature item
12h is stood under part.PbI2Since recrystallization is precipitated, PbI is obtained2The suspension of micro wire simultaneously can long-term preservation；With sol evenning machine by institute
PbI must be contained2The suspension of micro wire is spun on the substrate of ITO electrode, through 100 DEG C of annealing 10min, makes PbI2Preferably
Crystallization；It is then immersed in the CsBr methanol solution of 3mg/ml and reacts 2 hours, growth obtains CsPbBr3Perovskite micro wire.It takes
Substrate is cleaned with isopropanol out, and is dried up isopropanol with nitrogen.Obtained sample is annealed at 250 DEG C, and the time is
10min。
4, test: sample is placed on probe station, left and right electrode adds scanning voltage, obtains under dark current and different wave length
Photoelectric current, as shown in Figure 4.For spectral response curve as shown in figure 5, under -5V bias, 520nm obtains peak response degree
15.35A/W is 5.82A/W in the ultraviolet band responsiveness of 300nm.
Embodiment 3
1, the cleaning of substrate: with embodiment 1.
2, the preparation of ITO electrode: with embodiment 1.
3, perovskite micro wire growth: configuration PbI2/ DMF mixed solution, PbI2: the mass ratio of DMF is 1:12, is then existed
90 DEG C of stirrings are allowed to be completely dissolved, and a certain amount of deionized water is then added, forms it into supersaturated solution, then in room temperature item
10h is stood under part.PbI2Since recrystallization is precipitated, PbI is obtained2The suspension of micro wire simultaneously can long-term preservation.With sol evenning machine by institute
PbI must be contained2The suspension of micro wire is spun on the substrate of ITO electrode, through 100 DEG C of annealing 10min, makes PbI2Preferably
Crystallization, is then immersed in the CsBr methanol solution of 3mg/ml and reacts 1 hour, and growth obtains CsPbBr3Perovskite micro wire.It takes
Substrate is cleaned with isopropanol out, and is dried up isopropanol with nitrogen.Obtained sample carries out 30min at 50 and 250 DEG C respectively
Annealing.
4, test: sample is placed on probe station, left and right electrode adds scanning voltage, obtains under dark current and different wave length
Photoelectric current, be illustrated in figure 6 50 DEG C of voltage-current curve, obtain under -5V bias, 520nm responsiveness be 0.33A/W,
300nm responsiveness is 0.92A/W.It is illustrated in figure 7 250 DEG C of voltage-current curve, is obtained under -5V bias, 520nm is rung
Response is 0.19A/W, and 300nm responsiveness is 0.94A/W.
Embodiment 4
1, the cleaning of substrate: with embodiment 1.
2, the preparation of ITO electrode: with embodiment 1.
3, the growth of perovskite micro wire: PbI is first grown as described in Example 32Micro wire will stand 10 hours PbI2It is micro-
Rice noodles are spun to the substrate of ITO electrode.Place the substrate into the CsBr methanol solution of 10mg/ml that react 1 under room temperature small
When.It takes out substrate to be cleaned with isopropanol, and is dried up isopropanol with nitrogen.Obtained sample carries out at 50 and 250 DEG C respectively
10min annealing.
4. test: sample being placed on probe station, left and right electrode adds scanning voltage, obtains under dark current and different wave length
Photoelectric current, be illustrated in figure 8 50 DEG C of voltage-current curve, obtain under -5V bias, 520nm responsiveness be 1.33A/W,
300nm responsiveness is 4.53A/W.It is illustrated in figure 9 250 DEG C of voltage-current curve, is obtained under -5V bias, 520nm is rung
Response is 1.27A/W, and 300nm responsiveness is 8.26A/W.
The data that above embodiments obtain illustrate the one-dimensional CsPbBr using solwution method synthesis3The micro-nano multistage knot of perovskite
The multi-pore micron line of structure can Successful utilization in perovskite photodetector.It forms Schottky contacts, structure letter with ITO electrode
Single, preparation process is simple, and has the characteristics that high-responsivity, high sensitivity, quick.And solution concentration can in reaction process
It adjusts, there is very big practicability, and when device is after 50 and 250 DEG C of processing, device still has good performance, illustrates its tool
There is good thermal stability.
Claims (9)
1. a kind of preparation method of full-inorganic perovskite micro wire, which comprises the steps of:
Step (1) configures PbI2/ DMF mixed solution, PbI2: the mass ratio of DMF is 1:7~1:12, is stirred at 60~90 DEG C,
Make PbI2It is completely dissolved, a certain amount of deionized water is then added, form it into supersaturated solution, stand at room temperature, make
PbI2Recrystallization is precipitated, and obtains PbI2The suspension of micro wire；
Step (2), with sol evenning machine by PbI obtained by step (1)2The suspension of micro wire is spun on substrate, is then immersed in CsBr
It is sufficiently reacted in methanol solution, growth obtains CsPbBr3Perovskite micro wire.
2. the preparation method of full-inorganic perovskite micro wire according to claim 1, which is characterized in that obtained by step (1)
PbI2Micron linear diameter is 2~5 μm, and length is 30~60 μm.
3. the preparation method of full-inorganic perovskite micro wire according to claim 1, which is characterized in that step is adopted in (2)
The concentration of CsBr methanol solution is 3~10mg/ml.
4. the preparation method of full-inorganic perovskite micro wire according to claim 1, which is characterized in that will in step (2)
PbI2After the suspension of micro wire is spun on substrate, anneal 10~30min at 70~100 DEG C, then to immerse CsBr methanol molten
In liquid.
5. the preparation method of full-inorganic perovskite micro wire according to claim 1, which is characterized in that resulting CsPbBr3
Micro wire is made of nano particle and has porous structure.
6. a kind of preparation method of full-inorganic perovskite Schottky photodetector, which comprises the steps of:
Step a, substrate clean and to be dried with nitrogen；
Step b, preparation is in the ITO electrode of tiled configuration on the substrate obtained by step a；
Step c, using the described in any item methods of claim 1-5, by PbI2The suspension of micro wire is spun to obtained by step b
Substrate on, continue to grow CsPbBr on the resulting substrate of step b using the described in any item methods of claim 1-53
Perovskite micro wire；
Step d, by gained CsPbBr3Perovskite micro wire is made annealing treatment, and full-inorganic perovskite Schottky photodetection is obtained
Device ITO/CsPbBr3/ITO。
7. the preparation method of full-inorganic perovskite Schottky photodetector according to claim 6, which is characterized in that institute
The substrate stated is Si/SiO2。
8. the preparation method of full-inorganic perovskite Schottky photodetector according to claim 6, which is characterized in that step
The temperature of annealing described in rapid d is 50~250 DEG C, and the time is 10~30min.
9. a kind of full-inorganic perovskite Schottky photodetector, which is characterized in that using any one of the claims 6-8 institute
The method of stating is prepared.
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