CN107342365B - A kind of perovskite photodetector and preparation method thereof - Google Patents
A kind of perovskite photodetector and preparation method thereof Download PDFInfo
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- CN107342365B CN107342365B CN201710495524.6A CN201710495524A CN107342365B CN 107342365 B CN107342365 B CN 107342365B CN 201710495524 A CN201710495524 A CN 201710495524A CN 107342365 B CN107342365 B CN 107342365B
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/20—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising organic-organic junctions, e.g. donor-acceptor junctions
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- H—ELECTRICITY
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- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
- H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
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Abstract
The present invention provides a kind of stable perovskite photodetectors, the substrate (1) that is sequentially connected is blended active layer (2), electrode (3), and the blendings active layer (2), which is perovskite, and poly- 3- hexyl thiophene is blended makes poly- 3- hexyl thiophene be wrapped in perovskite surface to form.Further the present invention provides the preparation methods of photodetector, comprising the following steps: substrate prepares and cleaning, processing；Perovskite precursor solution is prepared, then crystallizes to form perovskite nano-powder dispersion liquid by solvent-induced method；Prepare poly- 3- hexyl thiophene solution；Prepare the blend solution of perovskite and poly- 3- hexyl thiophene；Perovskite and poly- 3- hexyl thiophene blend film are prepared using spin coating or blade coating mode, high quality is obtained after thermal anneal process, active layer is blended；Electrode is prepared using vapour deposition method.Product of the invention has many advantages, such as that the response time is short, stablizes in air, is at low cost.
Description
Technical field
The present invention relates to photoelectric device technical fields, and in particular to a kind of stable perovskite photodetector and its preparation
Method.
Background technique
Photodetector can effectively detect optical signal, measurement intensity of illumination, and the optical signal of time correlation is turned
Change electric signal into.Therefore, have in fields such as bio-sensing, optical imagery, optic communication, environmental monitoring, defence and militaries extensive
Application.Past decades, the semiconductor materials such as silicon, molybdenum disulfide, indium gallium arsenic, zinc oxide, cadmium sulfide are applied to light
Electrical resistivity survey is surveyed.
It is compared to above-mentioned material, the perovskite (CH of organic inorganic hybridization3NH3PbA3Or CH3NH3PbA3-xBx, wherein A, B
=I, Cl or Br) it is receive more and more attention.There is suitable forbidden bandwidth, high absorption just because of perovskite material
Coefficient, the electron hole pair diffusion length of length and carrier lifetime and outstanding charge transmission, so that perovskite material
It is used widely in photovoltaic industry, such as photodetector, Light-Emitting Diode, laser device.Perovskite material was in 2009
It is applied to solar battery for the first time, and achieves 3.81% photoelectric conversion efficiency.Through research and development in a few years, current
The photoelectric conversion efficiency of perovskite solar battery is more than 20%.
It is well known that perovskite material is very sensitive to hydrone, and when exposing in air, perovskite material meeting and air
In water react, cause perovskite material decompose and fail.Therefore, perovskite material or device are improved by suitable means
The aerial stability of part is to improve perovskite photoelectric device service life and promote perovskite photodetector practical
Key also becomes the key technology for developing perovskite material practical application.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
The stable perovskite photodetector of performance in kind photodetection excellent performance, air correspondingly provides a kind of technical process letter
List, good product performance, the preparation method of aforementioned stable perovskite photodetector at low cost.
First aspect present invention provides a kind of perovskite photodetector, including substrate, the blending activity being sequentially connected
Layer, electrode, the blending active layer are that perovskite and the blending of poly- 3- hexyl thiophene make poly- 3- hexyl thiophene be wrapped in perovskite table
Face forms, and the perovskite is perovskite nano-powder, and perovskite chemical formula is CH3NH3PbA3, wherein A=I, Cl or Br.
For the use condition of perovskite photodetector, the invention proposes one kind with perovskite and poly- 3- hexyl thiophene
Bulk-heterojunction structure of the blend film as active layer, is based particularly on following thinking and research experience: perovskite material is
Emerging light absorbing material absorbs preferable optical absorption characteristics in ultraviolet, visible light, near infrared region, can satisfy light
The requirement that electrical resistivity survey is surveyed.But the photoelectric detector of simple perovskite thin film is not able to satisfy the requirement of atmospheric environment, calcium
Titanium ore material can with the water molecule reaction in atmosphere and decompose, so as to cause photoelectric properties failure.Poly- 3- hexyl thiophene (P3HT)
Be it is a kind of have prepare it is simple, at low cost, can low temperature preparation outstanding organic semiconducting materials, poly- 3- hexyl thiophene is with excellent
Air stability, water in air and oxygen diffusion can be prevented, to realize the protection to perovskite material.In addition, poly-
3- hexyl thiophene has extraordinary air stability and high hole mobility, realizes bulk-heterojunction structure by being blended, by
It is matched in the interface energy level of two class materials, to achieve the purpose that light absorption enhances.By our research repeatedly, poly- 3- hexyl
Thiophene is wrapped in perovskite nano powder surface, and the separation of photo-generate electron-hole pairs may be implemented, and reduces answering for electron hole pair
It closes, to improve the performance of photodetector, finally provides premise and basis for the implementation and realization of the technology of the present invention thinking.
Preferably, the blending active layer thickness is 50~500nm.
More preferred, the substrate is silica, potsherd or thin polymer film.
Second aspect of the present invention provides the preparation method of above-mentioned perovskite photodetector, and step includes:
S1, it is handled by substrate cleaning, drying, with UV-ozone；
S2, perovskite precursor solution is prepared, then crystallizes to form the dispersion of perovskite nano-powder by solvent-induced method
Liquid；
S3, poly- 3- hexyl thiophene solution is prepared；
S4, the blend solution for preparing perovskite and poly- 3- hexyl thiophene；
S5, perovskite and poly- 3- hexyl thiophene blend film, thermal annealing are prepared in substrate using spin coating or blade coating mode
It obtains that active layer is blended after processing；
S6, electrode is prepared on active layer is blended using vapour deposition method.
Specifically, in step S1, the cleaning of substrate, drying, handled with UV-ozone refer to by substrate using deionized water,
Acetone, dehydrated alcohol are cleaned by ultrasonic respectively, are then dried up using high-purity gas, and finally UV-ozone is handled 20 minutes again.Pass through
Above-mentioned steps ultrasonic cleaning, high-purity gas drying, can effectively remove organic matter, impurity of substrate surface etc., advantageously form
The blending active layer of high quality；In addition, handling substrate by UV-ozone, blend solution can be improved in the infiltration of substrate surface
Property, be conducive to the formation that active layer is blended.
Preferably, in step S2, the perovskite precursor solution preparation steps include: by CH3NH3A:PbA2By mole
It after being weighed than 1:1, is dissolved in N-N dimethylformamide, forms concentration in the perovskite presoma of 300mg/ml~600mg/ml
Solution, heating stirring 12h at a temperature of 60 DEG C.Using said ratio, and by means such as heating, stirrings, material can be made to fill
Divide and dissolve each other, to guarantee the proportion of each component in film seat preparation process, react film can sufficiently in subsequent anneal link,
Reduce the PbI of remaining2、PbCl2Or PbBr2Substance.
Preferably, described that the step of forming perovskite nano-powder dispersion liquid is crystallized by solvent-induced method in step S2
Include: by perovskite precursor solution: after 100:1~5 is mixed by volume, perovskite crystal is precipitated to be formed perovskite and receives solvent
Rice flour dispersion liquid, the solvent are one or more of chlorobenzene, o-dichlorohenzene.By solvent engineering philosophy, chlorobenzene is selected
Or the anti-solvent of o-dichlorohenzene this perovskite-like substance, perovskite crystal can be made quickly to be precipitated in chlorobenzene or o-dichlorohenzene,
To obtain perovskite nano-powder dispersion liquid.
Preferably, in step S3, the poly- 3- hexyl thiophene solution preparation steps include: by poly- 3- hexyl thiophene: chlorobenzene
200:1~3 mix after weighing in mass ratio, form concentration in the poly- 3- hexyl thiophene solution of 5mg/ml~15mg/ml.
Preferably, in step S4, the blend solution preparation steps of the perovskite and poly- 3- hexyl thiophene include: by poly- 3-
Hexyl thiophene solution: perovskite nano-powder dispersion liquid presses the volume ratio of 20:1~2, is uniformly mixed.Due to poly- 3- hexyl thiophene
Solution and perovskite nano-powder dispersion liquid are benzene kind solvent, during two substances dissolve each other to form blend solution, energy
It is enough sufficiently mixed, in subsequent film forming, is easier to obtain the finely dispersed bulk-heterojunction structure film of perovskite.
Preferably, in step S5, the thermal anneal process is 10~120min of annealing at 80~120 DEG C.Pass through
Above-mentioned annealing can guarantee that perovskite sufficiently reacts, form the crystalline membrane of high quality.
The beneficial effects of the present invention are:
1. stable perovskite photodetector of the invention is designed using bulk-heterojunction structure, composite material function is utilized
It can be superimposed and the principle that has complementary advantages, light absorbing material receives body using perovskite nanometer, and organic material selects poly- 3- hexyl thiophene.Calcium
Titanium ore material has outstanding photoelectric characteristic, for example suitable direct band gap width, lesser excitation combine energy, wider absorption
Bandwidth, longer exciton diffusion length and carrier lifetime.Poly- 3- hexyl thiophene organic material of the invention has extraordinary
Air stability, the bulk-heterojunction structure of formation can make poly- 3- hexyl thiophene package perovskite nano-powder, the protective layer of formation
Increase the air service life of perovskite material；In addition, poly- 3- hexyl thiophene organic material has high exciton mobility, make photoproduction
The network transmission that carrier is formed by poly- 3- hexyl thiophene forms stable perovskite photodetector to electrode.
2. the more simple perovskite material photodetector of the present invention, as perovskite thin film, perovskite monocrystalline, perovskite are received
The photodetectors such as rice noodles, perovskite nanometer sheet, service life is significantly improved in optical detection performance and air.
On the whole, the present invention provides a kind of stable perovskite photodetector, the photodetector finally obtained
The distinguishing feature good, at low cost with air stability substantially improves the optical detection of simple perovskite thin film photodetector
Performance and used life is of great significance to perovskite-based photodetector functionization is improved.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the stable perovskite photodetector structure schematic diagram of the present invention.
Fig. 2 is perovskite organic heterojunction cross-sectional scans electromicroscopic photograph in the embodiment of the present invention 1.
Fig. 3 is the X-ray diffraction spectrum of perovskite dispersion liquid in the embodiment of the present invention 1.
Fig. 4 is photoelectric current-voltage curve of perovskite photodetector stable in the embodiment of the present invention 1.
Fig. 5 is the response time-photocurrent curve of perovskite photodetector stable in the embodiment of the present invention 1.
Fig. 6 is the stability curve of perovskite photodetector stable in the embodiment of the present invention 1.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with Figure of description and embodiment to the present invention make more comprehensively, it is careful
Ground description, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1
Present embodiments provide a kind of stable perovskite photodetector, including be sequentially connected silica substrate 1,
CH3NH3PbI3Active layer 2 is blended with poly- 3- hexyl thiophene and electrode 3, the 2 upper surface two sides of blending active layer are respectively set
There is electrode 3, wherein the blending active layer 2 is with a thickness of 500nm.Poly- 3- hexyl thiophene is wrapped in calcium in the blending active layer 2
4 surface of titanium ore nano-powder, structural schematic diagram are as shown in Fig. 1.
In the present embodiment stable perovskite photodetector preparation method the following steps are included:
(1) substrate is cleaned by ultrasonic 20min using deionized water, acetone, dehydrated alcohol respectively, then uses high-purity gas
Drying, finally UV-ozone handles 20min again.
(2) by CH3NH3I:PbI2After 1:1 is weighed in molar ratio, first by CH3NH3I is dissolved in N-N dimethylformamide, so
Afterwards by CH3NH3I solution and PbI2Mixing, finally heated stirring, wherein heating temperature is 60 DEG C, and mixing time 12h is obtained
The CH of 600mg/ml3NH3PbI3Precursor solution.
(3) by CH3NH3PbI3Precursor solution: after chlorobenzene solvent 100:1 mixing by volume, shape is precipitated in perovskite crystal
At nano-powder dispersion liquid.
(4) by poly- 3- hexyl thiophene: chlorobenzene is uniformly mixed after 200:3 is weighed in mass ratio, forms concentration in 15mg/ml
Poly- 3- hexyl thiophene solution.
(5) by poly- 3- hexyl thiophene solution: perovskite nano-powder dispersion liquid presses the volume ratio of 20:2, is uniformly mixed standby
With.
(6) perovskite and poly- 3- hexyl thiophene blend film are prepared in substrate using spin coating mode, and is moved back at 120 DEG C
Fire processing 10min.
(7) electrode is prepared on active layer is blended using vapour deposition method and prepares electrode.
Through the above steps, a kind of stable perovskite photodetector, the knot of the photodetector can be prepared
Structure schematic diagram, blend film cross-sectional scans electromicroscopic photograph, X-ray diffraction spectrum, photodetector photoelectric current-voltage curve, sound
Seasonable m- photocurrent curve, stability curve are distinguished as shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 4, Fig. 5 and Fig. 6.Cross-sectional scans Electronic Speculum is shone
Piece shows that the blend film of above method preparation has fine and close continuous structure and crystallinity, can provide for photo-generated carrier
Complete transmission channel, so that the recombination rate of photo-generated carrier be effectively reduced.Photoelectric current-voltage curve and response time-photoelectricity
Flow curve shows that perovskite photodetector has outstanding photodetection performance.Stability curve shows that the air of device is steady
It is qualitative to be obviously improved compared with relevant report.After measured, in the stable perovskite photodetector blend film with a thickness of
500nm。
The stable perovskite photodetector of the present embodiment as made from the above method, to ultraviolet light, visible light with
And near infrared light all has good photoresponse, after placing 40 days in air, performance reaches target without obvious decaying.
Embodiment 2
A kind of stable perovskite photodetector is present embodiments provided, including the Al being sequentially connected2O3Potsherd substrate
1、CH3NH3PbCl3Active layer 2 and electrode 3 is blended with poly- 3- hexyl thiophene, wherein the blending active layer 2 with a thickness of
300nm.Poly- 3- hexyl thiophene is wrapped in 4 surface of perovskite nano-powder in the blending active layer 2, and structural schematic diagram is for example attached
Shown in Fig. 1.
In the present embodiment stable perovskite photodetector preparation method the following steps are included:
(1) substrate is cleaned by ultrasonic 20min using deionized water, acetone, dehydrated alcohol respectively, then uses high-purity gas
Drying, finally UV-ozone handles 20min again.
(2) by CH3NH3Cl:PbCl2After 1:1 is weighed in molar ratio, first by CH3NH3Cl is dissolved in N-N dimethylformamide,
Then by CH3NH3Cl solution and PbCl2Mixing, finally heated stirring, wherein heating temperature is 60 DEG C, and mixing time 12h is obtained
To the CH of 400mg/ml3NH3PbCl3Precursor solution.
(3) by CH3NH3PbCl3Precursor solution: after the 100:5 mixing by volume of o-dichlorohenzene solvent, perovskite crystal
Precipitation forms nano-powder dispersion liquid.
(4) by poly- 3- hexyl thiophene: chlorobenzene is uniformly mixed after 200:1 is weighed in mass ratio, forms concentration 5mg/ml's
Poly- 3- hexyl thiophene solution.
(5) by poly- 3- hexyl thiophene solution: perovskite nano-powder dispersion liquid presses the volume ratio of 20:1, is uniformly mixed standby
With.
(6) perovskite and poly- 3- hexyl thiophene blend film are prepared in substrate using blade coating mode, and is moved back at 80 DEG C
Fire processing 120min.
(7) electrode is prepared on active layer is blended using vapour deposition method and prepares electrode.
Through the above steps, a kind of stable perovskite photodetector as shown in Figure 1 can be prepared.Through surveying
It is fixed, the 300nm of the thickness of blend film respectively in the stable perovskite photodetector.This reality as made from the above method
The stable perovskite photodetector for applying example, all has good photoresponse to ultraviolet light, visible light and near infrared light,
After placing 20 days in air, performance reaches target without obvious decaying.
Embodiment 3
A kind of stable perovskite photodetector is present embodiments provided, including the poly terephthalic acid second being sequentially connected
Terephthalate polymer film substrate 1, CH3NH3PbBr3Active layer 2 and electrode 3 is blended with poly- 3- hexyl thiophene, wherein described total
Mixed 2 layers of activity is with a thickness of 50nm.Poly- 3- hexyl thiophene is wrapped in 4 surface of perovskite nano-powder in the blending active layer 2,
Structural schematic diagram is as shown in Fig. 1.
In the present embodiment stable perovskite photodetector preparation method the following steps are included:
(1) substrate is cleaned by ultrasonic 20min using deionized water, acetone, dehydrated alcohol respectively, then uses high-purity gas
Drying, finally UV-ozone handles 20min again.
(2) by CH3NH3Br:PbBr2After 1:1 is weighed in molar ratio, first by CH3NH3Br is dissolved in N-N dimethylformamide,
Then by CH3NH3Br solution and PbBr2Mixing, finally heated stirring, wherein heating temperature is 60 DEG C, and mixing time 12h is obtained
To the CH of 300mg/ml3NH3PbBr3Precursor solution.
(3) by CH3NH3PbBr3Precursor solution: after chlorobenzene solvent 100:2 mixing by volume, perovskite crystal is precipitated
Form nano-powder dispersion liquid.
(4) by poly- 3- hexyl thiophene: chlorobenzene is uniformly mixed after 200:2 is weighed in mass ratio, forms concentration in 10mg/ml
Poly- 3- hexyl thiophene solution.
(5) by poly- 3- hexyl thiophene solution: perovskite nano-powder dispersion liquid presses the volume ratio of 20:1, is uniformly mixed standby
With.
(6) perovskite and poly- 3- hexyl thiophene blend film are prepared in substrate using spin coating mode, and is moved back at 100 DEG C
Fire processing 30min.
(7) electrode is prepared on active layer is blended using vapour deposition method and prepares electrode.
Through the above steps, a kind of stable perovskite photodetector as shown in Figure 1 can be prepared.Through surveying
It is fixed, the 50nm of the thickness of blend film respectively in the stable perovskite photodetector.This reality as made from the above method
The stable perovskite photodetector for applying example, all has good photoresponse to ultraviolet light, visible light and near infrared light,
After placing 30 days in air, performance reaches target without obvious decaying.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of perovskite photodetector, including be sequentially connected substrate (1), active layer (2), electrode (3), feature is blended
Be: the blending active layer (2) is that perovskite and the blending of poly- 3- hexyl thiophene make poly- 3- hexyl thiophene be wrapped in perovskite table
Face forms, and the perovskite is perovskite nano-powder (4), and perovskite chemical formula is CH3NH3PbA3, wherein A=I, Cl or Br.
2. perovskite photodetector as described in claim 1, it is characterised in that: the blending active layer thickness be 50~
500nm。
3. perovskite photodetector as claimed in claim 2, it is characterised in that: the substrate is silica, potsherd
Or thin polymer film.
4. the preparation method of perovskite photodetector described in any one of claims 1 to 3 claim, it is characterised in that: step
Suddenly include:
S1, it is handled by substrate cleaning, drying, with UV-ozone；
S2, perovskite precursor solution is prepared, then crystallizes to form perovskite nano-powder dispersion liquid by solvent-induced method；
S3, poly- 3- hexyl thiophene solution is prepared；
S4, the blend solution for preparing perovskite and poly- 3- hexyl thiophene；
S5, perovskite and poly- 3- hexyl thiophene blend film, thermal anneal process are prepared in substrate using spin coating or blade coating mode
After obtain be blended active layer；
S6, electrode is prepared on active layer is blended using vapour deposition method.
5. the preparation method of perovskite photodetector as claimed in claim 4, it is characterised in that: in step S2, the calcium
Titanium ore precursor solution preparation steps include: by CH3NH3A:PbA2After 1:1 is weighed in molar ratio, it is dissolved in N-N dimethylformamide
In, concentration is formed in the perovskite precursor solution of 300mg/ml~600mg/ml.
6. the preparation method of perovskite photodetector as claimed in claim 4, it is characterised in that: described logical in step S2
Cross solvent-induced method and crystallize the step of forming perovskite nano-powder dispersion liquid and include: by perovskite precursor solution: solvent is pressed
After volume ratio 100:1~5 is mixed, perovskite crystal is precipitated to form perovskite nano-powder dispersion liquid, and the solvent is chlorobenzene, neighbour
One or more of dichloro-benzenes.
7. the preparation method of perovskite photodetector as claimed in claim 4, it is characterised in that: described poly- in step S3
3- hexyl thiophene solution preparation steps include: by poly- 3- hexyl thiophene: chlorobenzene 200:1~3 in mass ratio mix after weighing, and are formed
Poly- 3- hexyl thiophene solution of the concentration in 5mg/ml~15mg/ml.
8. the preparation method of perovskite photodetector as claimed in claim 4, it is characterised in that: in step S4, the calcium
The blend solution preparation steps of titanium ore and poly- 3- hexyl thiophene include: by poly- 3- hexyl thiophene solution: perovskite nano-powder point
Dispersion liquid presses the volume ratio of 20:1~2, is uniformly mixed.
9. the preparation method of perovskite photodetector as claimed in claim 4, it is characterised in that: in step S5, the heat
Annealing is 10~120min of annealing at 80~120 DEG C.
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| CN111463350A (en) * | 2020-04-20 | 2020-07-28 | 浙江大学 | X-ray detector based on perovskite quantum dots and preparation method thereof |
| CN113823742A (en) * | 2021-08-05 | 2021-12-21 | 中国科学院深圳先进技术研究院 | perovskite-based X-ray detector with p-i-n structure and preparation method thereof |
| CN113823740A (en) * | 2021-08-05 | 2021-12-21 | 中国科学院深圳先进技术研究院 | Perovskite-based X-ray detector with n-i structure and preparation method thereof |
| CN113823741A (en) * | 2021-08-05 | 2021-12-21 | 中国科学院深圳先进技术研究院 | X-ray active material and preparation method and application thereof |
| CN113659090B (en) * | 2021-08-19 | 2023-10-31 | 广东省科学院半导体研究所 | Preparation method of modified perovskite quantum dot and preparation method of electroluminescent device |
| CN117186462B (en) * | 2023-11-08 | 2024-02-02 | 华中科技大学 | Polymer-based flexible film with oriented bridging structure, preparation and application |
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