CN107342365A - 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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- CN107342365A CN107342365A CN201710495524.6A CN201710495524A CN107342365A CN 107342365 A CN107342365 A CN 107342365A CN 201710495524 A CN201710495524 A CN 201710495524A CN 107342365 A CN107342365 A CN 107342365A
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- H—ELECTRICITY
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- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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- H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
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Abstract
The invention provides a kind of perovskite photodetector of stabilization, the substrate (1) that is sequentially connected, blending active layer (2), electrode (3), the blending active layer (2) is perovskite and the blending of poly- 3 hexyl thiophene makes poly- 3 hexyl thiophene be wrapped in perovskite surface to form.Further the invention provides the preparation method of photodetector, comprise 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 blending active layer is obtained after thermal anneal process；Electrode is prepared using vapour deposition method.The product of the present invention has that the response time is short, stable, low cost and other advantages in air.
Description
Technical field
The present invention relates to photoelectric device technical field, and in particular to a kind of perovskite photodetector of stabilization and its preparation
Method.
Background technology
Photodetector can effectively detect optical signal, measurement intensity of illumination, and the optical signal of time correlation is turned
Change electric signal into.Therefore, it has extensive in fields such as bio-sensing, optical imagery, optic communication, environmental monitoring, defence and militaries
Application.The semi-conducting material such as past decades, silicon, molybdenum disulfide, indium gallium arsenic, zinc oxide, cadmium sulfide is 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 of increased attention.There is suitable energy gap, high absorption just because of perovskite material
The electron hole pair diffusion length and carrier lifetime of coefficient, length, 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
First Application achieves 3.81% photoelectric transformation efficiency in solar cell.Through research and development in a few years, current
The photoelectric transformation efficiency of perovskite solar cell is more than 20%.
It is well known that perovskite material is very sensitive to hydrone, and when exposing in atmosphere, 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, it is to improve perovskite photoelectric device service life and promote perovskite photodetector practical
Key, also become the key technology of development perovskite material practical application.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, there is provided one
The perovskite photodetector of stable performance in kind photodetection excellent performance, air, correspondingly provide a kind of technical process letter
The preparation method of the perovskite photodetector of the low foregoing stabilization of list, good product performance, 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 thiophenes make poly- 3- hexyl thiophenes 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 present invention proposes one kind with perovskite and poly- 3- hexyl thiophenes
Bulk-heterojunction structure of the blend film as active layer, it is based particularly on following thinking and research experience：Perovskite material is
Emerging light absorbing material, it absorbs preferable optical absorption characteristics in ultraviolet, visible ray, near infrared region, disclosure satisfy that light
The requirement that electrical resistivity survey is surveyed.But the photoelectric detector of simple perovskite thin film can not meet the requirement of atmospheric environment, calcium
Titanium ore material can decompose with the water molecule reaction in air, so as to cause photoelectric properties to fail.Poly- 3- hexyl thiophenes (P3HT)
Be it is a kind of have prepare simple, cost is low, can low temperature preparation outstanding organic semiconducting materials, poly- 3- hexyl thiophenes have excellent
Air stability, water in air and oxygen diffusion can be prevented, so as to realize the protection to perovskite material.It is in addition, poly-
3- hexyl thiophenes have extraordinary air stability and high hole mobility, and bulk-heterojunction structure is realized by blending, by
Matched in the interface energy level of two class materials, so as to reach the purpose of light absorbs enhancing.By our research repeatedly, poly- 3- hexyls
Thiophene is wrapped in perovskite nano powder surface, it is possible to achieve the separation of photo-generate electron-hole pair, reduces answering for electron hole pair
Close, so as to improve the performance of photodetector, finally provide 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, substrate cleaned, dries up, handled with UV-ozone；
S2, perovskite precursor solution is prepared, then crystallize to form perovskite nano-powder and disperse by solvent-induced method
Liquid；
S3, prepare poly- 3- hexyl thiophenes solution；
S4, the blend solution for preparing perovskite and poly- 3- hexyl thiophenes；
S5, using spin coating or blade coating mode perovskite and poly- 3- hexyl thiophenes blend film, thermal annealing are prepared in substrate
Obtain that active layer is blended after processing；
S6, using vapour deposition method blending active layer on prepare electrode.
Specifically, in step S1, the cleaning of substrate, drying, handled with UV-ozone refer to by substrate using deionized water,
Acetone, absolute ethyl 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 are cleaned by ultrasonic, 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, infiltration of the blend solution in substrate surface can be improved
Property, be advantageous to be blended the formation of active layer.
Preferably, in step S2, the perovskite precursor solution preparation steps include：By CH3NH3A:PbA2By mole
Than 1:After 1 weighs, it is dissolved in N-N dimethylformamides, forms perovskite presoma of the concentration in 300mg/ml~600mg/ml
Solution, the heating stirring 12h at a temperature of 60 DEG C.Using said ratio, and by the means such as heating, stirring, material can be filled
Divide and dissolve each other, to ensure the proportioning of each component in film seat preparation process, film is fully reacted in subsequent anneal link,
Reduce the PbI of remaining2、PbCl2Or PbBr2Material.
Preferably, it is described that the step of forming perovskite nano-powder dispersion liquid is crystallized by solvent-induced method in step S2
Including：By perovskite precursor solution：Solvent by volume 100：After 1~5 mixing, perovskite crystal, which separates out, to be formed perovskite and receives
Ground rice dispersion liquid, the solvent are the one or more in chlorobenzene, o-dichlorohenzene.By solvent engineering philosophy, from chlorobenzene
Or the anti-solvent of o-dichlorohenzene this perovskite-like material, perovskite crystal can be made quickly to be separated out in chlorobenzene or o-dichlorohenzene,
So as to obtain perovskite nano-powder dispersion liquid.
Preferably, in step S3, the poly- 3- hexyl thiophenes solution preparation steps include：By poly- 3- hexyl thiophenes：Chlorobenzene
In mass ratio 200：1~3 weigh after mix, formed concentration 5mg/ml~15mg/ml poly- 3- hexyl thiophenes solution.
Preferably, in step S4, the blend solution preparation steps of the perovskite and poly- 3- hexyl thiophenes include：By poly- 3-
Hexyl thiophene solution：Perovskite nano-powder dispersion liquid presses 20：1~2 volume ratio, it is well mixed.Due to poly- 3- hexyl thiophenes
Solution and perovskite nano-powder dispersion liquid are benzene kind solvent, during two class materials dissolve each other and to form blend solution, energy
Enough it is sufficiently mixed, in follow-up film forming, is more easy 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, it can ensure that perovskite fully reacts, form the crystalline membrane of high quality.
The beneficial effects of the invention are as follows：
1. the perovskite photodetector of the stabilization of the present invention is designed using bulk-heterojunction structure, composite work(make use of
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 thiophenes.Calcium
Titanium ore material has outstanding photoelectric characteristic, for example suitable direct band gap width, less excite combine energy, wider absorption
Bandwidth, longer exciton diffusion length and carrier lifetime.The poly- 3- hexyl thiophenes organic material of the present invention has extraordinary
Air stability, the bulk-heterojunction structure of formation, poly- 3- hexyl thiophenes parcel perovskite nano-powder, the protective layer of formation can be made
Add the air life-span of perovskite material；In addition, poly- 3- hexyl thiophenes organic material has high exciton mobility, make photoproduction
Carrier forms stable perovskite photodetector by the network transmission that poly- 3- hexyl thiophenes are formed 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 invention provides a kind of perovskite photodetector of stabilization, the photodetector finally obtained
With the distinguishing feature that air stability is good, cost is low, the optical detection of simple perovskite thin film photodetector is substantially improved
Performance and used life, it is practical significant to improving perovskite-based photodetector.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are the present invention
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
These accompanying drawings obtain other accompanying 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 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.
Embodiment
For the ease of understanding the present invention, the present invention is made below in conjunction with Figure of description and embodiment more comprehensively, it is careful
Ground describes, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical terms used hereinafter are generally understood that with those skilled in the art
It is identical.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to the limitation present invention
Protection domain.
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 perovskite photodetector of stabilization, including be sequentially connected silica substrate 1,
CH3NH3PbI3Active layer 2 and electrode 3 is blended with poly- 3- hexyl thiophenes, the blending active layer 2 upper surface both sides are set respectively
There is electrode 3, wherein the blending thickness of active layer 2 is 500nm.Poly- 3- hexyl thiophenes are wrapped in calcium in the blending active layer 2
The surface of titanium ore nano-powder 4, its structural representation is as shown in Figure 1.
The preparation method of stable perovskite photodetector comprises the following steps in the present embodiment：
(1) substrate is cleaned by ultrasonic 20min respectively using deionized water, acetone, absolute ethyl alcohol, then using high-purity gas
Drying, finally UV-ozone handles 20min again.
(2) by CH3NH3I:PbI2In molar ratio 1:After 1 weighs, first by CH3NH3I is dissolved in N-N dimethylformamides, so
Afterwards by CH3NH3I solution and PbI2Mixing, wherein finally heated stirring, heating-up temperature are 60 DEG C, mixing time 12h, are obtained
600mg/ml CH3NH3PbI3Precursor solution.
(3) by CH3NH3PbI3Precursor solution：Chlorobenzene solvent by volume 100：After 1 mixing, perovskite crystal separates out shape
Into nano-powder dispersion liquid.
(4) by poly- 3- hexyl thiophenes：Chlorobenzene in mass ratio 200：After 3 weigh, it is well mixed, forms concentration in 15mg/ml
Poly- 3- hexyl thiophenes solution.
(5) by poly- 3- hexyl thiophenes solution：Perovskite nano-powder dispersion liquid presses 20：2 volume ratio, it is well mixed standby
With.
(6) perovskite and poly- 3- hexyl thiophenes blend film are prepared in substrate using spin coating mode, and moved back at 120 DEG C
Fire processing 10min.
(7) electrode is prepared on blending active layer using vapour deposition method and prepares electrode.
Pass through above-mentioned steps, you can a kind of perovskite photodetector of stabilization, the knot of the photodetector is prepared
Structure schematic diagram, blend film cross-sectional scans electromicroscopic photograph, X-ray diffraction spectrum, photoelectric current-voltage curve, the sound of photodetector
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 blend film prepared by the above method has fine and close continuous structure and crystallinity, can be provided for photo-generated carrier
Complete transmission channel, so as to effectively reduce the recombination rate of photo-generated carrier.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, the thickness of blend film is in the perovskite photodetector of the stabilization
500nm。
By the perovskite photodetector of the stabilization of the present embodiment made from the above method, to ultraviolet light, visible ray with
And near infrared light is respectively provided with good photoresponse, after placing 40 days in atmosphere, performance reaches target without obvious decay.
Embodiment 2
Present embodiments provide a kind of perovskite photodetector of stabilization, including the Al being sequentially connected2O3Potsherd substrate
1、CH3NH3PbCl3Active layer 2 and electrode 3 is blended with poly- 3- hexyl thiophenes, wherein the blending thickness of active layer 2 is
300nm.Poly- 3- hexyl thiophenes are wrapped in the surface of perovskite nano-powder 4 in the blending active layer 2, and its structural representation is for example attached
Shown in Fig. 1.
The preparation method of stable perovskite photodetector comprises the following steps in the present embodiment：
(1) substrate is cleaned by ultrasonic 20min respectively using deionized water, acetone, absolute ethyl alcohol, then using high-purity gas
Drying, finally UV-ozone handles 20min again.
(2) by CH3NH3Cl:PbCl2In molar ratio 1:After 1 weighs, first by CH3NH3Cl is dissolved in N-N dimethylformamides,
Then by CH3NH3Cl solution and PbCl2Mixing, wherein finally heated stirring, heating-up temperature are 60 DEG C, mixing time 12h, are obtained
To 400mg/ml CH3NH3PbCl3Precursor solution.
(3) by CH3NH3PbCl3Precursor solution：O-dichlorohenzene solvent by volume 100：After 5 mixing, perovskite crystal
Precipitation forms nano-powder dispersion liquid.
(4) by poly- 3- hexyl thiophenes：Chlorobenzene in mass ratio 200：After 1 weighs, it is well mixed, forms concentration 5mg/ml's
Poly- 3- hexyl thiophenes solution.
(5) by poly- 3- hexyl thiophenes solution：Perovskite nano-powder dispersion liquid presses 20：1 volume ratio, it is well mixed standby
With.
(6) perovskite and poly- 3- hexyl thiophenes blend film are prepared in substrate using blade coating mode, and moved back at 80 DEG C
Fire processing 120min.
(7) electrode is prepared on blending active layer using vapour deposition method and prepares electrode.
Pass through above-mentioned steps, you can a kind of perovskite photodetector of stabilization as shown in Figure 1 is prepared.Through surveying
It is fixed, the 300nm of the thickness of blend film respectively in the stable perovskite photodetector.Pass through this reality made from the above method
The perovskite photodetector of the stabilization of example is applied, good photoresponse is respectively provided with to ultraviolet light, visible ray and near infrared light,
After being placed 20 days in air, performance reaches target without obvious decay.
Embodiment 3
A kind of perovskite photodetector of stabilization 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 thiophenes, wherein described common
2 thickness degree of mixed activity are 50nm.Poly- 3- hexyl thiophenes are wrapped in the surface of perovskite nano-powder 4 in the blending active layer 2, its
Structural representation is as shown in Figure 1.
The preparation method of stable perovskite photodetector comprises the following steps in the present embodiment：
(1) substrate is cleaned by ultrasonic 20min respectively using deionized water, acetone, absolute ethyl alcohol, then using high-purity gas
Drying, finally UV-ozone handles 20min again.
(2) by CH3NH3Br：PbBr2In molar ratio 1:After 1 weighs, first by CH3NH3Br is dissolved in N-N dimethylformamides,
Then by CH3NH3Br solution and PbBr2Mixing, wherein finally heated stirring, heating-up temperature are 60 DEG C, mixing time 12h, are obtained
To 300mg/ml CH3NH3PbBr3Precursor solution.
(3) by CH3NH3PbBr3Precursor solution：Chlorobenzene solvent by volume 100：After 2 mixing, perovskite crystal separates out
Form nano-powder dispersion liquid.
(4) by poly- 3- hexyl thiophenes：Chlorobenzene in mass ratio 200：After 2 weigh, it is well mixed, forms concentration in 10mg/ml
Poly- 3- hexyl thiophenes solution.
(5) by poly- 3- hexyl thiophenes solution：Perovskite nano-powder dispersion liquid presses 20：1 volume ratio, it is well mixed standby
With.
(6) perovskite and poly- 3- hexyl thiophenes blend film are prepared in substrate using spin coating mode, and moved back at 100 DEG C
Fire processing 30min.
(7) electrode is prepared on blending active layer using vapour deposition method and prepares electrode.
Pass through above-mentioned steps, you can a kind of perovskite photodetector of stabilization as shown in Figure 1 is prepared.Through surveying
It is fixed, the 50nm of the thickness of blend film respectively in the stable perovskite photodetector.Pass through this reality made from the above method
The perovskite photodetector of the stabilization of example is applied, good photoresponse is respectively provided with to ultraviolet light, visible ray and near infrared light,
After being placed 30 days in air, performance reaches target without obvious decay.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (9)
1. a kind of perovskite photodetector, including be sequentially connected substrate (1), blending active layer (2), electrode (3), its feature
It is：The blending active layer (2) is that perovskite and the blending of poly- 3- hexyl thiophenes make poly- 3- hexyl thiophenes 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 claimed in claim 1, it is characterised in that：It is described 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, substrate cleaned, dries up, handled with UV-ozone；
S2, perovskite precursor solution is prepared, then crystallize to form perovskite nano-powder dispersion liquid by solvent-induced method；
S3, prepare poly- 3- hexyl thiophenes solution；
S4, the blend solution for preparing perovskite and poly- 3- hexyl thiophenes；
S5, using spin coating or blade coating mode perovskite and poly- 3- hexyl thiophenes blend film, thermal anneal process are prepared in substrate
After obtain be blended active layer；
S6, using vapour deposition method blending active layer on prepare electrode.
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:PbA2In molar ratio 1:After 1 weighs, N-N dimethylformamides are dissolved in
In, form perovskite precursor solution of the concentration in 300mg/ml~600mg/ml.
6. the preparation method of perovskite photodetector as claimed in claim 4, it is characterised in that：It is described logical in step S2
Crossing solvent-induced method and crystallizing the step of forming perovskite nano-powder dispersion liquid includes：By perovskite precursor solution：Solvent is pressed
Volume ratio 100：After 1~5 mixing, perovskite crystal separates out to form perovskite nano-powder dispersion liquid, and the solvent is chlorobenzene, neighbour
One or more in dichloro-benzenes.
7. the preparation method of perovskite photodetector as claimed in claim 4, it is characterised in that：It is described poly- in step S3
3- hexyl thiophene solution preparation steps include：By poly- 3- hexyl thiophenes：Chlorobenzene in mass ratio 200：1~3 weigh after mix, 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 thiophenes include：By poly- 3- hexyl thiophenes solution：Perovskite nano-powder point
Dispersion liquid presses 20：1~2 volume ratio, it is well 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 |
| CN113659090A (en) * | 2021-08-19 | 2021-11-16 | 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 |
| 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 |
| 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 |
| CN117186462A (en) * | 2023-11-08 | 2023-12-08 | 华中科技大学 | Polymer-based flexible film with oriented bridging structure, preparation and application |
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| 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 |
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