CN110212094A - A kind of preparation method of the flexible photoelectric device of novel perovskite material - Google Patents
A kind of preparation method of the flexible photoelectric device of novel perovskite material Download PDFInfo
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- CN110212094A CN110212094A CN201910388350.2A CN201910388350A CN110212094A CN 110212094 A CN110212094 A CN 110212094A CN 201910388350 A CN201910388350 A CN 201910388350A CN 110212094 A CN110212094 A CN 110212094A
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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
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- 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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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
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Abstract
The invention belongs to material devices preparation technical field, in particular to a kind of preparation method of the flexible photoelectric device of novel perovskite material.The present invention uses fiber to prepare novel perovskite material as the method for template using organic inorganic hybridization lead halogen perovskite material as light active material, and is packaged into flexible optoelectronic sensitive detection parts.This method is easy to operate, environmentally protective, and this method is suitable for the preparation of size adjustable photoelectric device, provides new method for the preparation of large area industrialization device and has further pushed perovskite material in the application in flexible wearable field.
Description
Technical field
The invention belongs to material devices preparation technical field, in particular to a kind of flexible light electric appliance of novel perovskite material
The preparation method of part.
Background technique
With the fast development of science and technology and to the growing demand of the energy, flexible wearable photodetector device draws
The fervent concern of people is played.Photodetector is including image sensing, optic communication, fire detection, biomedical imaging, environment
Many scientific researches such as monitoring, space exploration and safety detection and industrial technical field have highly important application.In recent years,
Hybrid inorganic-organic perovskite material based on lead halogen becomes the photodetector of production hypersensitivity and quick response
One of ideal material.
Currently, the building of lead halogen perovskite flexible photoelectric device predominantly use flexible substrate such as PET, PEN, carbon cloth,
Metal substrate etc. grows perovskite material on its surface using spin coating method.The pattern of common perovskite material includes: plycrystalline diamond
Film, micron be rodlike, nanometer rods, nanometer sheet, quantum dot etc., wherein has research to confirm that bar perovskite material has direct
The material that carrier transport channel is thus compared to other patterns has superior photoelectric characteristic.More commonly used perovskite material
The preparation method of material has spin-coating method, and sample prepared by this method is mainly plycrystalline diamond film, such as the prior art
CN107591481A.Saturation degree by controlling solution can prepare perovskite material crystal, or be combined to method using oil
Perovskite quantum dot can be prepared, but material surface prepared by this method has organic ligand, influences carrier transport
Therefore prepared photoelectric detector performance is undesirable for performance, such as prior art CN106252520A.Also, for soft
Inevitably there is stress in use for property device, be previously mentioned the perovskite material of pattern by
The decaying of material property is concentrated in a little and then caused when stress, while perovskite material itself has more crisp lack
It falls into, these factors greatly hinder its application in flexible optoelectronic part.
Therefore, seek a kind of method and prepare photoelectric detector flexible to it in flexible wearable optoelectronic areas
Using with great meaning.
Summary of the invention
In view of the problems existing in the prior art, the present invention provides a kind of flexible photoelectric devices of novel perovskite material
Preparation method, this method is easy to operate, favorable repeatability, and flexible device size, pattern prepared by this method are controllable, are
Its large-scale industrialized production is pushed to provide new thinking.
The present invention is achieved through the following technical solutions, a kind of preparation side of the flexible photoelectric device of novel perovskite material
Method, comprising:
Using organic inorganic hybridization lead halogen perovskite material powder as light active material, use fiber as growth mould
Plate prepares novel perovskite material, and uses metal wire as electrode, is packaged into flexible optoelectronic sensitive detection parts.
More specifically, aforementioned preparation process specific experiment step includes:
(1) firstly, using fiber as template, fibrous template is the flexible material that can be woven, and can be woven into arbitrary shape
Shape；
(2) fibrous template is immersed in perovskite precursor liquid, due to modes such as capillarities, fiber can be filled calcium titanium
Mine precursor solution；
(3) fibrous template for being filled perovskite precursor liquid obtained in step (2) is heat-treated, i.e., in a template
It is in situ that perovskite crystal is precipitated, novel perovskite material is obtained, and use metal wire as electrode to get to being packaged into flexible light
Electric explorer part.
The selection gist and realization principle of aforementioned schemes are: the capillarity based on selected template, by utilizing solution
Surface tension, the equably absorption of precursor liquid in a template may be implemented, to prepare the perovskite material of even compact.
It is compared to the synthetic method of other perovskite materials, this method is easy to operate, morphology controllable, the system suitable for large scale material
It is standby.
One of preferred embodiment is that fibrous template can have flexible material for any threadiness in step (1), including but not
It is limited to: carbon cloth, cotton thread, polymer fiber, metallic fiber beam etc.；Fibrous template can not be arbitrary shape, arbitrary dimension, including but not
It is limited to: linear type, spring shape, bending pattern, netted pattern etc., since fibrous template has flexible and can be woven into any
Shape is to realize the morphology controllable of perovskite material.
Preferred material is cotton thread, proves that the material has perovskite precursor liquid selected in experiment by Experimental comparison
Better suction-operated.Preferable shape is class spring-like structures, since this structure can play absorption and the dispersion work of stress
With, and then improve the deformation upper limit of material.
One of preferred embodiment is that perovskite Concentration of precursor solution is 0.01mM-10mM, perovskite material in step (2)
APbX3, wherein A is organic cation CH3NH3 +、MA+、NH2CHNH2 +、FA+、Cs+One of or it is several mixed with arbitrary proportion
It closes, X is halide anion I-、Br-、Cl-One of or it is several mixed with arbitrary proportion, be further specifically preferably selected from
MAPbI3、MAPbBr3、MAPbCl3、FAPbI3、FAPbBr3、FAPbCl3、CsPbI3、 CsPbBr3、CsPbCl3；Precursor liquid it is molten
Agent includes but is not limited to: n,N-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), toluene, chlorobenzene, butyrolactone, isopropyl
Alcohol etc..Perovskite component chooses organic inorganic hybridization perovskite material, including but not limited to: or mixed-cation, mixed halogen
The perovskite material of ion.
Preferred solvent is n,N-Dimethylformamide (DMF), and perovskite material Concentration of precursor solution is 1mM, perovskite material
Choose MAPbI3.It was proved that sample even compact prepared by under this condition, crystal connectivity is good, more conducively the biography of electronics
It is defeated.Perovskite material is selected to choose MAPbI3It is since the ABSORPTION EDGE of the material is in 800nm or so, is all perovskite materials
The middle longer wavelengths of material of photoresponse, the more conducively utilization of light.
One of preferred embodiment is that heat treatment process heating temperature is -150 DEG C of room temperature in step (3), or can arbitrarily be volatilized
The temperature of perovskite precursor liquid solvent；Heat-treatment temperature range is room temperature to 150 DEG C.
Wherein, the excessively high perovskite material that will lead to of temperature is decomposed.Heat treatment time is 10min to 5h.Time is too short
It will lead to dissolvent residual, overlong time will lead to the reduction of perovskite material crystal quality.
Preferable temperature is 100 DEG C, heating time 3h, and solvent volatilization is thorough under this condition, conducive to the analysis of perovskite crystal
Out.
One of preferred embodiment be as electrode metal wire can be the arbitrary dimensions such as gold, silver, copper metal wire.
It is preferred that metal wire is silver metal line, silver has more preferably anticorrosion effect, more conducively electrode to selected solvent
Locate the collection of electronics.
More specifically optimal technical scheme is that the method carries out at room temperature in glove box, uses MAPbI3Material
As light active material, steps are as follows for specific experiment:
(1) firstly, using cotton thread fiber as template, fibrous template is the flexible material that can be woven, and is woven into class spring
Shape network, and upper metal silver wire is woven in the fibre as electrode；
(2) cotton thread fibrous template is immersed in (MAPbI in perovskite precursor liquid3Concentration of precursor solution is 1mM, and solvent is
DMF), due to capillarity, fiber can be filled perovskite precursor solution；
(3) fibrous template for being filled perovskite precursor liquid obtained in step (2) is subjected to 100 DEG C of heat treatment, 3 is small
When, perovskite crystal is precipitated in template hole Central Plains position.Perovskite flexible optoelectronic sensitive detection parts are obtained.
Through a large number of experiments the study found that using this scheme, it is compared to perovskite material prepared by conventional method,
This method prepares the good perovskite material of morphology controllable, even compact, crystal connectivity for the first time.Meanwhile being compared to other
The flexible perovskite device of pattern, device photoresponse rate prepared by this method is fast, and performance is stablized, and mechanical tenacity is good.
Another object of the present invention is to provide a kind of flexible photoelectric device of novel perovskite material, the flexible optoelectronics
Device is prepared by preparation method above-mentioned.
For flexible optoelectronic sensitive detection parts, photoelectric current VA characteristic curve, dark current VA characteristic curve, open the light ratio
(photoelectric current/dark current ratio), photoelectric current rise time (tr), photoelectric current fall time (td) it is that the device performance is critically important
Assessment parameter, photoelectric current is higher, and dark current is lower, and on-off ratio is bigger, and the luminous sensitivity for illustrating device is higher.Photoelectric current rises
Time and fall time are smaller, illustrate that device photoresponse rate is faster.It is curved under equal angular meanwhile for flexible device
Whether roll over performance after different circle numbers to decay is to characterize device mechanical tenacity and the critically important parameter of stability.
Compared with the prior art, the beneficial effects of the invention include:
(1) this method is easy to operate, and this method is suitable for the preparation of size adjustable photoelectric device, is large area industrialization device
Part preparation provides new method.
(2) simultaneously, this method can regulate and control the pattern of perovskite material by adjusting template shape, to realize different dimensions
, the perovskite light-detecting device of lead halogen compound of different shapes possibility is provided.
(3) the perovskite flexible optoelectronic that the present invention can be woven using large-sized, the morphology controllable that this method is prepared
Device is technically to break through compared with the existing technology.
Detailed description of the invention
Fig. 1 is used experimental method schematic diagram.
Fig. 2 is the SEM picture using the perovskite material on the preparation-obtained single fiber beam of this method.
Fig. 3 is to use the preparation-obtained perovskite material being woven on class spring like mesh fibers beam of this method
SEM picture.
Fig. 4 is to be characterized using photoelectric properties under the different biass of the preparation-obtained flexible optoelectronic detector of this method.
Fig. 5 is to be characterized using the transient state photoresponse stability of the preparation-obtained flexible optoelectronic detector of this method.
Fig. 6 is to be characterized using the photoelectric respone rate capability of the preparation-obtained flexible optoelectronic detector of this method.
Fig. 7 passes through different bendings (130 DEG C) from No. 2 samples prepared by conventional method for No. 1 sample prepared by the present invention
After enclosing number, the photoelectric respone contrast schematic diagram of device.
Specific embodiment
Below with reference to preferred embodiments and drawings, the present invention is described in further detail, but the embodiment invented is not
It is limited to this.
Embodiment 1
The schematic diagram shown in Fig. 1, fibrous template selects single thick 15 μm of cotton thread beam in figure, and precursor liquid is concentration 1mM's
MAI and PbI2DMF solution.Specific step is as follows:
(1) firstly, using cotton thread fiber as template；
(2) template is immersed in perovskite precursor liquid, due to capillarity, it is molten that fiber can be filled perovskite forerunner
Liquid；
(3) fibrous template for being filled perovskite precursor liquid obtained in step (1) is subjected to 100 DEG C of heat treatment, 3 is small
When, perovskite crystal is precipitated in template hole Central Plains position, obtains novel perovskite material.
Lower Fig. 2 is that the scanning electron microscope (SEM) carried out to prepared perovskite material characterizes, obtained perovskite
Crystal closely connects fasciculation, and grows along fibrous template, and crystal has good continuity and uniformity.
Also, result above confirms that we successfully grown perovskite material using template, and this method has
Universality can be used to the perovskite material for growing other different cations, different halogens.
Embodiment 2
The schematic diagram shown in Fig. 1, fibrous template selects single thick 15 μm of cotton thread beam in figure, and electrode is thick 50 μm of silver
Line, precursor liquid are the MAI and PbI of concentration 1mM2DMF solution.Specific step is as follows:
(1) firstly, fibrous template is woven into class spring like network；
(2) cotton thread fibrous template is immersed in perovskite precursor liquid, due to capillarity, fiber can be filled perovskite
Precursor solution；
(3) fibrous template for being filled perovskite precursor liquid obtained in step (2) is subjected to 100 DEG C of heat treatment, 3 is small
When, perovskite crystal is precipitated in template hole Central Plains position；And using metal silver wire as electrode, two o'clock pole is spaced about 15 mm, i.e.,
The perovskite flexible optoelectronic sensitive detection parts (being named as No. 1 sample) being packaged into.
Lower Fig. 3 is back-scattered scanning electron microscope (BE-SEM) photo of prepared sample, prepared as shown in the figure
Sample is equably grown in the gap of template, and obtained sample particle connection is fine and close, is closely linked between this particle
Conducive to photoelectronic transmission.Show that perovskite material different dimensions, the preparation of different-shape may be implemented in this method simultaneously.
Fig. 4 is photoelectric characteristic characterization of the prepared device under different biass, in 50mW cm-2Simulated solar irradiation irradiation
Under, photoelectric current is 1.5 μ A, 5V lower switch than about 500 under 5V bias.
Fig. 5 is that the transient state photoelectric respone of prepared device characterizes, the results showed that detection time does not observe in 200s
The decline of device performance.
Fig. 6 is that the photophase rate of prepared device characterizes, the results showed that the response device rate is compared with block, rising edge (tr)
Less than 20ms, failing edge (td) it is less than 20ms.Result above proves that device prepared by this method has more excellent photoelectricity special
Property.
Comparative example 1
Spin-coating method is prepared for perovskite plycrystalline diamond film (being named as No. 2 samples) on flexible PET substrate, and specific steps are such as
Under:
Choose the MAI and PbI that precursor liquid is concentration 1mM2DMF solution, choose 80 μ L solution be spin-coated on PET substrate,
Revolving speed chooses 4000r/min 30s, then in 100 DEG C of heating 3h, silver is deposited on PET and is used as electrode, two o'clock pole is spaced about
15mm。
After to (130 DEG C) circle numbers of different bendings, the photoelectric response performance of device is compared, as shown in fig. 7, using
No. 1 sample prepared by our method after 100 circle bendings performance do not decay, and keep preferable photoelectric respone
Stability.But in contrast to No. 2 samples prepared by conventional method, after 100 circle bendings device performance decaying it is serious, say
Flexible device performance prepared by we bright method is more preferable, this can be attributed to the fact that our class spring-like structures design, the knot
Structure can be well dispersed in the stress being applied on device in bending process, and then improve the deformation upper limit of device.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the flexible photoelectric device of novel perovskite material, it is characterised in that: use organic inorganic hybridization
Lead halogen perovskite material powder uses fiber to prepare novel perovskite material as growth templates as light active material, and
Use metal wire as electrode, is packaged into flexible optoelectronic sensitive detection parts.
2. preparation method according to claim 1, it is characterised in that: specific experiment step includes:
(1) firstly, using fiber as template, fibrous template is the flexible material that can be woven, and can be woven into arbitrary shape；
(2) fibrous template is immersed in perovskite precursor liquid, fiber can be filled perovskite precursor solution；
(3) fibrous template for being filled perovskite precursor liquid obtained in step (2) is heat-treated, i.e., it is in situ in a template
Perovskite crystal is precipitated, obtains novel perovskite material, and use metal wire as electrode, is packaged into flexible optoelectronic detector
Part.
3. preparation method according to claim 2, it is characterised in that: can there is soft fibrous template for any threadiness in step (1)
The material of toughness, including but not limited to: carbon cloth, cotton thread, polymer fiber, metallic fiber beam etc..
4. preparation method according to claim 2, it is characterised in that: fibrous template can be arbitrary shape, any ruler in step (1)
It is very little, including but not limited to: linear type, spring shape, bending pattern, netted pattern etc., due to fibrous template have it is flexible and
Arbitrary shape can be woven into realize the morphology controllable of perovskite material.
5. preparation method according to claim 2, it is characterised in that: perovskite material APbX in step (2)3, wherein A is organic
Cationic CH3NH3 +、MA+、NH2CHNH2 +、FA+、Cs+One of or it is several mixed with arbitrary proportion, X is halide anion
I-、Br-、Cl-One of or several mixed with arbitrary proportion；The solvent of precursor liquid includes but is not limited to: N, N- dimethyl methyl
Amide (DMF), dimethyl sulfoxide (DMSO), toluene, chlorobenzene, butyrolactone, isopropanol etc..
6. preparation method according to claim 5, it is characterised in that: perovskite Concentration of precursor solution is 0.01mM-10mM.
7. preparation method according to claim 5, it is characterised in that: perovskite material is selected from MAPbI3、MAPbBr3、MAPbCl3、
FAPbI3、FAPbBr3、FAPbCl3、CsPbI3、CsPbBr3、CsPbCl3。
8. preparation method according to claim 2, it is characterised in that: heat treatment process heating temperature is room temperature-in step (3)
150 DEG C, or the temperature for the perovskite precursor liquid solvent that can arbitrarily volatilize；Heat treatment time is 10min to 5h.
9. preparation method according to claim 1, it is characterised in that: the metal wire as electrode can be any for gold, silver, copper etc.
The metal wire of size.
10. a kind of flexible photoelectric device of novel perovskite material, it is characterised in that: by described in claim any one of 1-9
Preparation method be prepared.
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Cited By (3)
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| CN111058085A (en) * | 2020-01-17 | 2020-04-24 | 合肥工业大学 | Growing method of perovskite single crystal |
| CN111117613A (en) * | 2019-12-17 | 2020-05-08 | 深圳先进技术研究院 | Basalt fiber-based photoelectric material and preparation method thereof |
| CN117529192A (en) * | 2024-01-03 | 2024-02-06 | 浙江省白马湖实验室有限公司 | Manufacturing device and process of light absorption layer in perovskite solar cell |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111117613A (en) * | 2019-12-17 | 2020-05-08 | 深圳先进技术研究院 | Basalt fiber-based photoelectric material and preparation method thereof |
| WO2021121298A1 (en) * | 2019-12-17 | 2021-06-24 | 深圳先进技术研究院 | Basalt fiber-based photoelectric material and preparation method therefor |
| CN111117613B (en) * | 2019-12-17 | 2021-07-30 | 深圳先进技术研究院 | Basalt fiber-based photoelectric material and preparation method thereof |
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| CN111058085B (en) * | 2020-01-17 | 2021-06-25 | 合肥工业大学 | Growing method of perovskite single crystal |
| CN117529192A (en) * | 2024-01-03 | 2024-02-06 | 浙江省白马湖实验室有限公司 | Manufacturing device and process of light absorption layer in perovskite solar cell |
| CN117529192B (en) * | 2024-01-03 | 2024-04-16 | 浙江省白马湖实验室有限公司 | Manufacturing device and process of light absorption layer in perovskite solar cell |
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