CN107221612A - A kind of preparation method of full-inorganic perovskite thin film - Google Patents
A kind of preparation method of full-inorganic perovskite thin film Download PDFInfo
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- CN107221612A CN107221612A CN201710450803.0A CN201710450803A CN107221612A CN 107221612 A CN107221612 A CN 107221612A CN 201710450803 A CN201710450803 A CN 201710450803A CN 107221612 A CN107221612 A CN 107221612A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- 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
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract
The invention provides a kind of preparation method of full-inorganic perovskite thin film, comprise the following steps：(1) temperature control technique is used, at a certain temperature, by PbX2It is dissolved into CsX (X=Br, Cl, I) powder in organic solvent, obtains mixed solution；(2) above-mentioned mixed solution is spun on substrate；(3) the good substrate of spin coating is stood and obtains full-inorganic perovskite thin film for a period of time.Wherein step (3) takes the unnecessary organic solvent of film surface away using vacuum pumping method, the method is more simple and easy to operate compared with conventional anneal film drying method, and the perovskite thin film coverage rate obtained is bigger (close to 100%), particle is smaller, the more excellent benefit of performance of electroluminescent device.The method of the invention technology is simple, and cost is low, is conducive to promoting the large-scale production of full-inorganic perovskite electroluminescent device.
Description
Technical field
The present invention relates to technical field of film preparation, and in particular to a kind of preparation method of full-inorganic perovskite thin film.
Background technology
2014, Friend research groups proposed synthesis halide perovskite light emitting diode, calcium at room temperature for the first time
Titanium ore material causes the extensive concern of each research group of the world as luminescent layer.According to the research of Friend groups, it was demonstrated that
Full-inorganic caesium lead halide perovskite has more preferable heat endurance compared with organic perovskite.It moreover has been found that CsPbBr3Can
To provide high charge carrier mobilityLow trap density and high fluorescence quantum yield are (molten
In liquid up to 90%), and at room temperature spectrum have very high excitation (half-peak breadth, FWHM,)。CsPbBr3
These calorifics, electrical and optical properties be favourable to perovskite light emitting diode.
Full-inorganic perovskite light emitting diode realizes that one of key factor of high electroluminescent (EL) performance is that of obtaining tool
There are high coverage rate and the high-quality smooth uniform perovskite thin film of little crystal grain.Prepare full-inorganic caesium lead halogenation perovskite thin film master
There are three kinds of methods, first method is to prepare perovskite quantum with the dispersion of the perovskite colloid nanocrystal of pre-synthesis
Point film.The perovskite colloid nanocrystal of pre-synthesis is formed, it is necessary to N with Kovalenko method2Protection and high reaction temperature
(scope is), preparation process condition is more harsh.Further, since perovskite nano particle in toluene not
The use of dissolubility and insulation long-chain surface ligand material (such as oleic acid and oleyl amine) so that the film synthesized by the method is showed
Go out relatively poor film surface coverage and electrical conductivity.
The method for preparing perovskite thin film second is to directly obtain perovskite thin film from perovskite precursor aqueous solution.Will
PbBr2It is dissolved in organic solvent such as DMSO to obtain perovskite precursor aqueous solution with CsBr powder, this method compares Kovalenko
Method it is more simple to operation.
Above two method synthesis full-inorganic perovskite thin film is all to make perovskite thin film fast by the way of high annealing
Speed crystallization.It can be seen that using first method and annealed processing that (90 DEG C are moved back in glove box from the article delivered at present
Fiery 5min) formed perovskite thin film prepare device, high-high brightness is 1698cd/m2(PbBr2:CsBr=1:1) and
3853cd/m2(PbBr2:CsBr=1:2).Using first method and without annealing, dried only under atmospheric environment
Device prepared by the perovskite thin film of 10min formation, high-high brightness is 2335cd/m2(PbBr2:CsBr=1:1).Use second
Device prepared by the perovskite thin film that the method for kind and annealed processing (70 DEG C of annealing 5min in glove box) are formed, high-high brightness
For 666cd/m2(PbBr2:CsBr=1:1).
In order to improve brightness, Wei. et al. proposes the third and prepares CsPbBr3The method of film, it is first that CsBr is water-soluble
Drop is added to PbBr2In-HBr solution, CsPbBr is obtained3Powder, then by acquired CsPbBr3Powder is dissolved in DMSO,
CsPbBr is obtained finally by a step spin-coating method3Film.But the method complex steps, workload are big, relatively time-consuming.
At present, although preparing smooth CsPbBr3Perovskite LED aspect has very big breakthrough, but simultaneously uncomfortable
For mass producing, how optimizing preparation section and improving film coverage turns into the key that perovskite light emitting diode is studied
Technology.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of full-inorganic perovskite thin film, the method is not only simple, it is easy to grasp
Make, and the film synthesized using the method, compared with the film synthesized using conventional anneal film drying method, film surface coverage rate is more
Greatly (close to 100%), particle is smaller, and more preferably, performance, the stability of device are also more preferable for film quality.
To achieve the above object, the technical scheme used is as follows：
A kind of preparation method of full-inorganic perovskite thin film, comprises the following steps：
1) at a certain temperature, by PbX2It is dissolved into CsX powder in organic solvent, obtains mixed solution；
2) above-mentioned mixed solution is spin-coated on substrate；
3) the good substrate of spin coating is stood and obtains full-inorganic perovskite thin film for a period of time；
Wherein described X is a kind of, PbX in halogen element Br, Cl, I2It is different with CsX mol ratio, and organic solvent species
It is different.
It is preferred that, gained caesium lead halide perovskite is CsPbX3(X=Br, Cl, I), its PbX2Mol ratio with CsX is
1:0.25~4.
It is preferred that, gained caesium lead halide perovskite is CsPbX3(X=Br, Cl, I), its concentration be 0.1wt%~
60wt%.
It is preferred that, step 1) described in halide powder dissolved in organic solvent at 2 DEG C~600 DEG C.
It is preferred that, step 1) described in organic solvent be dimethyl sulfoxide (DMSO) (Dimethylsulfoxide, DMSO), N, N-
One kind in dimethylformamide (N, N-Dimethylformamide, DMF), chloroform, chlorobenzene, toluene.
It is preferred that, step 2) described in mixed solution be spin-coated on spin coating hole-injecting material (such as PEDOT:PSS、MoO3、
V2O5、GeO2Deng) substrate on.
It is preferred that, step 2) in spin coating rotating speed be 2000rpm~6000rpm, spin-coating time be 5s~200s.
It is preferred that, step 3) in stand environment be vacuum (10-4Pa~105), Pa time of repose is 5min~60min.
It is an advantage of the invention that：
(1) present invention is compared with device prepared by conventional anneal film drying method, and preparation method is simpler, it is easy to operate,
So that opening, bright voltage is lower, and more preferably, its stability is also more preferable for performance；
(2) obtained full-inorganic perovskite thin film is prepared by the method for the present invention, film surface coverage rate is bigger (close
100%), particle is smaller, and film quality is more preferable.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The accompanying drawing used required in embodiment or description of the prior art is briefly described.
Fig. 1 is configuration of surface contrast schematic diagram, wherein (a) is the surface that the acquisition of film drying method is vacuumized using the present invention
The SEM schematic diagram of form, (b) is that the scanning electron for the configuration of surface that conventional anneal film drying method is obtained shows
Micro mirror schematic diagram；
Fig. 2 is PbBr2With the comparison diagram of CsBr electroluminescent device performances under identical mol ratio, figure intermediate cam shape mark
Line represents that the present invention vacuumizes film drying method data, and round dot line represents conventional anneal film drying method data, wherein (a)
For luminance-voltage figure, (b) is electroluminescent efficiency-voltage pattern；
Fig. 3 is to vacuumize film drying method based on the present invention to prepare PbBr2(mol ratio is 1 with CsBr different mol ratios:1
With 1:1.2) the performance comparison figure of electroluminescent device, wherein it is electroluminescent efficiency-electricity that (a), which is luminance-voltage figure, (b),
Pressure figure；
Fig. 4 is to vacuumize film drying method based on the present invention to prepare PbBr2(mol ratio is 1 with CsBr different mol ratios:1
With 1:1.2), and mol ratio be 1:The performance map of the electroluminescent device of 1 traditional annealing methods.
Embodiment
The embodiment of technical solution of the present invention is described in detail below in conjunction with accompanying drawing.Following examples are only used for
Clearly illustrate technical scheme, therefore be only used as example, and the protection model of the present invention can not be limited with this
Enclose.
Embodiment one：Film drying method is vacuumized with the present invention to prepare with CsPbBr3As the light emitting diode of luminescent layer,
Wherein PbBr2It is 1 with CsBr mol ratios:1：
The CsPbBr of preparation3Light emitting diode construction is：ITO/PEDOT:PSS/CsPbBr3/TPBi/Liq/Al。
CsPbBr is prepared in substrate surface3The method of film is as follows：
(1) by PbBr at 10 DEG C2With CsBr powder according to 1:1 mol ratio is dissolved in organic solvent DMSO.
(2) by above-mentioned CsPbBr3Mixed solution is spin-coated on spin coating hole injection layer PEDOT:On PSS substrate, spin coating
Rotating speed is 4000rpm, and spin-coating time is 60s.
(3) it is rotary with CsPbBr by above-mentioned3The substrate of film is placed under low vacuum (0.1MPa) environment and stands 20min, passes through
Vacuum pumping method takes unnecessary organic solvent away.
Figure (a), (b) in Fig. 1 are to vacuumize film drying method and conventional anneal film drying method using the present invention respectively
The CsPbBr of preparation3The scanning electron microscope diagram of film, it can be seen that vacuumizing the acquisition of film drying method
CsPbBr3Film coverage is higher, and particle is smaller, and film quality is more preferable.
Figure (a), (b) in Fig. 2 vacuumize film drying method respectively and prepared by conventional anneal film drying method
CsPbBr3The luminance-voltage figure of light emitting diode, electroluminescent efficiency-voltage pattern.From figure (a) it can be seen that using the present invention
Vacuumize the CsPbBr of film drying method preparation3The brightness of LED device will be apparently higher than using conventional anneal film drying
CsPbBr prepared by method3The brightness of LED device.Meanwhile, done from figure (b) it can be seen that vacuumizing film with the present invention
CsPbBr prepared by dry method3The efficiency of LED device is also apparently higher than being prepared with conventional anneal film drying method
CsPbBr3The efficiency of LED device.
Embodiment two：Film drying method is vacuumized with the present invention to prepare with PbBr2With the CsPbBr of CsBr different mol ratios3
It is used as the light emitting diode of luminescent layer：
The CsPbBr of preparation3Light emitting diode construction is：ITO/PEDOT:PSS/CsPbBr3/TPBi/Liq/Al。
CsPbBr is prepared in substrate surface3The method of film is as follows：
(1) by PbBr at 10 DEG C2With CsBr powder respectively according to 1:1、1:1.2 mol ratio is dissolved in organic solvent
In DMSO.
(2) by above-mentioned CsPbBr3Mixed solution is spin-coated on spin coating hole injection layer PEDOT respectively:The substrate of PSS films
On, spin coating rotating speed is 4000rpm, and spin-coating time is 60s.
(3) it is rotary with CsPbBr by above-mentioned3The substrate of film is placed under low vacuum (0.1MPa) environment and stands 20min.
Referring to Fig. 3, Fig. 4, figure (a), (b) in Fig. 3 are to vacuumize film drying method using the present invention to prepare respectively
PbBr2It is respectively 1 with CsBr mol ratios:1、1:1.2 CsPbBr3The luminance-voltage figure of light emitting diode, electroluminescent effect
Rate-voltage pattern.From figure (a) it can be seen that working as PbBr2It is 1 with CsBr mol ratios:When 1.2, the brightness of device will be apparently higher than
PbBr2It is 1 with CsBr mol ratios:1 device brightness.Simultaneously from figure (b) it can be seen that working as PbBr2It is 1 with CsBr mol ratios:1.2
When, the efficiency of device is also apparently higher than PbBr2It is 1 with CsBr mol ratios:1 device efficiency.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：It still may be used
To be modified to the technical scheme described in previous embodiment, or which part or all technical characteristic are equal
Replace；And these modifications or replacement, the essence of appropriate technical solution is departed from the model of technical scheme of the embodiment of the present invention
Enclose, it all should cover among the claim of the present invention and the scope of specification.
Claims (8)
1. a kind of preparation method of full-inorganic perovskite thin film, it is characterised in that comprise the following steps：
1) at a certain temperature, by PbX2It is dissolved into CsX powder in organic solvent, obtains mixed solution；
2) above-mentioned mixed solution is spin-coated on substrate；
3) the good substrate of spin coating is stood and obtains full-inorganic perovskite thin film for a period of time；
Wherein described X is Br, Cl, a kind of in I.
2. the preparation method of full-inorganic perovskite thin film according to claim 1, it is characterised in that gained caesium lead halide
Perovskite is CsPbX3, its PbX2Mol ratio with CsX is 1:0.25~4.
3. the preparation method of full-inorganic perovskite thin film according to claim 1, it is characterised in that gained caesium lead halide
Perovskite is CsPbX3, its concentration is 0.1wt%~60wt%.
4. the preparation method of full-inorganic perovskite thin film according to claim 1, it is characterised in that step 1) described in one
Constant temperature degree is 2 DEG C~600 DEG C.
5. the preparation method of full-inorganic perovskite thin film according to claim 1, it is characterised in that step 1) described in have
Machine solvent is one kind in dimethyl sulfoxide (DMSO), N,N-dimethylformamide, chloroform, chlorobenzene, toluene.
6. the preparation method of full-inorganic perovskite thin film according to claim 1, it is characterised in that step 2) described in mix
Solution is closed to be spin-coated on the substrate of spin coating hole-injecting material.
7. the preparation method of full-inorganic perovskite thin film according to claim 1, it is characterised in that step 2) in spin coating turn
Speed is 2000rpm~6000rpm, and spin-coating time is 5s~200s.
8. the preparation method of full-inorganic perovskite thin film according to claim 1, it is characterised in that step 3) middle standing ring
Border is vacuum, and time of repose is 5min~60min.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107863424A (en) * | 2017-11-13 | 2018-03-30 | 吉林大学 | A kind of full-inorganic luminescent device based on perovskite thin film and preparation method thereof |
| CN108251110A (en) * | 2018-01-29 | 2018-07-06 | 福州大学 | The method that a kind of perovskite quantum dot/thin film system builds multicolor luminous film |
| CN108539012A (en) * | 2018-02-28 | 2018-09-14 | 湖北大学 | A kind of full-inorganic perovskite resistance-variable storing device and preparation method thereof |
| CN108682749A (en) * | 2018-06-13 | 2018-10-19 | 西南大学 | Perovskite light emitting diode of multi-quantum pit structure and preparation method thereof |
| CN108735910A (en) * | 2018-05-25 | 2018-11-02 | 西南大学 | A kind of purely inorganic perovskite light emitting diode and preparation method thereof based on compound exciton recovery layer |
| CN108807704A (en) * | 2018-05-02 | 2018-11-13 | 西南大学 | A kind of perovskite laminated film and light emitting diode and preparation method thereof |
| CN109659394A (en) * | 2018-12-14 | 2019-04-19 | 北京化工大学 | A kind of preparation method and application of high quality full-inorganic perovskite thin film material |
| CN109686841A (en) * | 2018-11-23 | 2019-04-26 | 浙江理工大学上虞工业技术研究院有限公司 | A kind of hypotoxicity anti-solvent prepares the method and its application of Br based perovskite film |
| CN109713100A (en) * | 2018-12-21 | 2019-05-03 | 华中科技大学 | A method of preparing full-inorganic perovskite light emitting diode active layer |
| CN109980037A (en) * | 2019-03-07 | 2019-07-05 | 武汉大学 | Full-inorganic perovskite micron chip, Schottky type UV photodetector and preparation method |
| CN111874941A (en) * | 2020-07-10 | 2020-11-03 | 五邑大学 | CsPbBr3Perovskite and preparation method and device thereof |
| CN115124256A (en) * | 2022-06-24 | 2022-09-30 | 北京大学深圳研究生院 | Preparation method of all-inorganic perovskite thin film and narrow-band photoelectric detector |
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| CN106676631A (en) * | 2016-11-28 | 2017-05-17 | 昆明理工大学 | Method for preparing ABX3 perovskite single crystal film |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107863424A (en) * | 2017-11-13 | 2018-03-30 | 吉林大学 | A kind of full-inorganic luminescent device based on perovskite thin film and preparation method thereof |
| CN108251110A (en) * | 2018-01-29 | 2018-07-06 | 福州大学 | The method that a kind of perovskite quantum dot/thin film system builds multicolor luminous film |
| CN108539012A (en) * | 2018-02-28 | 2018-09-14 | 湖北大学 | A kind of full-inorganic perovskite resistance-variable storing device and preparation method thereof |
| CN108807704A (en) * | 2018-05-02 | 2018-11-13 | 西南大学 | A kind of perovskite laminated film and light emitting diode and preparation method thereof |
| CN108735910A (en) * | 2018-05-25 | 2018-11-02 | 西南大学 | A kind of purely inorganic perovskite light emitting diode and preparation method thereof based on compound exciton recovery layer |
| CN108682749B (en) * | 2018-06-13 | 2020-08-28 | 西南大学 | Perovskite light emitting diode with multi-quantum well structure and preparation method thereof |
| CN108682749A (en) * | 2018-06-13 | 2018-10-19 | 西南大学 | Perovskite light emitting diode of multi-quantum pit structure and preparation method thereof |
| CN109686841A (en) * | 2018-11-23 | 2019-04-26 | 浙江理工大学上虞工业技术研究院有限公司 | A kind of hypotoxicity anti-solvent prepares the method and its application of Br based perovskite film |
| CN109659394A (en) * | 2018-12-14 | 2019-04-19 | 北京化工大学 | A kind of preparation method and application of high quality full-inorganic perovskite thin film material |
| CN109713100A (en) * | 2018-12-21 | 2019-05-03 | 华中科技大学 | A method of preparing full-inorganic perovskite light emitting diode active layer |
| CN109980037A (en) * | 2019-03-07 | 2019-07-05 | 武汉大学 | Full-inorganic perovskite micron chip, Schottky type UV photodetector and preparation method |
| CN111874941A (en) * | 2020-07-10 | 2020-11-03 | 五邑大学 | CsPbBr3Perovskite and preparation method and device thereof |
| CN111874941B (en) * | 2020-07-10 | 2022-09-27 | 五邑大学 | CsPbBr 3 Perovskite and preparation method and device thereof |
| CN115124256A (en) * | 2022-06-24 | 2022-09-30 | 北京大学深圳研究生院 | Preparation method of all-inorganic perovskite thin film and narrow-band photoelectric detector |
| CN115124256B (en) * | 2022-06-24 | 2024-02-20 | 北京大学深圳研究生院 | Preparation method of all-inorganic perovskite film and narrow-band photoelectric detector |
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