CN107195710A - A kind of method that the inorganic perovskite thin film of high-luminous-efficiency is prepared based on one-step method - Google Patents
A kind of method that the inorganic perovskite thin film of high-luminous-efficiency is prepared based on one-step method Download PDFInfo
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- CN107195710A CN107195710A CN201710401775.3A CN201710401775A CN107195710A CN 107195710 A CN107195710 A CN 107195710A CN 201710401775 A CN201710401775 A CN 201710401775A CN 107195710 A CN107195710 A CN 107195710A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000010409 thin film Substances 0.000 title claims abstract description 37
- 238000004528 spin coating Methods 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 17
- -1 caesium halide Chemical class 0.000 claims abstract description 17
- 150000004820 halides Chemical class 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 8
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000031700 light absorption Effects 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 30
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 10
- 238000001704 evaporation Methods 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 239000002096 quantum dot Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
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Abstract
The present invention provides a kind of method that the inorganic perovskite thin film of high-luminous-efficiency is prepared based on one-step method；Lead halide and caesium halide are dissolved in solvent, perovskite precursor solution is obtained；Then heating after precursor solution spin coating is obtained into the inorganic perovskite thin film of high-luminous-efficiency；The mol ratio of the lead halide and caesium halide is 1: 1~1.3.The present invention has that cost is low, easy to operate, heat treatment temperature requires low feature, is easy to the large-scale production of perovskite thin film, and by limiting predecessor ratio, on the premise of no change perovskite crystalline phase, be obviously improved the luminous efficiency of film.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic perovskite material, and in particular to one kind is prepared occurred frequently based on one-step method
The method of the inorganic perovskite thin film of light efficiency.
Background technology
In the past few years, perovskite material shows huge potentiality in field of photoelectric devices.Perovskite material has
Have the advantages that manufacturing cost is low, absorption coefficient is high, carrier transport distance and adjustable band-gap, with organic inorganic hybridization calcium titanium
Pit wood material CH3NH3PbX3（X is halogen）The solar cell prepared as light absorbing layer, its photoelectric transformation efficiency has exceeded
20%.At the same time, as a kind of high efficiency semiconductor luminescent material, perovskite is in fields such as fluorescent device, laser, optical detections
Also there are a series of breakthroughs.However, traditional hydridization perovskite material is easily by factors such as temperature, humidity and illumination
Influence, property stable in the air is poor, degradable.This characteristic seriously constrains practicality of the associated materials in production, life.
At the same time, purely inorganic perovskite starts to receive more and more attention due to its excellent heat endurance and air stability.
Currently, how the inorganic perovskite thin film of synthesizing high lumineseent efficiency, have become a big focus of perovskite research field.Calcium titanium
The performance of ore deposit film and preparation method are closely bound up.The preparation method of current inorganic perovskite thin film can be divided into evaporation and spin coating
Method.Evaporation, which prepares perovskite thin film, to be needed to carry out under vacuum environment and high evaporating temperature, and harsh preparation condition is very big
The preparation cost of material is added, is unfavorable for the industrialized production of inorganic perovskite thin film.
Quantum dot (CQDs) because of it there is quantum size effect and spectrum peak position can be caused by characteristics such as particle size adjustments
People widely pay close attention to.Lead selenide（PbSe）It is a kind of direct low energy gap（0.28eV）Semi-conducting material, because it is to infrared band
Light can produce many exciton effects when there is stronger absorption, illumination, therefore prior art is for the report of caesium halide lead quantum dot
Road is more；Unfortunate existing CsPbX3The report of film does not have, and is primarily due to CsPbX3Film can not be prepared according to prior art.
If according to the preparation method of existing other materials, operating procedure is first in one layer of PbBr of substrate surface spin coating2Film,
After low temperature drying, the alcohol solution for soaking by film in CsBr passes through high-temperature heat treatment formation calcium again for a period of time, finally
Titanium ore film.In immersion process, overlong time can influence the growth quality of film, and the time is too short, and predecessor can not fully be sent out
Raw reaction, easily forms dephasign, requires very high to preparation manipulation；In addition, CsBr heat endurance is high, after the characteristics of being difficult diffusion makes
Phase heat treatment becomes difficult, it is necessary to which prolonged high-temperature process could form perovskite crystalline phase, and therefore, two step infusion methods are due to reality
The limitation of border application can not be in inorganic CsPbX3It is promoted in terms of perovskite thin film preparation.
Therefore, research and develop new preparation technology and obtain the inorganic perovskite thin film of high-luminous-efficiency very with realistic meaning.
The content of the invention
For defect of the prior art, it is an object of the invention to provide it is a kind of based on one-step method prepare high-luminous-efficiency without
The method of machine perovskite thin film；With cost is low, easy to operate, heat treatment temperature requires low feature, it is easy to perovskite thin film
Large-scale production, and by limiting predecessor ratio, on the premise of no change perovskite crystalline phase, it has been obviously improved film
Luminous efficiency.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method that the inorganic perovskite thin film of high-luminous-efficiency is prepared based on one-step method, is comprised the following steps, by lead halide and
Caesium halide is dissolved in solvent, obtains perovskite precursor solution；Then heating after precursor solution spin coating is obtained into light efficiency occurred frequently
The inorganic perovskite thin film of rate；The mol ratio of the lead halide and caesium halide is 1: 1~1.3.
In above-mentioned technical proposal, the lead halide and caesium halide are respectively lead bromide, cesium bromide.
In above-mentioned technical proposal, the solvent is dimethyl sulfoxide (DMSO).
In above-mentioned technical proposal, the solid content of the perovskite precursor solution is 15wt%.
In above-mentioned technical proposal, the rotating speed of the spin coating is 3000rpm, and the time of spin coating is 60s.
In above-mentioned technical proposal, the temperature of the heating is 70 DEG C, and the time is 15min.
The method that the predecessor ratio regulation and control that the present invention is provided prepare inorganic perovskite thin film, is prepared by a step spin-coating method
Described inorganic perovskite thin film is obtained, be may comprise steps of：
By lead halide PbX2It is dissolved in corresponding caesium halide CsX according to certain stoichiometric proportion in a kind of predecessor solvent, often
Temperature stirring forms certain density perovskite precursor solution to being completely dissolved.
A certain amount of precursor solution is added dropwise on a glass substrate using liquid-transfering gun, spin coating forms film.
Film after spin coating is placed on warm table, it is thin to prepare inorganic perovskite through heat treatment after a while
Film.
The present invention also disclosed a kind of inorganic perovskite thin film of high-luminous-efficiency；The inorganic perovskite of high-luminous-efficiency is thin
The preparation method of film comprises the following steps, and lead halide and caesium halide are dissolved in solvent, obtains perovskite precursor solution；Then
Heating after precursor solution spin coating is obtained into the inorganic perovskite thin film of high-luminous-efficiency；The mol ratio of the lead halide and caesium halide
For 1: 1~1.3.
Stoichiometric proportion of the invention by regulating and controlling predecessor lead halide and caesium halide so that what a step spin-coating method was prepared
Inorganic perovskite thin film has higher quantum yield, is preferably 1: 1.2 especially by the mol ratio of lead halide and caesium halide
Limiting slight excessive caesium halide can promote lead halide thoroughly to react, it is to avoid produce the defect states such as metallic lead, supplement simultaneously
Halogen, compensate for the volatile easy deficiency for forming vacancy defect of halogen.
Compared with prior art, the present invention has the advantage that：
The present invention uses simple step spin-coating method, compared to evaporation and two step infusion methods, and process costs are low, easy to operate, repeat
Property it is high, the demand of scale industrial production can be met.
The present invention regulates and controls the performance of film by changing the stoichiometric proportion of predecessor, is not required to add other materials, system
Standby film still keeps original crystalline phase, is produced without other dephasigns.
Inorganic perovskite thin-film material luminous efficiency prepared by the present invention is high, is conducive to the photoelectric device in later stage to prepare and group
Dress.
Brief description of the drawings
Fig. 1 is PbBr2The PLQY data comparison figures of sample are prepared under different mol ratio with CsBr；
Fig. 2 is CsPbBr made from embodiment 13The SEM figures of film；
Fig. 3 is CsPbBr made from embodiment 33The SEM figures of film；
Fig. 4 is CsPbBr made from embodiment 1 and embodiment 33The XRD comparison diagrams of film.
Embodiment
Below by way of specific embodiment, the invention will be further described.
The present invention prepares inorganic perovskite thin film using a step spin-coating method, is carried out under inert gas shielding, first by halogen
Change lead PbX2Be dissolved in caesium halide CsX according to certain stoichiometric proportion in a kind of predecessor solvent, stirred under certain temperature to
It is completely dissolved, forms certain density perovskite precursor solution, then a certain amount of precursor solution is added dropwise in glass lined
On bottom, spin coating forms film, then the film after spin coating is placed on warm table, and nothing is prepared through heat treatment after a while
Machine perovskite thin film.
Embodiment 1
Weigh 0.0614g PbBr2Added with 0.0356g CsBr in 0.5ml DMSO, stirring at normal temperature is matched somebody with somebody to being completely dissolved
Into PbBr2It is 1 with CsBr mol ratios:1, solution concentration is 15wt% perovskite precursor solution.
25 μ l perovskite precursor solution is pipetted using liquid-transfering gun, be slowly added dropwise on a glass substrate, 3000rpm,
Spin coating forms film under the conditions of 60s.
Film is placed on warm table, by 70 DEG C, 15min heat treatment prepares inorganic perovskite thin film, sample
Product are labeled as a1.
Embodiment 2
Using the identical technique of embodiment 1, difference is, by the PbBr of embodiment 121 is changed to CsBr mol ratios:1.1, other
Condition is consistent, and sample is labeled as a2.
Embodiment 3
Using the identical technique of embodiment 1, difference is, by the PbBr of embodiment 121 is changed to CsBr mol ratios:1.2, other
Condition is consistent, and sample is labeled as a3.
Embodiment 4
Using the identical technique of embodiment 1, difference is, by the PbBr of embodiment 121 is changed to CsBr mol ratios:1.3, other
Condition is consistent, and sample is labeled as a4.
Fig. 1 is PbBr2PL comparison diagrams, the PLQY data comparison figures of sample are prepared under different mol ratio with CsBr；Fig. 2 is
CsPbBr made from embodiment 13The SEM figures of film；Fig. 3 is CsPbBr made from embodiment 33The SEM figures of film；Fig. 4 is implementation
CsPbBr made from example 1 and embodiment 33The XRD comparison diagrams of film.
By limiting PbBr in perovskite precursor solution2With CsBr mol ratio, inorganic perovskite can be significantly improved
The luminous efficiency of film.As seen in Figure 1, with the increase of CsBr ratios in predecessor, the luminous intensity of film by
It is cumulative to add, work as PbBr2It is higher than 1 with CsBr mol ratio:When 1.2, luminous intensity almost no longer changes, the quantum production of film
Rate also tends to stabilization, therefore, PbBr21 is elected as with CsBr mol ratio:It is optimal when 1.2；As seen in Figure 2, even if changing
Ratio in predecessor shared by CsBr, but significant change does not occur for the pattern of film, original pattern is maintained well；
Although can be seen that PbBr in precursor solution by Fig. 3, Fig. 42It is non-stoichiometric with CsBr, but the inorganic calcium prepared
Other dephasigns are not found in titanium ore film, are still single CsPbBr3Crystalline phase.
Claims (10)
1. a kind of method that the inorganic perovskite thin film of high-luminous-efficiency is prepared based on one-step method, it is characterised in that including following step
Suddenly, lead halide and caesium halide are dissolved in solvent, obtain perovskite precursor solution；Then it will be heated after precursor solution spin coating
Obtain the inorganic perovskite thin film of high-luminous-efficiency；The mol ratio of the lead halide and caesium halide is 1: 1~1.3.
2. preparing the method for the inorganic perovskite thin film of high-luminous-efficiency based on one-step method according to claim 1, its feature exists
In the lead halide and caesium halide are respectively lead bromide, cesium bromide.
3. preparing the method for the inorganic perovskite thin film of high-luminous-efficiency based on one-step method according to claim 1, its feature exists
In the solvent is dimethyl sulfoxide (DMSO).
4. preparing the method for the inorganic perovskite thin film of high-luminous-efficiency based on one-step method according to claim 1, its feature exists
In the solid content of the perovskite precursor solution is 15wt%.
5. preparing the method for the inorganic perovskite thin film of high-luminous-efficiency based on one-step method according to claim 1, its feature exists
In the rotating speed of the spin coating is 3000rpm, and the time of spin coating is 60s.
6. preparing the method for the inorganic perovskite thin film of high-luminous-efficiency based on one-step method according to claim 1, its feature exists
In the temperature of the heating is 70 DEG C, and the time is 15min.
7. preparing the method for the inorganic perovskite thin film of high-luminous-efficiency based on one-step method according to claim 1, its feature exists
In the mol ratio of the lead halide and caesium halide is 1: 1.2.
8. prepared by the method for preparing the inorganic perovskite thin film of high-luminous-efficiency based on one-step method according to claim 1 inorganic
Perovskite thin film.
9. a kind of solar cell, it is characterised in that the light absorption layer material of the solar cell is nothing described in claim 8
Machine perovskite thin film.
10. application of the inorganic perovskite thin film in solar cell is prepared described in claim 8.
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| CN107946465A (en) * | 2017-11-16 | 2018-04-20 | 中南大学 | A kind of prepared in air high efficiency, perovskite solar cell of stabilization and preparation method thereof |
| CN108467208A (en) * | 2018-04-04 | 2018-08-31 | 武汉理工大学 | A kind of CsPbX3Nanocrystalline doping borogermanates glass and the preparation method and application thereof |
| CN108511706A (en) * | 2018-03-13 | 2018-09-07 | 合肥国轩高科动力能源有限公司 | Preparation method of two-dimensional inorganic perovskite negative electrode material for lithium battery |
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| CN109300805A (en) * | 2018-08-31 | 2019-02-01 | 华南师范大学 | Vacuum control CsPbIxBr3-xThe method and photovoltaic device of perovskite growth |
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