CN108649125A - A method of improving perovskite material humidity stability - Google Patents
A method of improving perovskite material humidity stability Download PDFInfo
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- CN108649125A CN108649125A CN201810563019.5A CN201810563019A CN108649125A CN 108649125 A CN108649125 A CN 108649125A CN 201810563019 A CN201810563019 A CN 201810563019A CN 108649125 A CN108649125 A CN 108649125A
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- perovskite material
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Abstract
The invention discloses a kind of methods improving perovskite humidity stability, that is, by introducing fluorine carbon hydrophobic chain molecule RNH2Perovskite material is surface modified to improve the humidity stability of perovskite material, including perovskite material preparation and perovskite material be modified two steps with fluorine carbon hydrophobic chain molecular mixing.Perovskite material is modified using hydrophobic chain molecule in the present invention, amino is combined with Perovskite Phase can be such that the reduction of its surface defect and carrier lifetime increases, alkyl chain and C F functional groups can improve the hydrophobicity of material surface, finally the photoelectric properties of perovskite material and moisture stable performance is made to be obviously improved, the service life of perovskite-based photoelectric device is extended simultaneously so that perovskite material has fine development prospect in the practical application of photoelectric field.
Description
Technical field
The present invention relates to perovskite-based technical field of photoelectric material preparation, specially a kind of raising perovskite material humidity is steady
Qualitative method.
Background technology
In recent years, with CH3NH3PbI3It is rapidly developed, has become for the hybrid inorganic-organic perovskite material of representative
For most potential photovoltaic material.Compared with other semi-conducting materials, perovskite material has excellent photoelectric property, has
The excellent properties such as absorptivity height, longer, the bipolarity carrier transport of exciton diffusion length, and preparation process is simple, these are excellent
Point makes perovskite be not only ideal solar cell material, is led in other photoelectricity such as light emitting diode, laser and optical detector
Domain is also widely used.
Photoelectric device has general two big important technology indexs, includes the use longevity of the photoelectric conversion efficiency of device and device
Life.In recent years, having obtained extensive research, calcium titanium in relation to the efficient solar cell of perovskite and sensitive optical detector
The excellent photoelectric properties of pit wood material are constantly confirmed.But the stability problem of perovskite material has become restriction perovskite
The bottleneck of photoelectric device development, especially humidity stability, moisture can be such that it gradually decomposes, lead to the decline of photoelectric property.
Invention content
The present invention is directed to perovskite labile problem in air, provides a kind of raising perovskite material humidity stability
Method, i.e., perovskite material is surface modified by fluorine carbon hydrophobic chain molecule, obtain high efficiency and humidity stability it is excellent
Different perovskite material.By fluorine carbon hydrophobic chain molecule to perovskite material surface modification while improving stability test,
It can also achieve the purpose that passivated surface defect by the introducing of the active function groups of molecular end, to effectively promote perovskite
The opto-electronic conversion performance of material,
To achieve the above object, the technical solution adopted by the present invention is：
A method of perovskite material humidity stability being improved, by introducing fluorine carbon hydrophobic chain RNH2Molecule is to perovskite
Material is surface modified to improve the humidity stability of perovskite material, wherein fluorine carbon hydrophobic chain RNH2Molecule is CnF2n+ 1NH2, CnF2n+1CH2NH2, CnF2n+1CH2CH2NH2And CnF2n+1CH2CH2CH2NH2In it is one or more, wherein n be >=6, including
Following steps：
Step 1 weighs lead halide and halogenation methylamine and prepares solution using solvent dissolving respectively, by prepared lead halide
Solution is slowly added drop-wise in halogenation methylamine solution at room temperature, and 30min~2h is stirred under atmosphere of inert gases, obtains perovskite
Material；
A certain proportion of Hydrophobic small molecules RNH is added in step 2, the perovskite material obtained to step 12, after stirring
To the perovskite material of modification.
Preferably, the molar ratio of lead halide and halogenation methylamine is 1 in step 1:1~1.1.
Preferably, the solvent in step 1 for dissolving lead halide is formamide, acetamide, N-METHYLFORMAMIDE, N, N- bis-
It is one or more in methylformamide, n,N-dimethylacetamide and dimethyl sulfoxide (DMSO), the solvent for dissolving halogenation methylamine
For isopropanol, the inert atmosphere is nitrogen or argon gas.
Preferably, perovskite material includes the perovskite quantum dot of zero dimension, one-dimensional perovskite Nano/micron in step 1
The perovskite particle of line, two perovskite nanometer sheets and three-dimensional.
Preferably, fluorine carbon hydrophobic chain molecule RNH in step 22Mass ratio with perovskite material is 0.05~0.5：1, instead
It is 0 DEG C~60 DEG C to answer temperature, and the reaction time is 30min~4h.
Compared with prior art, beneficial effects of the present invention are as follows：
1, preparation method of the invention is simple, and mild condition is of low cost, while preparation process controllability is high.
2, perovskite material surface defect prepared by the present invention reduces, and carrier lifetime increases, which is answered
When for optical detector, responsiveness rises to 1.27A/W from 0.52A/W, and when being applied to solar cell, efficiency increases from 11%
To 15%.
3, the humidity stability of perovskite material of the invention has apparent improvement, is 55% ± 5% in relative humidity
Under conditions of, using in the present invention perovskite material prepare detector and solar cell without encapsulation place 30 days it is several
It does not decompose, photoelectric properties still keep initial 80% or more.
Specific implementation mode
The present invention is described in detail below in conjunction with specific implementation mode, so that those skilled in the art can be more
Good understanding is of the invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
According to 1:The score of the amount of 1 substance also known as amount 461.01mg lead iodides (PbI2) and 158.97mg iodate methylamines
(CH3NH3I), by PbI2It is dissolved in stirring 2h in the N,N-dimethylformamide (DMF) of 1mL and obtains the N of lead iodide, N- dimethyl
Formamide solution, by CH3NH3It is dissolved in stirring 2h in the aqueous isopropanol of 20mL and obtains the aqueous isopropanol of iodate methylamine, then
The n,N-Dimethylformamide solution of lead iodide is slowly dropped in the aqueous isopropanol of iodate methylamine under argon atmosphere, after
Continuous stirring 20min obtains flaxen suspension, and the perfluoro capryl second of the 0.05mol% of 10 μ L is finally added into suspension
Amine, stirs 30min, and the perovskite micro wire modified is denoted as 1#.
Embodiment 2
According to 1:The score of the amount of 1 substance also known as amount 461.01mg lead iodides (PbI2) and 158.97mg iodate methylamines
(CH3NH3I), by PbI2It is dissolved in stirring 2h in the N,N-dimethylformamide (DMF) of 1mL and obtains the N of lead iodide, N- dimethyl
Formamide solution, by CH3NH3It is dissolved in stirring 2h in the aqueous isopropanol of 20mL and obtains the aqueous isopropanol of iodate methylamine, then
The n,N-Dimethylformamide solution of lead iodide is slowly dropped in the aqueous isopropanol of iodate methylamine under argon atmosphere, after
Continuous stirring 20min obtains flaxen suspension, and the perfluoro capryl amine of the 0.05mol% of 10 μ L is finally added into suspension,
30min is stirred, the perovskite micro wire modified is denoted as 2#.
Embodiment 3
According to 1:The score of the amount of 1 substance also known as amount 461.01mg lead iodides (PbI2) and 158.97mg iodate methylamines
(CH3NH3I), then according to 4:1 volume ratio weighs the diformazan of the N,N-dimethylformamide (DMF) and 200 μ L of 800 μ L respectively
Base sulfoxide is simultaneously mixed to get mixed solvent, then by PbI2And CH3NH3I is added in the mixed solvent and stirs 3h at 50 DEG C,
Obtain perovskite precursor solution；Compound concentration is that the chlorobenzene solution of the perfluoro capryl ethamine of 0.2mg/mL is for use.
The perovskite micro wire being prepared in embodiment 1 and embodiment 2 is further assembled optical detector by us, is gone forward side by side
Row photoelectric properties are tested.1# suspension and 2# suspension are made calcium titanium 10 times by us with the rotating speed spin coating of 2000rpm respectively first
Substrate of glass is completely covered in mine micro wire, and 30min is then heated at 100 DEG C, then 300nm Au electricity is deposited under condition of high vacuum degree
Pole obtains 1# optical detectors and 2# optical detectors.
We carry out photoelectric properties test to 1# optical detectors and 2# optical detectors, and the responsiveness of 1# optical detectors is
1.35A/W, and under conditions of relative humidity is 55% ± 5%, no encapsulation places 30 days photoelectric currents and still keeps initial 88%,
Without being only original 25% under perovskite optical detector the same terms of modification.The responsiveness of 2# optical detectors is 1.27A/
W, and under conditions of relative humidity is 55% ± 5%, no encapsulation places 30 days photoelectric currents and still keeps initial 85%, without
The responsiveness of the perovskite material of modification is 0.52A/W, and photoelectric current is only original 30% after placing 30 days under the same terms.
The perovskite precursor solution that we obtain embodiment 3 is applied in solar cell, first in clean FTO
On with spin-coating method prepare TiO2Layer, anneal 1h in 500 DEG C.Then precursor solution embodiment 3 obtained in glove box with
The rotating speed of 2000rpm is spin-coated on TiO2On layer, the perfluoro capryl of a concentration of 0.2mg/mL of 200 μ L is added dropwise during spin coating
The chlorobenzene of amine heats 60min as anti-solvent, in 100 DEG C and obtains perovskite light-absorption layer, finally again with the rotating speed spin coating of 5000rpm
The Au electrodes of last layer 100nm thickness are deposited as hole transmission layer in the Spiro of 72mg/mL, you can obtain solar cell.
We have carried out performance test to obtained solar cell, and the efficiency of the solar cell is 15%, opposite
Under conditions of humidity is 55% ± 5%, no encapsulation places 30 days photoelectric currents and still keeps initial 80%, without the calcium titanium of modification
The corresponding efficiency of pit wood material is 11%, and photoelectric current is only original 25% after placing 30 days under the same terms.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of method improving perovskite material humidity stability, which is characterized in that by introducing fluorine carbon hydrophobic chain RNH2Molecule
Perovskite material is surface modified to improve the humidity stability of perovskite material, the fluorine carbon hydrophobic chain RNH2Molecule is
CnF2n+1NH2, CnF2n+1CH2NH2, CnF2n+1CH2CH2NH2And CnF2n+1CH2CH2CH2NH2In it is one or more, wherein n be >=
6, include the following steps：
Step 1 weighs lead halide and halogenation methylamine and prepares solution using solvent dissolving respectively, by prepared halogenation lead solution
It is slowly dropped at room temperature in halogenation methylamine solution, 30min~2h is stirred under atmosphere of inert gases, obtains perovskite material
Material；
A certain proportion of hydrophobic chain molecule RNH is added in step 2, the perovskite material obtained to step 12, modified after stirring
Perovskite material.
2. a kind of method improving perovskite material humidity stability according to claim 1, which is characterized in that step 1
The molar ratio of middle lead halide and halogenation methylamine is 1：1~1.1.
3. a kind of method improving perovskite material humidity stability according to claim 1, which is characterized in that step 1
In for dissolve lead halide solvent be formamide, acetamide, N-METHYLFORMAMIDE, N,N-dimethylformamide, N, N- diformazans
One or more in yl acetamide and dimethyl sulfoxide (DMSO), the solvent for dissolving halogenation methylamine is isopropanol, the indifferent gas
Atmosphere is nitrogen or argon gas.
4. a kind of method improving perovskite material humidity stability according to claim 1, which is characterized in that step 1
The perovskite material includes that the perovskite quantum dot, one-dimensional perovskite Nano/micron line, two perovskites of zero dimension are received
Rice piece and three-dimensional perovskite particle.
5. a kind of method improving perovskite material humidity stability according to claim 1, which is characterized in that step 2
The fluorine carbon hydrophobic chain molecule RNH2Mass ratio with perovskite material is 0.05~0.5：1, reaction temperature is 0 DEG C~60
DEG C, the reaction time is 30min~4h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110867519A (en) * | 2019-11-26 | 2020-03-06 | 吉林大学 | Light emitting diode and preparation method thereof |
| CN110887811A (en) * | 2019-12-03 | 2020-03-17 | 南方科技大学 | Perovskite-based composite material for laser humidity sensor, and preparation method and application thereof |
| CN111816772A (en) * | 2020-06-22 | 2020-10-23 | 隆基绿能科技股份有限公司 | Perovskite solar cell, production method and perovskite cell component |
| CN111933802A (en) * | 2020-08-18 | 2020-11-13 | 昆山协鑫光电材料有限公司 | Application of ionic liquid in preparation of perovskite photosensitive layer and perovskite solar cell |
| CN113340948A (en) * | 2021-06-09 | 2021-09-03 | 重庆大学 | Preparation method of high-response humidity sensor based on halogenated perovskite microcrystal and product thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110867519A (en) * | 2019-11-26 | 2020-03-06 | 吉林大学 | Light emitting diode and preparation method thereof |
| CN110887811A (en) * | 2019-12-03 | 2020-03-17 | 南方科技大学 | Perovskite-based composite material for laser humidity sensor, and preparation method and application thereof |
| CN110887811B (en) * | 2019-12-03 | 2023-01-13 | 南方科技大学 | Perovskite-based composite material for laser humidity sensor, and preparation method and application thereof |
| CN111816772A (en) * | 2020-06-22 | 2020-10-23 | 隆基绿能科技股份有限公司 | Perovskite solar cell, production method and perovskite cell component |
| CN111816772B (en) * | 2020-06-22 | 2024-03-08 | 隆基绿能科技股份有限公司 | Perovskite solar cell, production method thereof and perovskite cell assembly |
| CN111933802A (en) * | 2020-08-18 | 2020-11-13 | 昆山协鑫光电材料有限公司 | Application of ionic liquid in preparation of perovskite photosensitive layer and perovskite solar cell |
| CN111933802B (en) * | 2020-08-18 | 2024-04-19 | 昆山协鑫光电材料有限公司 | Application of ionic liquid in preparation of perovskite photosensitive layer and perovskite solar cell |
| CN113340948A (en) * | 2021-06-09 | 2021-09-03 | 重庆大学 | Preparation method of high-response humidity sensor based on halogenated perovskite microcrystal and product thereof |
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