CN106410048B - A method for preparing secondary perovskite solar cells - Google Patents
A method for preparing secondary perovskite solar cells Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 25
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010409 thin film Substances 0.000 claims abstract description 26
- 230000005540 biological transmission Effects 0.000 claims abstract description 20
- 238000011065 in-situ storage Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004064 recycling Methods 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- AJRXEXGVDMEBCT-UHFFFAOYSA-M [NH4+].[I-].C[N+]1=CC=CC=C1.[I-] Chemical compound [NH4+].[I-].C[N+]1=CC=CC=C1.[I-] AJRXEXGVDMEBCT-UHFFFAOYSA-M 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000004528 spin coating Methods 0.000 claims abstract description 8
- 238000004090 dissolution Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 238000007654 immersion Methods 0.000 claims abstract description 4
- 239000002390 adhesive tape Substances 0.000 claims description 6
- 229910052736 halogen Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- -1 halogen lead compound Chemical class 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000007740 vapor deposition Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- 239000010408 film Substances 0.000 description 8
- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 description 5
- 238000000280 densification Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
Classifications
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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
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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- Manufacturing & Machinery (AREA)
- Hybrid Cells (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
A method of secondary perovskite solar battery being prepared, step: the metal electrode of removal perovskite thin film battery；It is immersed into dissolution in chlorobenzene solution and removes hole transmission layer；Perovskite material heat resolve is at solid PbA2With the gas methylpyridinium iodide ammonium of volatilization；Pass through immersion or spin coating CH3NH3A aqueous isopropanol diauxic growth perovskite thin film；Prepare hole transmission layer；Evaporation metal electrode.Advantages of the present invention are as follows: 1) realize the recycling and reuse of a variety of materials in perovskite battery, 2) using thermal decomposition perovskite, Pb element is with PbA2Solid form recycle in situ, 3) PbA that recycles in situ2May be implemented to perovskite thin film beneficial growth, 4) it is based on growth in situ perovskite thin film CH3NH3PbA3The solar battery process of preparation is simpler, and cost is lower.
Description
Technical field
The present invention relates to solar battery utilization technology fields, and in particular to a kind of recycling perovskite solar energy in situ
Middle halogen lead compound is come the method for preparing secondary perovskite solar battery.
Background technique
As the exhaustion of global fossil energy and greenhouse effects and environmental pollution increasingly sharpen, clean energy resource and low-carbon warp
Ji has become the project of countries in the world important research.System of the novel thin film solar battery due to cheap cost and large area
Standby technology is increasingly valued by people.Hybrid inorganic-organic perovskite material is as a kind of high absorption coefficient of light and tool
There is the material of good electrical performance, the concern by researcher.Over the past two years based on the solar battery of perovskite material
Technology is quickly grown.The efficiency of highest perovskite battery has broken through 21% in laboratory at present.
Although the efficiency and stability of perovskite solar cell have substantially met commercialized needs, but still have several keys
Factor restricts the large-area applications of perovskite solar cell, one of them the most key factor is exactly perovskite solar cell
Used in perovskite material contain soluble heavy metal Pb element, easily the life of environment and the mankind are polluted.Although mesh
The perovskite material of preceding substituted Pb element, but the battery efficiency and stability that prepare are far away from the perovskite based on Pb element
Material.It is envisioned that following take the lead in using in perovskite solar cell being the perovskite material based on Pb.It is most of at present
Scientific research all concentrate on improving the photoelectric conversion efficiency of battery and improve the stability of battery, and for perovskite sun electricity
The Pb element pollution in pond and the recycling and reusing problem of battery are but rarely reported and study.The present invention is exactly to solve above-mentioned Pb dirt
The recycling and reusing problem of dye and perovskite battery.
Summary of the invention
Technical problem to be solved by the invention is to provide halogen lead compounds in a kind of recycling perovskite solar energy in situ
Method to prepare secondary perovskite solar battery has the characteristics that simple process, at low cost.
The technical scheme of the invention to solve the technical problem is: a kind of prepare secondary perovskite solar battery
Method, it is characterised in that the following steps are included:
1) metal electrode of perovskite thin film battery is removed；
2) battery after electrode will be removed to be immersed into chlorobenzene solution, hole transmission layer is removed in dissolution；
3) recycling halogen lead compound PbA in situ2: by perovskite material CH3NH3PbA3Heat resolve is at solid PbA2With
The gas methylpyridinium iodide ammonium CH of volatilization3NH3A；
4) growth of secondary perovskite thin film: by the above-mentioned PbA recycled in situ2Pass through immersion or spin coating CH3NH3A isopropyl
Alcoholic solution, the corresponding perovskite thin film CH of solution diauxic growth3NH3PbA3；
5) hole transmission layer is prepared；
6) evaporation metal electrode；
Wherein A is halogens: I, Cl or Br；
As an improvement, the metal electrode of the step 1) is Ag electrode, the electrode of removal perovskite thin film battery is specifically
Refer to and removes Ag electrode using adhesive tape.
As an improvement, the step 1) and step 2) it is combinable battery is immersed into chlorobenzene solution for directly it is disposable complete
At.
As an improvement, the heating temperature of the step 3) is 200~300 degree, the time is 5~30 minutes.
Further preferably, the heating temperature is 250 degree.
Preferably, the step 4) CH3NH3The concentration of A aqueous isopropanol is 5-20mg/mL.
Preferably, the soaking time of the step 4) is 50~70s, it is spin-coated as 2500~3500rmp, 50~70s.
Finally, the evaporation metal electrode of the step 6) refers to vapor deposition Ag electrode.
Compared with the prior art, the advantages of the present invention are as follows:
1) recycling and reuse of a variety of materials in perovskite battery are realized；
2) using thermal decomposition perovskite, Pb element is with PbA2Solid form in situ recycle；
3) PbA recycled in situ2It may be implemented to perovskite thin film beneficial growth；
4) it is based on growth in situ perovskite thin film CH3NH3PbA3The solar battery process of preparation is simpler, and cost is more
It is low.
Detailed description of the invention
Fig. 1 is embodiment 1 provided by the invention recycling PbI in situ2And the preparation process stream of second of perovskite battery
Cheng Tu.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1
To recycle porous perovskite battery structure: glass/transparent conductive film/densification TiO2/ porous TiO2/ perovskite
CH3NH3PbI3/ hole transmission layer [2,2,7,7-tetrakis (N, N-di-p-methoxyphenlamine) -9,9 '-spiro-
Bifluorene] for (spiro-MeOTAD)/Ag,
Specific preparation process is as follows:
(I) remove metallic silver using adhesive tape；
(II) cell substrate for removing metal electrode is immersed into chlorobenzene solution, hole transmission layer spiro- is removed in dissolution
MeOTAD；Chlorobenzene solution is using pure chlorobenzene；
(III) perovskite material CH3NH3PbI3In 250 degree of 10 minutes heat resolves at solid PbI2With the gas of volatilization
Methylpyridinium iodide ammonium CH3NH3I；
(IV) pass through spin coating methylpyridinium iodide ammonium CH3NH3I, the corresponding perovskite thin film CH of solution diauxic growth3NH3PbI3；
(V) hole transmission layer spiro-MeOTAD is prepared；
(VI) Ag electrode is deposited.
Wherein first step recycling Ag electrode and second step hole transmission layer can directly be immersed in battery in chlorobenzene solution
It is disposable to complete.
PbI is recycled using in situ2Secondary perovskite thin film growth technique:
Use the CH of concentration 7mg/mL3NH3I aqueous isopropanol obtains the two of high quality by spin coating (3000rmp, 60s)
Secondary perovskite thin film.
Embodiment 2:
To recycle porous perovskite battery structure: glass/transparent conductive film/densification TiO2/ porous TiO2/ perovskite
CH3NH3PbBr3/ hole transmission layer P3For HT/Ag,
Specific step is as follows:
(I) remove metallic silver using adhesive tape；
(II) battery for removing metal electrode is immersed into chlorobenzene solution, hole transmission layer P is removed in dissolution3HT；Chlorobenzene
Solution is using pure chlorobenzene；
(III) perovskite material CH3NH3PbBr3In 250 degree of 30 minutes heat resolves at solid PbBr2With the gas of volatilization
Body methylpyridinium iodide ammonium CH3NH3Br；
(IV) pass through spin coating methylpyridinium iodide ammonium CH3NH3Br solution, the corresponding perovskite thin film CH of diauxic growth3NH3PbBr3；
(V) hole transmission layer spiro-MeOTAD is prepared；
(VI) Ag electrode is deposited.
Wherein first step recycling Ag electrode and second step hole transmission layer can be directly one in battery submergence chlorobenzene solutions
Secondary property is completed.
PbBr is recycled using in situ2Secondary perovskite thin film growth technique:
Use the CH of concentration 10mg/mL3NH3Br aqueous isopropanol obtains high quality by spin coating (3000rmp, 60s)
Secondary perovskite thin film.
Embodiment 3:
To recycle the perovskite battery structure of plane: glass/transparent conductive film/densification TiO2/CH3NH3PbI3/ hole passes
Defeated layer P3For HT/Ag,
Specific step is as follows:
(I) remove metallic silver using adhesive tape；
(II) battery for removing metal electrode is immersed into chlorobenzene solution, hole transmission layer P is removed in dissolution3HT；Chlorobenzene
Solution is using pure chlorobenzene；
(III) perovskite material CH3NH3PbI3In 250 degree of 30 minutes heat resolves at solid PbI2With the gas of volatilization
Methylpyridinium iodide ammonium CH3NH3I；
(IV) by impregnating methylpyridinium iodide ammonium CH3NH3I, the corresponding perovskite thin film CH of diauxic growth3NH3PbI3；
(V) hole transmission layer spiro-MeOTAD is prepared；
(VI) Ag electrode is deposited.
Wherein first step recycling Ag electrode and second step hole transmission layer can be directly one in battery submergence chlorobenzene solutions
Secondary property is completed.
PbI is recycled using in situ2Secondary perovskite thin film growth technique:
Use the CH of concentration 10mg/mL3NH3I aqueous isopropanol, by impregnating recycling PbI in situ2Film acquisition in 1 minute is high
The secondary perovskite thin film of quality.
Embodiment 4:
To recycle the perovskite battery structure of plane: glass/transparent conductive film/densification TiO2/CH3NH3PbI3/ hole passes
Defeated layer P3For HT/Ag,
Specific step is as follows:
(I) remove metallic silver using adhesive tape；
(II) battery for removing metal electrode is immersed into chlorobenzene solution, hole transmission layer P is removed in dissolution3HT；Chlorobenzene
Solution is using pure chlorobenzene；
(III) perovskite material CH3NH3PbI3In 300 degree of 10 minutes heat resolves at solid PbI2With the gas of volatilization
Methylpyridinium iodide ammonium CH3NH3I；
(IV) by impregnating methylpyridinium iodide ammonium CH3NH3I, the corresponding perovskite thin film CH of diauxic growth3NH3PbI3；
(V) hole transmission layer spiro-MeOTAD is prepared；
(VI) Ag electrode is deposited.
Wherein first step recycling Ag electrode and second step hole transmission layer can be directly one in battery submergence chlorobenzene solutions
Secondary property is completed.
PbI is recycled using in situ2Secondary perovskite thin film growth technique:
Use the CH of concentration 15mg/mL3NH3I aqueous isopropanol, by impregnating recycling PbI in situ2Film acquisition in 1 minute is high
The secondary perovskite thin film of quality.
In the recycling of entire battery, third step (III) perovskite material is thermally decomposed into PbA2With the gas of volatilization
CH3NH3A is crucial.By the research of thermogravimetry and differential scanning calorimetry, obtain optimal thermal decomposition temperature and
Time.We have found that perovskite starts to decompose at 200 degree, equation is decomposed are as follows: CH3NH3PbA3(Gu)=PbA2(Gu)+
CH3NH3A (gas).Simultaneously we have found that with heating time variation, PbA after decomposition2Film shows different patterns,
Due to PbA2Atomic migration occurs.
According to CH3NH3PbA3The characteristic of thermal decomposition, decomposition temperature are 200~300 degree, select optimal to be 250 degree.In order to
Obtain optimal PbA2Pattern, has studied the relationship of pattern and resolving time, find the resolving time in 5-30 minutes, film
Pattern be it is cavernous, be conducive to the secondary film-forming of perovskite.
Although being described in detail about example embodiment and its advantage, it should be understood that do not depart from spirit of the invention and
In the case where protection scope defined in the appended claims, various change, substitutions and modifications can be carried out to these embodiments, than
Such as structure of perovskite battery.For other examples, those skilled in the art, which should be readily appreciated that, is keeping this hair
While in bright protection scope, the order of processing step can change.In addition, application range of the invention is not limited to specification
Described in specific embodiment technique, material composition, method and step.Execute the corresponding embodiment described with the present invention substantially
Identical function or acquisition be substantially the same as a result, can be applied to them according to the present invention.Therefore, appended by the present invention
Claim is intended to for these techniques, material composition or step being included in its protection scope.
Claims (8)
1. a kind of method for preparing secondary perovskite solar battery, it is characterised in that the following steps are included:
1) metal electrode of perovskite thin film battery is removed；
2) battery after electrode will be removed to be immersed into chlorobenzene solution, hole transmission layer is removed in dissolution；
3) recycling halogen lead compound PbA in situ2: by perovskite material CH3NH3PbA3Heat resolve is at solid PbA2And volatilization
Gas methylpyridinium iodide ammonium CH3NH3A；
4) growth of secondary perovskite thin film: by the above-mentioned PbA recycled in situ2Pass through immersion or spin coating CH3NH3A isopropanol is molten
Liquid, the corresponding perovskite thin film CH of solution diauxic growth3NH3PbA3；
5) hole transmission layer is prepared；
6) evaporation metal electrode；
Wherein A is halogens: I, Cl or Br.
2. according to the method described in claim 1, it is characterized by: the metal electrode of the step 1) be Ag electrode, go deliming
The electrode of titanium ore hull cell specifically refers to remove Ag electrode using adhesive tape.
3. according to the method described in claim 1, it is characterized by: the step 1) and step 2) are combinable for directly battery
It is immersed into chlorobenzene solution and disposably completes.
4. according to the method described in claim 1, it is characterized by: the heating temperature of the step 3) be 200~300 degree, when
Between be 5~30 minutes.
5. according to the method described in claim 4, it is characterized by: the heating temperature is 250 degree.
6. according to the method described in claim 1, it is characterized by: the step 4) CH3NH3The concentration of A aqueous isopropanol is 5
~20mg/mL.
7. according to the method described in claim 1, it is characterized by: the immersion of the step 4) or the soaking time in spin coating
For 50~70s, it is spin-coated as 2500~3500rmp, 50~70s.
8. according to the method described in claim 1, it is characterized by: the evaporation metal electrode of the step 6) refers to vapor deposition Ag electricity
Pole.
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| WO2019138154A1 (en) | 2018-01-09 | 2019-07-18 | Aalto-Korkeakoulusäätiö Sr | Method for refurbishing of carbon based perovskite solar cells (cpscs) and modules via recycling of active materials |
| CN109037452B (en) * | 2018-07-05 | 2022-01-28 | 南京邮电大学 | Preparation method of sulfur-containing organic-inorganic hybrid perovskite film and nanorod |
| CN109786561B (en) * | 2019-01-22 | 2023-07-11 | 华清创智光电科技(清远)有限公司 | Process for recycling perovskite active layer in perovskite device by amine liquefied perovskite method |
| CN110767812B (en) * | 2019-10-31 | 2023-08-25 | 南通大学 | A novel approach to increasing the lifetime of perovskite thin films |
| CN113130764B (en) * | 2021-04-08 | 2022-06-10 | 山东大学 | Zero-bias high-sensitivity perovskite single crystal X-ray detector and preparation method thereof |
| CN114871254B (en) * | 2022-04-08 | 2023-02-28 | 西湖大学 | Method for recovering lead iodide and substrate of waste perovskite device |
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| CN105355790A (en) * | 2015-11-24 | 2016-02-24 | 杨秋香 | Low cost perovskite solar cell being suitable for production |
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Non-Patent Citations (2)
| Title |
|---|
| In situ observation of heat-induced degradation of perovskite solar cells;G. Divitini 等;《NATURE ENERGY》;20160118;第1卷;正文第3页右栏In situ heating in the TEM部分 |
| Recycling Perovskite Solar Cells To Avoid Lead Waste;Andreas Binek 等;《ACS APPLIED MATERIALS & INTERFACES》;20160525;第8卷(第20期);正文第12882页左栏results部分，图1 |
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