CN109943728B - Method for recovering lead in perovskite solar cell - Google Patents
Method for recovering lead in perovskite solar cell Download PDFInfo
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- CN109943728B CN109943728B CN201910379191.XA CN201910379191A CN109943728B CN 109943728 B CN109943728 B CN 109943728B CN 201910379191 A CN201910379191 A CN 201910379191A CN 109943728 B CN109943728 B CN 109943728B
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000005525 hole transport Effects 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000004821 distillation Methods 0.000 claims description 35
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000004408 titanium dioxide Substances 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000008247 solid mixture Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 241001411320 Eriogonum inflatum Species 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims 2
- 238000011084 recovery Methods 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- 239000007787 solid Substances 0.000 description 7
- 238000009835 boiling Methods 0.000 description 5
- 238000005292 vacuum distillation Methods 0.000 description 5
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 238000013082 photovoltaic technology Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- IKUCKMMEQAYNPI-UHFFFAOYSA-N [Pb].CN.[I] Chemical compound [Pb].CN.[I] IKUCKMMEQAYNPI-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
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- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- FZHSXDYFFIMBIB-UHFFFAOYSA-L diiodolead;methanamine Chemical compound NC.I[Pb]I FZHSXDYFFIMBIB-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for recovering lead in a perovskite solar cell, which comprises the following steps: manually stripping the substrate material, the conductive glass and the top electrode; removing the hole transport layer by a chemical solvent dissolving method; extracting a lead-containing compound; and (4) detecting the lead recovery rate, the recovery quality and the recovery effect. The method solves the problem of toxicity of the perovskite solar cell material, ensures green and environment-friendly performance in the implementation process, and avoids the pollution problem in the recovery process.
Description
Technical Field
The invention discloses a method for recovering lead in a perovskite solar cell, and belongs to the technical field of pollutant recovery.
Background
Among emerging photovoltaic technologies, organic lead halide perovskite solar cells with low temperature and dissolution processing capabilities have received increasing attention in recent years. In addition to the continuous progress in efficiency, perovskite solar cells have good stability, which shows great promise as a new photovoltaic technology for large-area use and cost competitiveness.
However, the problem of toxicity of lead in conventional lead-based perovskites has greatly limited the large-scale commercial application of perovskite solar cells. The environmental threat and ecotoxicity associated with the use of the toxic metallic lead may prevent perovskite solar cells from becoming a new and brisk photovoltaic technology. Therefore, from the economic and environmental aspects, the perovskite solar cell is widely applied and the economic benefit is improved, and the environmental problems such as lead pollution caused by the waste perovskite solar cell need to be solved.
Disclosure of Invention
The invention aims to provide a method for recovering lead in a perovskite solar cell, which solves the problem of lead pollution of an aged perovskite solar cell.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for recovering lead in a perovskite solar cell comprises the following steps:
1) stripping a substrate material, conductive glass and an electrode of the perovskite solar cell;
2) soaking the stripped perovskite solar cell in a dissolving agent to remove the hole transport layer;
3) the method for extracting the lead-containing compound specifically comprises the following steps:
31) soaking the surface of the perovskite solar cell in distilled water for a certain time, taking out the perovskite solar cell, and drying the perovskite solar cell in a small tubular heating furnace;
32) after drying, heating the small-sized tubular heating furnace to carry out heat treatment on the perovskite solar cell, so that the perovskite solar cell is decomposed into a solid mixture of lead iodide and titanium dioxide and organic gas;
33) soaking a solid mixture of lead iodide and titanium dioxide in a dissolving agent, stirring, and filtering to remove insoluble titanium dioxide to obtain a solution in which lead iodide is dissolved;
34) and (3) putting the solution dissolved with the lead iodide into a reduced pressure distillation device, setting the distillation temperature at 60 ℃ and the vacuum pressure at 1.3kPa, and continuing until the liquid is evaporated to dryness to separate out pure lead iodide.
In the step 1), the substrate material and the conductive glass of the perovskite solar cell are peeled off in a manual peeling mode, and the electrode on the top is taken out after the surface of the perovskite solar cell is pressed by transparent adhesive.
Ethyl acetate is selected as a dissolving agent in the step 2).
In the step 2), the entire perovskite solar cell is immersed in ethyl acetate while stirring, and after 1 minute, the perovskite solar cell is taken out of the solvent and dried under a nitrogen stream to complete the removal of the hole transport layer.
In the step 31), the surface of the perovskite solar cell is immersed in distilled water for 1 second and then taken out.
In the step 31), a nitrogen gas stream was introduced into a small tubular heating furnace to dry the mixture.
The aforementioned drying time was 3 minutes.
In the aforementioned step 32), the small-sized tube furnace was heated to 150 ℃ for ten minutes.
Dimethylformamide was selected as the dissolving agent in the aforementioned step 33).
In the aforementioned step 34), the distillation apparatus includes a distillation flask, a k-shaped distillation head, a straight condensation tube, a vacuum connecting tube and a receiving flask; a Kirschner distillation head is inserted on the distillation flask, a thermometer is inserted into the side opening of the Kirschner distillation head through a thermometer sleeve, and a capillary tube is inserted into the straight opening of the distillation flask; the upper end of the capillary tube is additionally provided with a rubber tube with a spiral clamp; the bottle stopper of the distillation bottle is provided with a joint hole for inserting a measuring joint of a vacuum pressure gauge; two joints on the straight condensing pipe are respectively a water inlet and a water outlet of condensed water, and the water outlet is connected with a receiving bottle; and the receiving bottle is provided with a vacuum connecting and leading pipe for connecting an air pumping system.
The invention achieves the following beneficial effects:
the method can effectively extract the toxic material lead in the perovskite solar cell, solves the problem of the toxicity of perovskite solar cell materials, is environment-friendly in the implementation process, and avoids the problem of secondary pollution in the recovery process.
Drawings
FIG. 1 is a view showing the construction of a vacuum distillation apparatus according to the present invention;
FIG. 2 is a flow chart of the recovery and detection of lead of the perovskite solar cell in the invention.
Detailed Description
The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The invention provides a method for recovering lead in a perovskite solar cell, which mainly comprises the following three steps: exfoliation of the battery components, removal of the hole transport layer, and extraction of the lead-containing compound. After the recovery is finished, the recovered product needs to be tested to evaluate the recovery effect and the feasibility of the recovery scheme. The specific process is shown in fig. 2, and includes:
(1) stripping of solar cells
In the step, the substrate material and the conductive glass are peeled off in a manual peeling mode, and the electrode on the top is taken out after the transparent adhesive tape is lightly pressed on the surface of the perovskite solar cell.
(2) Removal of hole transport layer
And immersing the whole perovskite solar cell into ethyl acetate, slowly stirring the solution, taking the perovskite solar cell out of the solution after 1 minute, and drying under nitrogen flow to finish the removal of the hole transport layer. The treatment can selectively remove the hole transport layer without damaging the perovskite thin film. Meanwhile, ethyl acetate is adopted to replace the traditional chlorobenzene as a dissolving agent in the recovery process, so that the pollution of chlorobenzene to water, soil and atmosphere and the harm to human health can be effectively avoided.
(3) Extraction of lead-containing compounds
And soaking the surface of the perovskite solar cell in distilled water for 1 second, and then taking out the perovskite solar cell. The battery taken out is placed in a small-sized tubular heating furnace, then nitrogen flow is introduced into the furnace to exhaust air in the furnace, and the situation that substances in the air in the furnace and the battery are subjected to chemical reaction to influence the recovery effect is prevented. The ventilation time is not suitable to be too long, so that the nitrogen flow is prevented from completely drying the surface of the battery, the moisture on the surface of the battery is ensured to exist, and the drying time is recommended to be 3 minutes in order to catalyze the decomposition process.
Subsequently, the methylamine lead iodide (CH) in the perovskite solar cell is heated to 150 ℃ by a small-sized tubular heating furnace for heat treatment for ten minutes3NH3PbI3) Can be decomposed into PbI2And (3) a solid. After heat treatmentExcept for the electron transport layer in the cell by titanium dioxide (TiO)2) The solid exists, and other substances except lead iodide decomposed from methylamine lead iodine are converted into organic gases, and the organic gases need to be collected and uniformly treated by adopting an organic waste gas treatment method.
Obtaining lead iodide (PbI) after heat treatment2) With titanium dioxide (TiO)2) The solid mixture of (1). Finally, the solid mixture was dissolved in Dimethylformamide (DMF) solvent and stirred, after two minutes, insoluble titanium dioxide solid was removed by filtration, and the DMF solution in which lead iodide was dissolved was placed in a reduced pressure distillation apparatus, as shown in fig. 1.
FIG. 1 shows a distillation part of a vacuum distillation apparatus, which comprises a distillation flask 1, a Kjeldahl head 2, a straight condensation pipe 3, a vacuum connecting pipe 4 and a receiving flask 5. A Kjeldahl head 2 is inserted into a distillation flask 1, a thermometer 7 is inserted into a side port of the Kjeldahl head 2 through a thermo-well tube 6, and a capillary 8 is inserted into a straight port of the distillation flask 1. The Kirschner distillation head can reduce the possibility of splashing into the condenser tube due to bumping of liquid; the capillary tube is used as a gasification center, so that the distillation is stable, and the phenomenon of bumping and rushing out caused by overheating of liquid is avoided; the upper end of the capillary tube is additionally provided with a rubber tube with a spiral clamp for adjusting air inflow, so that a very small amount of air enters liquid to form tiny bubbles during vacuumizing, and the effects of stirring and vaporizing center are achieved; a joint hole 9 is arranged on a bottle plug of the distillation bottle 1, and is used for inserting a measuring joint of a vacuum pressure gauge for measuring the pressure less than the atmospheric pressure into the device so as to measure the air pressure value in the device; two joints on the straight condensing tube 3 are respectively a water inlet and a water outlet of condensed water and are used for cooling DMF gas, and the liquefied DMF solution after cooling is collected through a receiving bottle 5. The vacuum lead-in pipe 4 on the receiving bottle 5 is used for connecting an air pumping system, and a water pump, a circulating water vacuum pump or a vacuum oil pump which are commonly used in a laboratory can be used for air pumping and pressure reduction.
The process condition of the vacuum distillation process is 60 ℃ because many organic compounds including DMF solution can be reduced in boiling point by about 100 ℃ from the boiling point at normal pressure when the pressure is reduced to 1.3kPa (10mmHg), which is also a pressure value that can be achieved by the vacuum distillation apparatus for separating organic compounds and is commonly used. DMF has a boiling point of 153 ℃ and therefore the boiling point becomes 53 ℃ in theory when the pressure is 1.3kPa, and it is more reliable to set the distillation temperature to 60 ℃ in consideration of the fluctuation of the atmospheric pressure.
Because of the reduced pressure distillation, the pressure value is stabilized at about 1.3kPa except the distillation temperature of 60 ℃. The purpose of the design and installation of the joint hole of the vacuum pressure gauge on the bottle plug of the distillation bottle is to stabilize the pressure value at about 1.3kPa by adjusting the air extractor through air pressure measurement.
The distillation process is continued until the liquid is evaporated to dryness, and the solid separated out in the device is pure lead iodide. The vacuum distillation device is used for distillation under the vacuum condition, the boiling point of substances is reduced, the energy consumption can be reduced, the distillation at a lower temperature is realized, the distillation time is shortened, the concentration efficiency is improved, and the decomposition and the damage of lead iodide are avoided. Therefore, the recovery of the lead element of the perovskite solar cell is realized.
(4) Recovery assay
The first step in the detection process is the recovery rate of lead and the recovered PbI2The purity of the solid powder is measured, the measurement methods of the solid powder and the solid powder are similar, and qualitative and quantitative analysis is carried out on the metal elements by an inductively coupled plasma emission spectrometer (ICP-OES). PbI2The microstructure of (a) is detected by using a Scanning Electron Microscope (SEM), and the recovered PbI is subjected to2With common PbI2And (4) placing the product under a microscope for comparison, taking the comparison result as a reference basis for judging whether the recovered product is defective or not, and judging the recovery quality.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for recovering lead in a perovskite solar cell is characterized by comprising the following steps:
1) stripping a substrate material, conductive glass and an electrode of the perovskite solar cell;
2) soaking the stripped perovskite solar cell in a dissolving agent to remove the hole transport layer;
3) the method for extracting the lead-containing compound specifically comprises the following steps:
31) soaking the surface of the perovskite solar cell in distilled water for a certain time, taking out the perovskite solar cell, and drying the perovskite solar cell in a small tubular heating furnace;
32) after drying, heating the small-sized tubular heating furnace to carry out heat treatment on the perovskite solar cell, so that the perovskite solar cell is decomposed into a solid mixture of lead iodide and titanium dioxide and organic gas;
33) soaking a solid mixture of lead iodide and titanium dioxide in a dissolving agent, stirring, and filtering to remove insoluble titanium dioxide to obtain a solution in which lead iodide is dissolved; the dissolving agent is dimethylformamide;
34) and (3) putting the solution dissolved with the lead iodide into a reduced pressure distillation device, setting the distillation temperature at 60 ℃ and the vacuum pressure at 1.3kPa, and continuing until the liquid is evaporated to dryness to separate out pure lead iodide.
2. The method for recycling lead in the perovskite solar cell as claimed in claim 1, wherein in the step 1), the substrate material and the conductive glass of the perovskite solar cell are peeled off by a manual peeling method, and the top electrode is taken out after the surface of the perovskite solar cell is pressed by transparent adhesive.
3. The method for recovering lead in a perovskite solar cell according to claim 1, wherein ethyl acetate is selected as a dissolving agent in the step 2).
4. The method according to claim 3, wherein in the step 2), the whole perovskite solar cell is immersed in ethyl acetate while stirring, and after 1 minute, the perovskite solar cell is taken out from the solvent and dried under a nitrogen stream to complete the removal of the hole transport layer.
5. The method for recovering lead from a perovskite solar cell according to claim 1, wherein in the step 31), the surface of the perovskite solar cell is taken out after being soaked in distilled water for 1 second.
6. The method for recovering lead in the perovskite solar cell as claimed in claim 5, wherein in the step 31), the drying is performed by introducing a nitrogen gas flow into a small-sized tubular heating furnace.
7. The method according to claim 6, wherein the drying time is 3 minutes.
8. The method according to claim 1, wherein in the step 32), the small-sized tubular heating furnace is heated to 150 ℃ for ten minutes.
9. The method for recycling lead in the perovskite solar cell as claimed in claim 1, wherein in the step 34), the distillation device comprises a distillation flask, a Kjeldahl head, a straight condensation pipe, a vacuum lead pipe and a receiving flask; a Kirschner distillation head is inserted on the distillation flask, a thermometer is inserted into the side opening of the Kirschner distillation head through a thermometer sleeve, and a capillary tube is inserted into the straight opening of the distillation flask; the upper end of the capillary tube is additionally provided with a rubber tube with a spiral clamp; the bottle stopper of the distillation bottle is provided with a joint hole for inserting a measuring joint of a vacuum pressure gauge; two joints on the straight condensing pipe are respectively a water inlet and a water outlet of condensed water, and the water outlet is connected with a receiving bottle; and the receiving bottle is provided with a vacuum connecting and leading pipe for connecting an air pumping system.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114871254B (en) * | 2022-04-08 | 2023-02-28 | 西湖大学 | Method for recovering lead iodide and substrate of waste perovskite device |
| CN116997223A (en) * | 2022-04-21 | 2023-11-03 | 杭州纤纳光电科技有限公司 | Lead halide recycling and utilizing method of perovskite solar cell |
| CN114798680A (en) * | 2022-06-27 | 2022-07-29 | 中国华能集团清洁能源技术研究院有限公司 | Recovery processing method of lead-calcium-titanium halide solar cell |
| CN115117184B (en) * | 2022-06-28 | 2024-04-30 | 河海大学 | Method for determining heterojunction solar cell structure to be recovered |
| WO2024077444A1 (en) * | 2022-10-10 | 2024-04-18 | 宁德时代新能源科技股份有限公司 | Method and system for recovering lead iodide from perovskite solar cell |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748812A (en) * | 2016-11-30 | 2017-05-31 | 天津市职业大学 | A kind of new method for preparing perovskite solar cell lead halide methylamine |
| CN109570195A (en) * | 2018-11-27 | 2019-04-05 | 河海大学常州校区 | A kind of double glass construction packages separation and recovery method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748812A (en) * | 2016-11-30 | 2017-05-31 | 天津市职业大学 | A kind of new method for preparing perovskite solar cell lead halide methylamine |
| CN109570195A (en) * | 2018-11-27 | 2019-04-05 | 河海大学常州校区 | A kind of double glass construction packages separation and recovery method |
Non-Patent Citations (1)
| Title |
|---|
| 太阳能电池中钙钛矿薄膜热结晶和热分解研究;徐洁;《万方学位论文》;20190327;正文第26页 * |
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