CN114988464A - Method and device for recycling lead salt from perovskite battery - Google Patents
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- C07C257/10—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines with replacement of the other oxygen atom of the carboxyl group by nitrogen atoms, e.g. amidines
- C07C257/12—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines with replacement of the other oxygen atom of the carboxyl group by nitrogen atoms, e.g. amidines having carbon atoms of amidino groups bound to hydrogen atoms
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Abstract
The invention provides a method and a device for recycling lead salt from a perovskite battery, and relates to the technical field of resource recycling. The method comprises the following steps: adding deionized water into the perovskite battery waste liquid, stirring uniformly to obtain a suspension, adding glacial acetic acid, heating the suspension in a water bath until orange yellow precipitates are completely settled to the bottom, washing and drying to obtain purified lead iodide crystals, mixing the purified lead iodide crystals with formamidine hydroiodide, dissolving the purified lead iodide crystals in a solvent, and synthesizing to obtain perovskite crystal powder; weighing perovskite crystal powder to prepare perovskite precursor solution for later use. The method can recover and obtain lead iodide from the perovskite battery, further synthesize the recovered lead iodide into perovskite crystal powder which can be used as a raw material of the perovskite battery, realize closed loop of recovery-purification-reutilization of perovskite waste liquid, and have the advantages of simple process, economy, environmental protection, high recovery rate and cost reduction.
Description
Technical Field
The invention belongs to the technical field of resource recycling, and particularly relates to a method and a device for recycling lead salt from a perovskite battery.
Background
With the technical progress of stability and large-area preparation, perovskite batteries are rapidly advancing toward industrialization. The common perovskite preparation technology at present is scraper, spraying or slit coating, and the consumption of perovskite precursor solution in the process is large. But a large amount of waste liquid is generated in the process of preparation, use and storage.
The main components of the waste liquid are aprotic polar solvent including N, N-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), gamma-butyrolactone (GBL), ethylene glycol formamidine (2-ME), Acetonitrile (ACN), etc., and perovskite precursor solute including lead ion (Pb) 2+ ) Methylamine (MA), Formamidine (FA), Guanidine (GA), cesium ions (Cs) + ) And the like. The waste liquid has high pollution and needs special treatment; and the waste liquid also contains a large amount of recoverable metal ions.
As a heavy metal element, the lead has the advantages of low melting point, high corrosion resistance, difficult penetration of X rays, gamma rays and the like, good plasticity and the like, and has wide application, and the lead and the compound thereof are applied to the fields of metallurgy, storage batteries, printing, pigments, paint, glaze, soldering tin and the like.
At present, halide perovskites used in photovoltaic devices have the general formula ABX 3 Wherein A is typically an organic amine ion or cesium ion, X is a halide ion, and B is a divalent metal ion, typically Pb 2+ . The three ions form cubic arrangement, and metal ions and halogen ions need to form octahedrons to form a three-dimensional frame, so that the size of the ions has a significant influence. The lead ion 6s track has lone pair electrons and the 6p track is inactive, and the cubic phase perovskite has high symmetry, so that the electronic dimensionality is high, and the perovskite current carrier has long service life and long diffusion length, and is very suitable for being applied to the photovoltaic field.
At the present stage, the perovskite material which is most widely produced in the industrialized production and has the best performance is lead-halogen perovskite, and the lead-halogen perovskite has a series of excellent comprehensive performances of strong light absorption capacity, high photocurrent transmission speed, high defect tolerance and the like.
But also brings corresponding problems, and lead as a toxic heavy metal is leaked in the environment to influence the environment and human body.
The perovskite material has a certain possibility of heavy metal pollution in the production process, and although the pollution can be reduced by optimizing the production process control, the pollution also means more complicated production process and byproduct treatment process and higher cost.
Meanwhile, as an ionic crystal material, different materials and structures in the perovskite material may have the defects of no high temperature resistance, no illumination resistance, easy hydrolysis, easy oxidation, easy secondary reaction and the like. The perovskite cells have a short average service life and a high rate of decay of the overall cell, and there is also the potential for efficiency sacrifice if additional protective measures are taken, such as protective coatings or doping.
Toxic lead is recycled from the waste materials of the perovskite solar module, so that the effects of protecting the environment and creating economic benefits from the recycled materials are achieved.
There are some technical solutions in the field for the recovery of lead, but they still have some drawbacks.
For example, patent CN 107513618A discloses a lead recycling method for perovskite battery, which comprises adding the lead-containing separation solution and a precipitating agent into a region surrounded by a plastic film for precipitation, and then removing the plastic film for precipitation separation; the precipitant is selected from sodium sulfide or potassium sulfide. The PbS sediment obtained by adding sulfide is stable in product, difficult to be converted into other lead salts and narrow in application range.
Patent CN 215365312U discloses a perovskite battery industry waste liquid processing system, including waste liquid jar, first retort, second retort and solid collecting tank. The organic solvent is removed by fractional distillation, and the lead-containing mixture with mixed components, including lead iodide and multi-phase perovskite, cannot be directly utilized.
Patent CN 113264838A discloses a method for recovering perovskite from waste perovskite, which comprises (1) treating waste perovskite devices by low-boiling-point chain amines until the waste perovskite is completely dissolved and taken out; (2) putting the substrate into new low-boiling-point amine for cleaning and repeated treatment, and recycling the substrate after the evaporation surface is dissolved; (3) pouring the waste liquid obtained in the step (2) into the waste liquid obtained in the step (1), mixing and standing for a certain time, and filtering the standing waste liquid to separate suspended particles or precipitates from the waste liquid; (4) the obtained waste liquid is heated according to the boiling point of the amine to evaporate the redundant amine to obtain the perovskite, the amine raw material adopted by the perovskite is dissolved with the perovskite, and the perovskite component in the waste perovskite battery is not suitable to be used as the raw material of the solar battery after being exposed and degraded, so the perovskite recovered by the method cannot be directly used.
Patent CN 111434614 a discloses a method for recovering and purifying lead iodide, which is to perform recovery treatment of lead iodide for perovskite precursor waste solution containing lead iodide components. The perovskite waste liquid is primarily treated by water or alcohols, filter residues are redissolved by DMSO, and a lead iodide product is obtained by reduced pressure distillation, wherein the DMSO has a high boiling point, and the reduced pressure distillation has high energy consumption.
In view of the above, it is an urgent technical problem to provide a method and apparatus for recovering and recycling lead salt from a perovskite battery.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method and a device for recycling lead salt from a perovskite battery, which can recycle lead iodide from the perovskite battery and further synthesize the recycled lead iodide into perovskite crystal powder which can be used as a raw material of the perovskite battery.
A method for recycling lead salt from waste liquid of a perovskite battery comprises the following steps:
(1) adding deionized water into the perovskite battery waste liquid, and uniformly stirring to obtain a suspension;
(2) adding glacial acetic acid into the suspension obtained in the step (1), and heating the suspension in a water bath until all orange-yellow precipitates are settled to the bottom;
(3) filtering the orange-yellow precipitate in the step (2), washing and drying the orange-yellow precipitate to obtain purified lead iodide crystals;
(4) mixing the purified lead iodide crystal in the step (3) with formamidine hydroiodide, dissolving in a solvent, and synthesizing to obtain perovskite crystal powder;
(5) weighing the perovskite crystal powder in the step (4) to prepare a perovskite precursor solution for later use.
Further, the method also comprises the step of preparing the perovskite battery waste liquid, and comprises the following steps:
obtaining solid waste of the perovskite battery, and crushing the perovskite battery to form fragments; and soaking the fragments in a soaking solution, and filtering to obtain the perovskite battery waste liquid.
The device further comprises a perovskite battery recycling device, wherein the perovskite battery recycling device comprises a perovskite waste solid soaking pool and a reaction container;
the perovskite waste solid soaking pool is used for soaking perovskite battery solid waste to obtain perovskite battery waste liquid;
the perovskite waste solid soaking pool is communicated with the reaction container through a perovskite waste liquid feeding pipe; the perovskite waste liquid feeding pipe is used for guiding perovskite battery waste liquid in the perovskite waste solid soaking pool into the reaction container;
the reaction vessel is provided with a material feeding pipe, and the material feeding pipe is used for guiding liquid materials into the reaction vessel.
Furthermore, a grid structure capable of moving up and down is arranged in the waste solid soaking pool for removing insoluble substances in the waste liquid of perovskite.
Further, a heating structure is arranged in the reaction container and used for heating liquid in the reaction container.
Further, a stirring structure is arranged in the reaction container and used for stirring liquid in the reaction container.
Further, a condensation pipe is arranged at the top end of the reaction container and used for condensing gasified liquid.
Further, a filtering structure is arranged at the bottom of the reaction container; the filter structure is used to separate solids and liquids.
Further, the filtering structure is connected with the reaction container through a communicating valve; the filtering structure is communicated with the reaction container when the communicating valve is opened; and when the communicating valve is closed, the filtering structure is not communicated with the reaction container.
Further, the filtering structure comprises a filter screen and a liquid discharge pipe;
wherein the screen is used to separate solids and liquids;
the liquid discharge pipe is used for discharging liquid.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages and positive effects as examples:
the method can recover and obtain lead iodide from the perovskite battery, further synthesize the recovered lead iodide into perovskite crystal powder which can be used as a raw material of the perovskite battery, and has the advantages of simple process, economy, environmental protection and high recovery rate.
In addition, the method does not need reduced pressure distillation or extra addition of a precipitator, does not additionally use a toxic organic solvent based on the property of the perovskite waste liquid, and is environment-friendly and energy-saving. The closed loop of recycling, purifying and reusing the perovskite waste liquid can be realized, and the cost is reduced.
Drawings
Fig. 1 is a schematic structural diagram of the apparatus for recycling lead salt from a perovskite battery provided by the invention.
Fig. 2 is an XRD spectrum of the lead iodide crystal powder obtained in example 1.
Fig. 3 is an SEM photograph of the lead iodide crystal powder obtained in example 1.
FIG. 4 shows alpha-FAPbI obtained in example 1 3 XRD pattern of crystal powder.
FIG. 5 is a flowchart of the operation of example 2.
Description of reference numerals:
the recycling device 100 for the perovskite battery, a perovskite waste solid soaking pool 110, a grid structure 111, a rod body 112, a connecting piece 113, a perovskite waste liquid feeding pipe 120, a reaction container 130, an air condensation pipe 131, a heating structure 132, a stirring structure 133, a material feeding pipe 140, a communication valve 150, a filtering structure 160, a filter cloth 161 and a filtrate discharging pipe 162.
Detailed Description
The technical solution disclosed in the present invention is described in detail below with reference to specific examples.
Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values.
The invention provides a method for recycling lead salt from waste liquid of a perovskite battery, which comprises the following steps:
(1) and adding deionized water into the perovskite battery waste liquid, and uniformly stirring to obtain a suspension.
(2) And (3) adding glacial acetic acid into the suspension obtained in the step (1), and heating the suspension in a water bath until all orange yellow precipitates are settled to the bottom.
In step (2), the hydrolysis of lead is inhibited by adding glacial acetic acid.
(3) And (3) filtering the orange-yellow precipitate in the step (2), and washing and drying the orange-yellow precipitate to obtain purified lead iodide crystals.
(4) And (4) mixing and dissolving the purified lead iodide crystals obtained in the step (3) and formamidine hydroiodide in a solvent to synthesize perovskite crystal powder.
In the step (4), by way of example and not limitation, perovskite crystal powder is obtained by reverse temperature crystallization, solid-liquid reaction, or antisolvent precipitation.
(5) Weighing the perovskite crystal powder in the step (4) to prepare a perovskite precursor solution for later use.
The perovskite battery waste liquid referred by the invention can be perovskite battery waste liquid generated in the production process; or the waste liquid of the perovskite battery obtained by treating the waste perovskite battery piece and/or the solid waste of the perovskite battery.
The method for recycling the lead salt from the perovskite battery waste liquid further comprises the step of preparing the perovskite battery waste liquid, and comprises the following steps:
obtaining solid waste of the perovskite battery, and crushing the perovskite battery to form fragments; and soaking the fragments in a soaking solution, and filtering to obtain the perovskite battery waste liquid.
The soaking solution includes but is not limited to DMF, DMSO, GBL, 2-ME.
The method for recycling lead salt from the perovskite battery waste liquid further comprises a perovskite battery recycling device 100, wherein the perovskite battery recycling device comprises a perovskite waste solid soaking pool 110 and a reaction container 130. As an example of a typical structure, refer to fig. 1.
The perovskite waste solid soaking pool 110 is used for soaking perovskite battery solid waste to obtain perovskite battery waste liquid.
The perovskite waste solid soaking pool is internally provided with a grid structure 111 capable of moving up and down, and the grid structure 111 is used for removing insoluble substances in the perovskite waste liquid.
By way of example and not limitation, as shown in fig. 1, the grid structure is a basket-shaped structure, and the bottom is a grid, so that the grid has a function of filtering liquid. The top department of useless solid fermentation vat of perovskite is provided with the body of rod 112 that extends to the bottom, and the cover is equipped with annular connecting piece 113 on the body of rod 112, and the internal diameter of connecting piece 113 is greater than the external diameter of the body of rod 112, reciprocates on the body of rod through the motor control connecting piece that sets up in the inside of the body of rod 112. The grid structure is arranged on the connecting piece, and the connecting piece drives the grid structure to move up and down on the rod body 112, so that the grid structure 111 can move up and down in the titanium ore waste solid soaking pool.
During specific implementation, the solid waste of the perovskite battery is placed in the grid structure 111, the grid structure 111 moves downwards and is immersed in the immersion liquid placed in the perovskite waste solid immersion tank 110 to be immersed, and perovskite battery waste liquid is obtained. After soaking, lattice construction 111 moves upwards for the waste material breaks away from perovskite battery waste liquid.
The perovskite waste solid soaking pool is characterized in that the perovskite waste solid soaking pool is provided with clamping grooves, clamping teeth are arranged on the side faces of the perovskite waste solid soaking pool, and the mesh structure can move up and down in the perovskite waste solid soaking pool through the matching of the clamping teeth and the clamping grooves.
The perovskite waste solid soaking pool 110 is communicated with the reaction container 130 through a perovskite waste liquid feeding pipe 120; the perovskite waste liquid inlet pipe is used for guiding perovskite battery waste liquid in the perovskite waste solid soaking pool into the reaction container.
A material feed pipe 140 is provided on the reaction vessel for introducing liquid material into the reaction vessel.
The liquid material enters a reaction container to react with the waste liquid of the perovskite battery. The liquid material in this embodiment includes, but is not limited to, acetic acid and/or water.
The reaction vessel 130 is provided with a heating structure 132 for heating the liquid in the reaction vessel. By way of example and not limitation, the heating structure may be provided in two, respectively on both side walls of the reaction vessel.
A stirring structure 133 is disposed in the reaction vessel, and is used for stirring the liquid in the reaction vessel. By way of example and not limitation, the stirring structure is a motor-driven stirring bar capable of continuously stirring blood at a uniform speed. Both the stirring speed of the stirring structure 133 and the heating temperature of the heating structure 132 can be adjusted by providing an external knob or button.
The top of the reaction vessel is provided with a condensing pipe 131, and the condensing pipe 131 is used for condensing the gasified liquid. The vaporized liquid herein refers to vaporized acetic acid and water vapor in the reaction vessel by way of example and not limitation. The number of the condensation duct 131 is not limited, and a plurality thereof may be provided.
The bottom of the reaction vessel is provided with a filtering structure 160; the filter structure is used to separate solids and liquids. By way of example and not limitation, the filtering structure may be a funnel structure with a wide top and a narrow bottom, as shown in fig. 1. Other structures that do not employ a funnel structure, such as a rectangular parallelepiped, a sphere, etc., are also possible.
The filtering structure is connected with the reaction vessel through a communicating valve 150; and the filtering structure is not communicated with the reaction container when the communicating valve is closed. When the communicating valve is opened, the filtering structure is communicated with the reaction container, and when the communicating valve is communicated with the reaction container, liquid and solid in the reaction container enter the filtering structure below through the communicating valve.
The filter structure 160 includes a filter cloth 161 and a liquid discharge pipe 162; wherein the filter cloth is used for separating solids and liquids; the liquid discharge pipe is used for discharging liquid.
Example 1
100mL of perovskite waste liquid is taken, 500-1000mL of deionized water is added into the perovskite waste liquid to form yellow suspension, and 50mL of glacial acetic acid is added into the yellow suspension.
And heating the yellow suspension at 100 ℃ for 3 hours until the precipitate is settled to the bottom of the reaction vessel to obtain orange yellow crystals with uniform size, filtering the orange yellow crystals while the orange yellow crystals are hot, and washing the orange yellow crystals with deionized water for 3-5 times to obtain purified lead iodide crystals. Fig. 2 is an XRD spectrum of the lead iodide crystal powder obtained in this example. Fig. 3 is an SEM photograph of the lead iodide crystal powder obtained in this example.
Lead iodide and formamidine hydroiodide in equal molar ratio were mixed in a mixed solvent of 2-ME ACN (v: v ═ 3:2), stirred at room temperature for 6 hours, and then filtered, and the resulting clear filtrate was heated at 80 ℃ for 1 hour to obtain a black perovskite crystal powder.
Filtered while hot and washed three times with IPA or ACN and dried to give optically active alpha-FAPbI 3 crystalline powder. FIG. 4 shows α -FAPBI obtained in this embodiment 3 XRD pattern of crystal powder.
The perovskite precursor can be obtained by dissolving the crystal powder in DMF, DMSO, GBL, 2-ME or methylamine ethanol solution.
The perovskite precursor can be further prepared into a perovskite thin film by means including but not limited to spin coating, blade coating, slit coating, spray coating and the like.
Example 2
The overall operational flow diagram is shown in fig. 5. Firstly, obtaining waste solid fragments of invalid perovskite, crushing the waste solid fragments by using a blunt instrument, and adding a quantitative DMF solvent into the crushed solid fragments to soak the crushed solid fragments to obtain waste perovskite liquid.
Deionized water and acetic acid were then added to the waste stream. Specifically, 100mL of the perovskite waste liquid is added with 500-1000mL of deionized water to form a yellow suspension immediately, and 50mL of glacial acetic acid is added into the yellow suspension.
The suspension was heated at 100 ℃ for 3 hours to obtain orange yellow crystals of uniform size at the bottom of the flask, i.e., lead iodide crystals, which were then filtered while hot. And washing with deionized water for 3-5 times, and drying to obtain purified lead iodide crystal.
And then adding iodoformamidine to synthesize perovskite crystal powder. Specifically, lead iodide and formamidine hydroiodide were mixed at an equal molar ratio, added to a mixed solvent of 2-ME: ACN (v: 3:2), stirred at room temperature for 6 hours, and then filtered, and the resulting clear filtrate was heated at 80 ℃ for 1 hour to obtain a black perovskite crystal powder.
The black perovskite crystal powder is filtered while hot and washed three times with IPA or ACN and dried to give optically active black alpha-FAPBI 3 A crystalline powder;
the crystal powder is dissolved in DMF, DMSO, GBL, 2-ME or methylamine ethanol solution and the like to prepare perovskite precursor solution.
And preparing the perovskite precursor into the perovskite thin film by means including but not limited to spin coating, blade coating, slit coating or spray coating.
Terms like "comprising" and "comprises" should be interpreted as inclusive or open-ended, rather than exclusive or closed-ended, within the scope of the intended protection of the present disclosure, unless explicitly defined to the contrary. All technical, scientific, or other terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs unless defined otherwise. Common terms found in dictionaries should not be interpreted too ideally or too realistically in the context of related art documents unless the present disclosure expressly limits them to that.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A method for recycling lead salt from perovskite battery waste liquid is characterized by comprising the following steps:
(1) adding deionized water into the perovskite battery waste liquid, and uniformly stirring to obtain a suspension;
(2) adding glacial acetic acid into the suspension obtained in the step (1), and heating the suspension in a water bath until all orange-yellow precipitates are settled to the bottom;
(3) filtering the orange-yellow precipitate in the step (2), washing and drying the orange-yellow precipitate to obtain purified lead iodide crystals;
(4) mixing the purified lead iodide crystal in the step (3) with formamidine hydroiodide, dissolving in a solvent, and synthesizing to obtain perovskite crystal powder;
(5) weighing the perovskite crystal powder in the step (4) to prepare a perovskite precursor solution for later use.
2. The method of claim 1, further comprising the step of producing a perovskite battery effluent as follows:
obtaining solid waste of the perovskite battery, and crushing the perovskite battery to form fragments; and soaking the fragments in a soaking solution, and filtering to obtain the perovskite battery waste liquid.
3. The method according to claim 1, further comprising a perovskite battery recycling device, wherein the perovskite battery recycling device comprises a perovskite waste solid soaking pool and a reaction container;
the perovskite waste solid soaking pool is used for soaking perovskite battery solid waste to obtain perovskite battery waste liquid;
the perovskite waste solid soaking pool is communicated with the reaction container through a perovskite waste liquid feeding pipe; the perovskite waste liquid feeding pipe is used for guiding perovskite battery waste liquid in the perovskite waste solid soaking pool into the reaction container;
the reaction vessel is provided with a material feeding pipe, and the material feeding pipe is used for guiding liquid materials into the reaction vessel.
4. An apparatus for recycling lead salts from perovskite cells as claimed in claim 3 wherein: the perovskite waste solid soaking pool is internally provided with a grid structure which can move up and down and is used for removing insoluble substances in the perovskite waste liquid.
5. An apparatus for recycling lead salts from perovskite cells as claimed in claim 3 wherein: and a heating structure is arranged in the reaction container and used for heating liquid in the reaction container.
6. An apparatus for recycling lead salts from perovskite cells as claimed in claim 3 wherein: and a stirring structure is arranged in the reaction container and is used for stirring liquid in the reaction container.
7. An apparatus for recycling lead salts from perovskite cells as claimed in claim 3 wherein: the top end of the reaction vessel is provided with a condensing tube which is used for condensing gasified liquid.
8. An apparatus for recycling lead salts from perovskite cells as claimed in claim 3 wherein: the bottom of the reaction container is provided with a filtering structure; the filter structure is used to separate solids and liquids.
9. An apparatus for recycling lead salts from perovskite cells as claimed in claim 8, wherein: the filtering structure is connected with the reaction container through a communicating valve; the filtering structure is communicated with the reaction container when the communicating valve is opened; and the filtering structure is not communicated with the reaction container when the communicating valve is closed.
10. An apparatus for recycling lead salts from perovskite cells as claimed in claim 8, wherein: the filtering structure comprises a filter screen and a liquid discharge pipe;
wherein the screen is used to separate solids and liquids;
the liquid discharge pipe is used for discharging liquid.
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| 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 |
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| CN107513618A (en) * | 2017-08-01 | 2017-12-26 | 苏州协鑫纳米科技有限公司 | The lead recovery method and device of perovskite battery |
| CN111434614A (en) * | 2019-08-21 | 2020-07-21 | 杭州纤纳光电科技有限公司 | Method for recovering and purifying lead iodide |
| CN113845428A (en) * | 2021-09-10 | 2021-12-28 | 中国科学院上海光学精密机械研究所 | Preparation method of perovskite material powder |
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| 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 |
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