CN106876597A - The device recycling of degraded perovskite solar cell and recycling technique - Google Patents
The device recycling of degraded perovskite solar cell and recycling technique Download PDFInfo
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- CN106876597A CN106876597A CN201710102252.9A CN201710102252A CN106876597A CN 106876597 A CN106876597 A CN 106876597A CN 201710102252 A CN201710102252 A CN 201710102252A CN 106876597 A CN106876597 A CN 106876597A
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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
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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
- 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
Abstract
The invention discloses it is a kind of degrade or discarded perovskite solar cell device recycling with recycle technique, including the degraded preliminary cleaning treatment of perovskite solar cell device, the thoroughly cleaning of gained substrate and treatment, substrate are used for the waste liquid for preparing solar cell device again, produce（The mixed organic solvents and suspension or precipitation of each functional layer chemical constituent）Preliminary treatment with the further treatment of the waste liquid for obtaining back electrode metal material, producing obtaining participating in the lead halide of new round device preparation.Wet processing of the present invention has the advantages that low temperature, low power consuming, lead can be avoided to be lost in the potential threat caused to environmental ecology and health of human body, can realize to the abundant of resource and recycle again, with potential good economic benefit, the practical of cheap perovskite solar cell can be pushed further into.
Description
Technical field
Device recycling and recycling technique the present invention relates to discard perovskite solar cell are a kind of based on solution
The Low temperature processing techniques of method, prepared by category solar cell and resource reclaim recycles field.
Background technology
Organic inorganic hybridization based semiconductor material has the good mechanical flexibility of organic component and inorganic component load higher concurrently
The advantage of transport factor is flowed, the photoelectronics parameter such as band gap can be adjusted by introducing appropriate different organic and inorganic component,
It is particularly suitable for being prepared by wet coating technique the opto-electronic device of large area.Among these, organic inorganic hybridization perovskite
Semi-conducting material CH3NH3PbX3(X=Cl, Br, I) and its it is various doping deformable material then because its suitable band gap and it is higher and
The excellent photoelectronic property such as the electronics and hole mobility of balance and turn into the focus material in solar cell field.Based on such
The solar cell device efficiency of material rises violently by 2016 more than 22% by the development of short time from 3.8% in 2009, fills
Divide and show great potential of such material in terms of the cheap solar cell of large area is realized.
Current efficiency highest perovskite solar cell generally uses the perovskite material containing lead element, such as methylamine lead iodine
（CH3NH3PbI3）And its halogen substituents methylamine lead bromine（CH3NH3PbBr3）Or methylamine lead iodine chlorine（CH3NH3PbI3-xClx）And
Organic component substituent carbonamidine lead iodine（NH2CH=NH2PbI3）Etc., it is contemplated that the toxicity of lead is to ecological environment and health of human body
Potential threat, the research work of lead substitution perovskite material is quite a few, such as on CH3NH3SnI3Report.But it is all these
The device efficiency that work is given all can not be compared with lead-based perovskite device.The excellent characteristic of perovskite comes from the s rails of lead element
Road is coupled with the strong antibonding of the p tracks of I, therefore the substitution of lead is very difficult.So, currently for lead-based perovskite
The research of solar cell is in the majority.It is contemplated that, the emphasis of the emphasis studied from now on, particularly efficiency may proceed to rest on lead
On based perovskite solar cell.
For solar cell, the energy acquiring way of cleanliness without any pollution is the original intention of people's research.The presence of lead is finished
Unexpectedly make us worry.There is group to specialize in lead-based perovskite to ecological environment and the potential threat of health of human body.This
It must be very careful to remind our utilizations to lead, to prevent the loss of lead.In addition, with the whole world research perovskite sun
The group of battery is more and more, and each laboratory can produce the device of many degradeds, may finally be taken as solid refuse and give up
Gurry is lost, and this can cause environmental pollution.Even if having the special Collection and conservation of experimenter these discarded devices, these solid refuses
Treatment be also cumbersome, these problems will after particularly following perovskite solar cell realizes large area practical application
It is more serious.There are recovery and the processing mechanism of lead accumulator at present, but the recovery of perovskite solar cell and treatment are also
It is blank.
A kind of recycle and reuse technique of the waste and old degraded device of perovskite solar cell of invention.The technique is not
Transparent conducting glass can only be re-used（Such as FTO）Or transparent conducting glass/titanium dioxide substrate, and reclaimed lead and
The heavy metals such as silver/gold and noble metal back electrode material, while the double effects of the feature of environmental protection and resources conservation are realized, with latent
Considerable economic benefit, be expected to further reduce manufacturing cost and the cost recovery cycle of perovskite solar cell, so as to promote
Entering perovskite solar cell turns into real clean energy resource and for the development of human society contributes.
The content of the invention
Recovery and the blank of handling process for the lead-based perovskite solar cell degraded at present and discard, in order to avoid
Environmental pollution and recycling for resource is realized, spy proposes based on cryogenic fluid treatment degraded perovskite solar cell and realizes
The technique of the recycling of substrate.
The recycling of degraded perovskite solar cell and recycling technique, it is characterised in that：Using low temperature solution polycondensation, bag
Include following steps：
（1）The preliminary cleaning treatment of waste battery device：Using dimethylformamide（N, N-Dimethylformamide, DMF）
Or dimethyl sulfoxide (DMSO) (Dimethyl sulfoxide, DMSO) such as is rinsed, soaks at the treatment to device；
（2）The thoroughly cleaning of substrate and treatment：To step（1）Gained substrate is carried out using DMF, chlorobenzene, deionized water etc. successively
Immersion, ultrasonic cleaning, UV ozone treatment.If necessary, titanium tetrachloride treatment is also carried out（70 DEG C, 30 minutes）And sintering；
（3）The re-using of substrate：It is prepared by the device for carrying out a new round using above-mentioned gained substrate.
（4）The preliminary treatment of the waste liquid of generation：To step（1）Each functional layer chemical constituent produced after flushing and immersion
Mixed solution carry out being filtrated to get the back electrode film such as argent or gold, collecting these metals can be with plus appropriate purification processes
Again it is used to prepare battery.
（5）The further treatment of the waste liquid of generation：To step（4）Dividing for each chemical constituent is carried out through the waste liquid of preliminary treatment
From, purification and lead iodide preparation with for new round device prepare etc..The equation of the main chemical reaction being related to is：
(CH3COO)2Pb + 2KX → 2(CH3COO)K + PbX2↓
X represents the halogens such as iodine or bromine in formula.
Brief description of the drawings
Fig. 1 is device recycling and the recycling process chart of present invention degraded perovskite solar cell；
Fig. 2 is the samples devices for processing（It is left）And the transparent conducting glass substrate obtained after treatment（It is right）；
Fig. 3 is original（On）, after one cycle（In）And after circulating twice（Under）Transparent conductive glass surface SEM schemes
Picture；
Fig. 4 is after original, one cycle and the Ultraviolet visible absorption spectrum of transparent conducting glass after circulating twice；
Fig. 5 is after original, one cycle and the XRD spectra of transparent conducting glass after circulating twice；
Fig. 6 is that the perovskite being sequentially deposited on after original, one cycle and after circulating twice transparent conducting glass is thin
The Ultraviolet visible absorption spectrum of film；
Fig. 7 is that the perovskite being sequentially deposited on after original, one cycle and after circulating twice transparent conducting glass is thin
The XRD spectra of film；
Fig. 8 be sequentially prepared it is after original, one cycle and twice circulate after transparent conducting glass on perovskite too
Positive electricity pondJ-VCharacteristic curve.
Specific embodiment
The present invention is further illustrated with reference to embodiments, but the present invention is not limited to embodiment described below.
Embodiment 1, device recycling and recycling technique without electron transfer layer planar structure perovskite solar cell：
The discarded device architecture without electron transfer layer perovskite solar cell involved by the present embodiment is transparent conducting glass/calcium
Titanium ore/hole transmission layer/back electrode and its any type of deformation, device recycling and recycling technological process such as Fig. 1 institutes
Show, the device for containing degraded perovskite solar cell is collected, preliminary to clean to obtain transparent conducting glass（Such as FTO, ITO,
AZO etc.）With the mixed solution and suspension of each functional layer chemical constituent of device, further to the thoroughly cleaning of substrate and treatment with
Prepare the device of a new round, the recycling of back electrode, the separation of the mixed solution of each functional layer chemical constituent of device, purification
And lead halide obtain with for new round device prepare etc. detailed step.
Fig. 2 gives the preliminary cleaning treatment and resulting transparent conducting glass photo to device of degrading.
Fig. 3 illustrates original（1）, one cycle uses（2）And recycle twice（3）Transparent conducting glass
Surface Scanning Electron microscope（SEM）Image.
Fig. 4 is that transparent conducting glass that is that original, one cycle is used and recycling twice and its electrically conducting transparent are thin
The ultraviolet-visible absorption collection of illustrative plates of film.
Fig. 5 is the transparent conductive film of transparent conducting glass that is that original, one cycle is used and recycling twice
X-ray diffraction（XRD）Collection of illustrative plates.
Fig. 6 is the calcium of the preparation on transparent conducting glass being used in original, one cycle and recycling twice
The ultraviolet-visible absorption collection of illustrative plates of titanium ore film.
Fig. 7 is the calcium of the preparation on transparent conducting glass being used in original, one cycle and recycling twice
The X-ray diffraction of titanium ore film（XRD）Collection of illustrative plates.
Fig. 8 is the nothing of the preparation on transparent conducting glass being used in original, one cycle and recycling twice
Electron transfer layer planar structure perovskite solar cellJ-VCharacteristic curve.
Embodiment 2, device recycling and the recycling technique of classical planar heterojunction structure perovskite solar cell：
The device architecture of the discarded planar heterojunction structure perovskite solar cell involved by the present embodiment be transparent conducting glass/
Electron transfer layer/perovskite/hole transmission layer/back electrode and its any type of deformation, device recycling and recycling work
The device that skill flow contains degraded perovskite solar cell is collected, preliminary to clean to obtain transparent conducting glass（This is directed to
The device of electron transfer layer or cathodic modification layer is made using organic solvent or water-soluble strong organic material）Or electrically conducting transparent glass
Glass/electron transfer layer（Such as FTO/TiO2, this is directed to using the inorganic material for having well attached characteristic with transparent conducting glass substrate
Material makees the device of electron transfer layer or cathodic modification layer）With the mixed solution and suspension of each functional layer chemical constituent of device, enter
One step is to the thoroughly cleaning of substrate and treatment preparing the device of a new round, the recycling of back electrode, each functional layer of device
The obtaining of the separation of the mixed solution of chemical constituent, purification and lead halide the detailed step such as prepares with for new round device.
Embodiment 3, device recycling and the recycling technique of meso-hole structure perovskite solar cell：
The device architecture of the discarded meso-hole structure perovskite solar cell involved by the present embodiment is transparent conducting glass/densification electricity
Sub- transport layer/meso-hole structure electron transfer layer/perovskite/hole transmission layer/back electrode and its any type of deformation, device are returned
Receive treatment and recycle the device that technological process contains degraded perovskite solar cell to collect, it is preliminary to clean to obtain transparent leading
Electric glass/densification electron transfer layer/meso-hole structure electron transfer layer（Such as FTO/ densifications TiO2/ mesoporous TiO2, this is directed to use
The inorganic material for having well attached characteristic with transparent conducting glass substrate makees the device of electron transfer layer or cathodic modification layer）And device
The mixed solution and suspension of each functional layer chemical constituent of part, further to the thoroughly cleaning of substrate and treatment preparing a new round
Device, the recycling of back electrode, the separation of the mixed solution of each functional layer chemical constituent of device, purification and lead halide
Obtain with for new round device prepare etc. detailed step.
In addition, for reverse mould transparent conducting glass/PEDOT:PSS/ perovskites/electron transfer layer/back electrode and its any
The perovskite solar cell of the distressed structure of form and with transparent conducting glass/electron transfer layer/perovskite/back electrode structure
Without hole transport layer device and its any type of deformation, recycle and reuse technique involved in the present invention can also have very
Good effect, these ought to be claimed content of the invention.
Claims (7)
1. the device of degraded perovskite solar cell is recycled and recycles technique, it is characterised in that：Using low temperature solution polycondensation,
Comprise the following steps：
（1）The preliminary cleaning treatment of degraded perovskite solar cell device：Using dimethylformamide（N,N-
Dimethylformamide, DMF）Or the highly polar organic solvent pair such as dimethyl sulfoxide (DMSO) (Dimethyl sulfoxide, DMSO)
Device such as is rinsed, soaks at the treatment；
（2）The thoroughly cleaning of substrate and treatment：To step（1）Gained substrate is carried out using DMF, chlorobenzene, deionized water etc. successively
Immersion, ultrasonic cleaning, UV ozone treatment.If necessary, titanium tetrachloride treatment is also carried out（70 DEG C, 30 minutes）And sintering；
（3）Substrate is used to prepare solar cell device again：It is prepared by the device for carrying out a new round using above-mentioned gained substrate；
（4）The waste liquid of generation（The mixed organic solvents and suspension or precipitation of each functional layer chemical constituent）Preliminary treatment with
To back electrode metal material：To step（1）The mixing of each functional layer chemical constituent produced after substrate is rinsed and soaked is molten
Liquid carries out being filtrated to get the back electrode film such as argent or gold, and collecting these metal materials can be again plus appropriate purification processes
It is used to prepare battery；
（5）The further treatment of the waste liquid of generation is obtaining participating in the lead halide of new round device preparation：To step（4）Through
Waste liquid obtained by preliminary treatment carries out separation, purification and the preparation of lead iodide of each chemical constituent and participates in the device of a new round
In the middle of preparing.
2. the device recycling of discarded perovskite solar cell as claimed in claim 1 exists with technique, its feature is recycled
In：Wet-treating is carried out to degraded device using low temperature solution polycondensation.
3. the recycling of perovskite solar cell is discarded as claimed in claim 1 and recycles technique, it is characterised in that：Step
Suddenly（1）Using dimethylformamide（N, N-Dimethylformamide, DMF）Or dimethyl sulfoxide (DMSO) (Dimethyl
Sulfoxide, DMSO) etc. can dissolve each functional layer can particularly dissolve perovskite material highly polar organic solvent make
It is effective device cleaning treatment solvent.
4. the recycling of perovskite solar cell is discarded as claimed in claim 1 and recycles technique, it is characterised in that：Step
Suddenly（2）Using DMF, chlorobenzene, deionized water equal solvent, the temperature and time of titanium tetrachloride treatment is 70 DEG C and 30 minutes.
5. the recycling of perovskite solar cell is discarded as claimed in claim 1 and recycles technique, it is characterised in that：Step
Suddenly（4）Using be filtrated to get back electrode metal material and for new device preparation.
6. the recycling of perovskite solar cell is discarded as claimed in claim 1 and recycles technique, it is characterised in that：Step
Suddenly（5）The techniques such as separation, purification are used to prepare lead halide.
7. the recycling of perovskite solar cell is discarded as claimed in claim 1 and recycles technique, it is characterised in that：Step
Suddenly（5）The solution of middle gained is using reaction：(CH3COO)2Pb + 2KX → 2(CH3COO)K + PbX2↓（X is halogen unit in formula
Element）Prepared to the device of a new round to prepare lead halide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610208780 | 2016-04-06 | ||
| CN2016102087808 | 2016-04-06 |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108823414A (en) * | 2018-06-30 | 2018-11-16 | 浙江天地环保科技有限公司 | A method of waste and old perovskite solar battery is recycled |
| CN109786561A (en) * | 2019-01-22 | 2019-05-21 | 南京华群光电技术有限公司 | A kind of technique with perovskite active layer in amine liquefaction perovskite method recycling and reusing perovskite device |
| 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 |
| CN110767812A (en) * | 2019-10-31 | 2020-02-07 | 南通大学 | Novel method for prolonging service life of perovskite film |
| 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 |
| CN112467032A (en) * | 2020-10-27 | 2021-03-09 | 南昌大学 | Method for preparing high-quality organic-inorganic perovskite film by using waste raw materials |
| TWI721664B (en) * | 2019-11-22 | 2021-03-11 | 東海大學 | Method for degrading conductive polymer |
| CN112620310A (en) * | 2020-12-15 | 2021-04-09 | 深圳市惠能材料科技研发中心(有限合伙) | Non-invasive recovery and reuse method and application of read-out circuit substrate integrated with halogen perovskite material |
| CN114602956A (en) * | 2022-03-04 | 2022-06-10 | 湖南铱太科技有限公司 | Recovery and regeneration method universal for positive and negative 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 |
| CN114871254A (en) * | 2022-04-08 | 2022-08-09 | 西湖大学 | Method for recovering lead iodide and substrate of waste perovskite device |
| CN114988464A (en) * | 2022-05-17 | 2022-09-02 | 华碧新能源技术研究(苏州)有限公司 | Method and device for recycling lead salt from perovskite battery |
| TWI810867B (en) * | 2022-03-28 | 2023-08-01 | 國立清華大學 | Method for recovering valuable material from perovskite solar cell |
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| US20140060643A1 (en) * | 2012-09-05 | 2014-03-06 | Lane W. Martin | Light Absorbing Oxide Materials for Photovoltaic and Photocatalytic Applications and Devices |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN108823414A (en) * | 2018-06-30 | 2018-11-16 | 浙江天地环保科技有限公司 | A method of waste and old perovskite solar battery is recycled |
| CN109786561A (en) * | 2019-01-22 | 2019-05-21 | 南京华群光电技术有限公司 | A kind of technique with perovskite active layer in amine liquefaction perovskite method recycling and reusing perovskite device |
| 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 |
| 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 |
| CN110767812A (en) * | 2019-10-31 | 2020-02-07 | 南通大学 | Novel method for prolonging service life of perovskite film |
| TWI721664B (en) * | 2019-11-22 | 2021-03-11 | 東海大學 | Method for degrading conductive polymer |
| CN112467032B (en) * | 2020-10-27 | 2022-12-06 | 南昌大学 | Method for preparing high-quality organic-inorganic perovskite film by using waste raw materials |
| CN112467032A (en) * | 2020-10-27 | 2021-03-09 | 南昌大学 | Method for preparing high-quality organic-inorganic perovskite film by using waste raw materials |
| CN112620310A (en) * | 2020-12-15 | 2021-04-09 | 深圳市惠能材料科技研发中心(有限合伙) | Non-invasive recovery and reuse method and application of read-out circuit substrate integrated with halogen perovskite material |
| CN114602956B (en) * | 2022-03-04 | 2022-12-09 | 湖南铱太科技有限公司 | Recovery and regeneration method universal for positive and negative perovskite solar cell |
| CN114602956A (en) * | 2022-03-04 | 2022-06-10 | 湖南铱太科技有限公司 | Recovery and regeneration method universal for positive and negative perovskite solar cell |
| TWI810867B (en) * | 2022-03-28 | 2023-08-01 | 國立清華大學 | Method for recovering valuable material from perovskite solar cell |
| CN114871254A (en) * | 2022-04-08 | 2022-08-09 | 西湖大学 | Method for recovering lead iodide and substrate of waste perovskite device |
| CN114871254B (en) * | 2022-04-08 | 2023-02-28 | 西湖大学 | Method for recovering lead iodide and substrate of waste perovskite device |
| CN114988464A (en) * | 2022-05-17 | 2022-09-02 | 华碧新能源技术研究(苏州)有限公司 | Method and device for recycling lead salt from perovskite battery |
| 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 |
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