CN104733618A - Method for preparing perovskite solar cell absorption layer - Google Patents
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- CN104733618A CN104733618A CN201510100131.1A CN201510100131A CN104733618A CN 104733618 A CN104733618 A CN 104733618A CN 201510100131 A CN201510100131 A CN 201510100131A CN 104733618 A CN104733618 A CN 104733618A
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Abstract
The invention relates to a method for preparing a perovskite solar cell absorption layer, and belongs to the technical field of photovoltaic and semiconductor device manufacturing. A cleaned substrate is placed in an evaporation chamber, PbX2 powder and a CH3NH3I crystal are evaporated step by step or jointly, annealing and mechanical extrusion are conducted, and then the extruded and optimized CH3NH3PbX3 absorption layer is acquired. Instruments commonly seen in industrial production are used in the whole preparation process, and device is simple in structure and convenient to operate. Adopted raw materials are low in price, the experimental period is short, and practicality is high. According to the method, the mechanical extrusion method which is simple and free of cost is used for conducting after-treatment on the prepared perovskite absorption layer CH3NHPbX2I, the stability of the absorption layer can be greatly improved, and the mechanical extrusion method has no bad effects on the process difficulty and the performance indexes of a perovskite solar cell.
Description
Technical field
The present invention relates to a kind of preparation method of perovskite solar cell absorbed layer, particularly relate to the method that evaporation prepares perovskite solar cell absorbed layer stability, belong to photovoltaic and semiconductor device processing technology field.
Background technology
A kind of CH based on perovskite structure
3nH
3pbX
3the solar cell of (X represents halogen) material causes global concern.Prepared first piece of battery from 2009, till now, the peak efficiency of perovskite solar cell reaches 19.3%.(Huanping Zhou et al.,Interface engineering of highly efficient perovskitesolar cells,Science 345,542(2014))
A few years, perovskite solar cell has developed multiple device architecture, generally can be divided into meso-hole structure and plane heterostructure two kinds.The perovskite solar cell of meso-hole structure is respectively from top to bottom: FTO electro-conductive glass, TiO
2compacted zone, TiO
2mesoporous layer, calcium titanium ore bed, HTM layer, metal electrode.Planar heterojunction structure is then on this basis, porous support layer n-type semiconductor TiO
2change insulating material Al into
2o
3, form a kind of heterojunction type solar cell (Liu M, Johnston M B, Snaith H J 2013Nature 501395) of the sight superstructure that is situated between.Further can also remove the shelf layer of insulation, prepare to have and be similar to p-i-n junction structure plane hetero-junction solar cell.
CH
3nH
3pbX
3absorbed layer material can adopt multiple method to be prepared, and compares and common are a step solwution method, two step solwution methods, evaporation and solution-vapour deposition process etc.The spin coating proceeding of solwution method is simple and easy to use, with low cost, but often causes surface coverage incomplete, occurs pin hole.The perovskite material impurity defect adopting coevaporation method to prepare is few, and compact structure, surface has perfect homogeneity.But the method needs high vacuum, higher to the requirement of equipment.
CH
3nH
3pbX
3absorbed layer material absorption co-efficient is up to 10
5.By regulating the composition of perovskite material, the color of its band gap width and battery can be changed.In addition, it is low that perovskite solar cell also has cost, preparation technology is simple, and the series of advantages such as flexibility, transparent and laminated cell can be prepared, and the defect characteristics of its uniqueness, make perovskite crystal material both can present the character of n-type semiconductor, also can present the character of p-type semiconductor, so its application is more diversified.And CH
3nH
3pbX
3have cheapness, can the feature prepared of solution, this extensive, low cost manufacture being perovskite solar cell provides possibility.
But stability test factor constrains the development of perovskite solar cell, CH
3nH
3pbX
3absorbed layer material is very responsive to steam, and the sight TiO that is situated between
2the perovskite battery of structure is decayed in the efficiency that UV light-induced lower existence is serious.
Summary of the invention
The object of the invention is the preparation method proposing a kind of perovskite solar cell absorbed layer, adopt hot evaporation coating technique preparation technology, prepare perovskite battery obsorbing layer CH on the surface of a substrate
3nH
3pbX
3, and mechanics extruding is carried out to this layer, realize the raising of perovskite solar cell absorbed layer self stability, thus improve the stability of whole battery.
The preparation method of the perovskite solar cell absorbed layer that the inventive method proposes, comprises the following steps:
(1) glass substrate after cleaning is put into thermal evaporation cavity, PbX will be housed
2first crucible of powder and CH is housed
3nH
3second crucible of I crystal is placed on the evaporation electrode in thermal evaporation cavity respectively, first crucible and the second crucible are wound with tungsten filament respectively, it is 5 ~ 8 circles that tungsten filament is wound around the number of turns, and make the vertical range H between the mouth of pot of the first crucible and the second crucible and glass substrate be 10 ~ 14cm, the PbX in the first crucible and the second crucible
2powder and CH
3nH
3the mol ratio of I crystal is: PbX
2powder: CH
3nH
3i crystal=1:(1 ~ 4), wherein X is halogens I or Cl;
(2) to thermal evaporation cavity extracting vacuum, vacuum degree is made to reach 3 × 10
-3below Pa, toasts the substrate of thermal evaporation cavity, and baking temperature is room temperature ~ 50 DEG C, toasts 15 minutes;
(3) to PbX is housed
2the tungsten filament of the first crucible of powder applies 6.4 ~ 7.4A evaporation current, evaporates after 10 minutes, evaporation current is enlarged to 7.4 ~ 8.4A, evaporate 5 minutes, the glass substrate of thermal evaporation cavity obtains PbX
2book film, then to CH is housed
3nH
3the tungsten filament of the second crucible of I crystal applies 5.6A, and evaporation current, evaporates 15 minutes, now in the glass substrate of thermal evaporation cavity, obtain CH
3nH
3pbX
2i film;
(4) make thermal evaporation cavity be down to room temperature, take out with CH from thermal evaporation cavity
3nH
3pbX
2the glass substrate of I book film, places 20 ~ 30 minutes in atmosphere, in atmosphere, by CH
3nH
3pbX
2i book film is heated to 80 ~ 120 DEG C, is incubated 30 minutes;
(5) step (4) is obtained with CH
3nH
3pbX
2the glass substrate of I book film faces up horizontal positioned, and at CH
3nH
3pbX
2a soft gasket is put on I book film surface, and soft gasket arranges one deck flat board, applies the pressure of one 50 ~ 100 Ns, maintain 12 ~ 48 hours on flat board, obtains extruding the perovskite solar cell absorbed layer CH optimized
3nH
3pbX
2i.
In the inventive method, described substrate can be ITO electro-conductive glass, FTO electro-conductive glass or simple glass.
The preparation method of the perovskite solar cell absorbed layer that the present invention proposes, has the following advantages:
1, hot evaporation process is used, CH in preparation method of the present invention
3nH
3pbX
2i impurities of materials defect is few, compact structure, and surface has perfect homogeneity, is conducive to large area and prepares solar cell.
2, the CH obtained in preparation method of the present invention
3nH
3pbX
2i material, in natural placement situation, light-induced degradation phenomenon obviously weakens, for commercially producing of battery provides feasible solution.
What 3, use in whole preparation process of the present invention is all instrument common in suitability for industrialized production, and device structure is simple, easy to operate.Raw materials used cheap, experimental period is short, and practicality is high.
4, in preparation method of the present invention, use the mechanics pressing method of simple cost free to the perovskite absorbed layer CH of preparation
3nH
3pbX
2i carries out reprocessing, can increase substantially the stability of absorbed layer, and the method for mechanics extruding to the technology difficulty of perovskite solar cell and performance index without any harmful effect.
Accompanying drawing explanation
Fig. 1 is the evaporation equipment structural representation of the perovskite solar cell absorbed layer for the preparation of the present invention's proposition.
Fig. 2 is the principle schematic that the solar cell absorbed layer prepared the present invention carries out mechanics extruding.
Fig. 3 is CH prepared by the inventive method
3nH
3pbI
3absorbed layer scanning electron microscope (SEM) photograph.
Fig. 4 is CH prepared by the inventive method
3nH
3pbI
3the X-ray diffractogram of absorbed layer.
Fig. 5-1, Fig. 5-2 are CH prepared by the inventive method
3nH
3pbI
3absorbed layer trap in natural placement situation changes collection of illustrative plates in time.
Fig. 6-1, Fig. 6-2 are CH prepared by the inventive method
3nH
3pbI
3absorbed layer transmitance in natural placement situation changes collection of illustrative plates in time.
In Fig. 1 and Fig. 2,1 is the first crucible, in-built inorganic matter PbX
2evaporation source, 2 is second crucibles, in-built organic substance CH
3nH
3i evaporation source, 3 is glass substrate, and 4 is tungsten filaments, and 5 is evaporation cavities, and 6 is soft gaskets, and 7 is dull and stereotyped.
Embodiment
The preparation method of the perovskite solar cell absorbed layer that the present invention proposes, as shown in Figure 1, the method comprises the following steps the device involved by its preparation process:
(1) glass substrate after cleaning is put into thermal evaporation cavity, PbX will be housed
2first crucible 1 of powder and CH is housed
3nH
3second crucible 2 of I crystal is placed on the evaporation electrode in thermal evaporation cavity 5 respectively, crucible is wound with tungsten filament 4, it is 5 ~ 8 circles that tungsten filament is wound around the number of turns, and makes the vertical range H between mouth of pot and glass substrate 3 be 10 ~ 14cm, the PbX in the first crucible 1 and the second crucible 2
2powder and CH
3nH
3the mol ratio of I crystal is: PbX
2powder: CH
3nH
3i crystal=1:(1 ~ 4), wherein X is halogens I or Cl;
(2) to thermal evaporation cavity extracting vacuum, vacuum degree is made to reach 3 × 10
-3below Pa, toasts the substrate of thermal evaporation cavity, and baking temperature is room temperature ~ 50 DEG C, toasts 15 minutes;
(3) to PbX is housed
2the tungsten filament of the first crucible of powder applies 6.4 ~ 7.4A evaporation current, evaporates after 10 minutes, evaporation current is enlarged to 7.4 ~ 8.4A, evaporate 5 minutes, the glass substrate of thermal evaporation cavity obtains PbX
2book film, then to CH is housed
3nH
3the tungsten filament of the second crucible of I crystal applies 5.6A, and evaporation current, evaporates 15 minutes, now in the glass substrate of thermal evaporation cavity, obtain CH
3nH
3pbX
2i film;
(4) make thermal evaporation cavity be down to room temperature, take out with CH from thermal evaporation cavity
3nH
3pbX
2the glass substrate of I book film, places 20 ~ 30 minutes in atmosphere, in atmosphere, by CH
3nH
3pbX
2i book film is heated to 80 ~ 120 DEG C, is incubated 30 minutes;
(5) step (4) is obtained with CH
3nH
3pbX
2the glass substrate of I book film faces up horizontal positioned, and at CH
3nH
3pbX
2a soft gasket 6 is put on I book film surface, and soft gasket arranges one deck flat board 7, applies the pressure of one 50 ~ 100 Ns, maintain 12 ~ 48 hours on flat board, obtains extruding the perovskite solar cell absorbed layer CH optimized
3nH
3pbX
2i.
In above-mentioned preparation method, substrate can be ITO electro-conductive glass, FTO electro-conductive glass or simple glass.
In above-mentioned preparation method, CH
3nH
3i raw material can pass through CH
3nH
2+ HI=CH
3nH
3the synthesis technique of I obtains, and concrete synthesis technique is at list of references: Lioz Etgar, Peng Gao, Zhaosheng Xue, | J.Am.Chem.Soc.2012,134,17396-17399 are fully open.
In preparation method of the present invention, be used for preparing CH
3nH
3pbX
2the parameter of I absorbed layer, as pulp furnish, annealing temperature, mechanics fashion of extrusion etc., allows to adjust in right amount.Wherein prepare CH
3nH
3pbX
3the method of absorbed layer is not limited to the thermal evaporation method of above introduction, also has multiple maturation process all successfully can prepare CH at present
3nH
3pbX
3absorbed layer, as a step solwution method, two step solwution methods and solution-vapour deposition process etc.
Below introduce the embodiment of the inventive method:
Embodiment one:
(1) glass substrate after cleaning is put into thermal evaporation cavity, PbI will be housed
2first crucible of powder and CH is housed
3nH
3second crucible of I crystal to be placed in thermal evaporation cavity on evaporation electrode respectively, crucible is wound with tungsten filament, it is 8 circles that first crucible tungsten filament is wound around the number of turns, it is 5 circles that second crucible tungsten filament is wound around the number of turns, and make the vertical range H between mouth of pot and glass substrate be 12cm, the PbI in the first crucible and the second crucible
2powder and CH
3nH
3the mol ratio of I crystal is: PbI
2powder: CH
3nH
3i crystal=1:3;
(2) to thermal evaporation cavity extracting vacuum, vacuum degree is made to reach 3 × 10
-3below Pa, toasts the substrate of thermal evaporation cavity, and baking temperature is 25 DEG C, toasts 15 minutes;
(3) to PbI is housed
2the tungsten filament of the first crucible of powder applies 6.4 evaporation current, evaporates after 10 minutes, evaporation current is enlarged to 7.4, evaporates 5 minutes, the glass substrate of thermal evaporation cavity obtains PbI
2book film, then to CH is housed
3nH
3the tungsten filament of the second crucible of I crystal applies 5.6A, and evaporation current, evaporates 15 minutes, now in the glass substrate of thermal evaporation cavity, obtain CH
3nH
3pbI
3film;
(4) make thermal evaporation cavity be down to room temperature, take out with CH from thermal evaporation cavity
3nH
3pbI
3the glass substrate of book film, places 30 minutes, in atmosphere in atmosphere, by CH
3nH
3pbI
3book film is heated to 80 DEG C, is incubated 30 minutes;
(5) step (4) is obtained with CH
3nH
3pbI
3the glass substrate of book film faces up horizontal positioned, and at CH
3nH
3pbI
3a soft gasket is put on book film surface, and soft gasket arranges one deck flat board, applies the pressure of one 50 Ns, maintain 12 hours on flat board, obtains extruding the perovskite solar cell absorbed layer CH optimized
3nH
3pbI
3.
Embodiment two:
(1) glass substrate after cleaning is put into thermal evaporation cavity, PbCl will be housed
2first crucible of powder and CH is housed
3nH
3second crucible of I crystal to be placed in thermal evaporation cavity on evaporation electrode respectively, crucible is wound with tungsten filament, it is 8 circles that first crucible tungsten filament is wound around the number of turns, it is 5 circles that second crucible tungsten filament is wound around the number of turns, and make the vertical range H between mouth of pot and glass substrate be 12cm, the PbCl in the first crucible and the second crucible
2powder and CH
3nH
3the mol ratio of I crystal is: PbCl
2powder: CH
3nH
3i crystal=1:3;
(2) to thermal evaporation cavity extracting vacuum, vacuum degree is made to reach 3 × 10
-3below Pa, toasts the substrate of thermal evaporation cavity, and baking temperature is 50 DEG C, toasts 15 minutes;
(3) to PbCl is housed
2the tungsten filament of the first crucible of powder applies 7.4 evaporation current, evaporates after 10 minutes, evaporation current is enlarged to 8.4, evaporates 5 minutes, the glass substrate of thermal evaporation cavity obtains PbCl
2book film, then to CH is housed
3nH
3the tungsten filament of the second crucible of I crystal applies 5.6A, and evaporation current, evaporates 15 minutes, now in the glass substrate of thermal evaporation cavity, obtain CH
3nH
3pbCl
2i film;
(4) make thermal evaporation cavity be down to room temperature, take out with CH from thermal evaporation cavity
3nH
3pbCl
2the glass substrate of I book film, places 30 minutes, in atmosphere in atmosphere, by CH
3nH
3pbCl
2i book film is heated to 100 DEG C, is incubated 30 minutes;
(5) step (4) is obtained with CH
3nH
3pbCl
2the glass substrate of I book film faces up horizontal positioned, and at CH
3nH
3pbCl
2a soft gasket is put on I book film surface, and soft gasket arranges one deck flat board, applies the pressure of one 50 Ns, maintain 12 hours on flat board, obtains extruding the perovskite solar cell absorbed layer CH optimized
3nH
3pbCl
2i.
Fig. 3 is CH prepared by the inventive method
3nH
3pbI
3the scanning electron microscope (SEM) photograph of absorbed layer, wherein left side A figure is non-mechanics extruding Sample Scan Electronic Speculum figure, right side B figure is mechanics extruding Sample Scan Electronic Speculum figure.As can see from Figure 3, through the sample of mechanics extruding, maintain the crystal grain of single stable, do not occur that unreacted is complete or separate out phenomenon.
Fig. 4 is CH prepared by the inventive method
3nH
3pbI
3the X-ray diffractogram of absorbed layer, wherein A figure is non-mechanics extruding sample X-ray diffractogram, B figure is mechanics extruding sample X-ray diffractogram, and C figure is that 15 days X-ray diffractograms placed naturally by non-mechanics extruding sample, and D figure is that 15 days X-ray diffractograms placed naturally by mechanics extruding sample.Wherein 14.62 ° (110), 28.93 ° (220), 43.71 ° (330), 59.31 ° of (440) positions are CH
3nH
3pbI
3crystalline phase.Through mechanics extruding sample naturally placement 15 days after, still remain with CH
3nH
3pbI
3crystalline phase.And without mechanics extruding sample naturally placement 15 days after, CH
3nH
3pbI
3crystalline phase disappears substantially completely.
The CH that Fig. 5-1 is prepared for the inventive method
3nH
3pbI
3absorbed layer does not extrude absorption of sample degree and changes collection of illustrative plates in time, the CH that Fig. 5-2 is prepared for the inventive method
3nH
3pbI
3extruding sample trap in natural placement situation of absorbed layer changes collection of illustrative plates in time.Obviously can contrast from figure, have at natural placement situation stability inferior through the sample of mechanics extruding and significantly improved.
The CH that Fig. 6-1 is prepared for the inventive method
3nH
3pbI
3absorbed layer does not extrude sample transmitance in natural placement situation and changes collection of illustrative plates in time, and Fig. 6-2 is CH prepared by the inventive method
3nH
3pbI
3absorbed layer extruding sample transmitance in natural placement situation changes collection of illustrative plates in time.Obviously can contrast from figure, have at natural placement situation stability inferior through the sample of mechanics extruding and significantly improved.
Claims (2)
1. a preparation method for perovskite solar cell absorbed layer, is characterized in that the method comprises the following steps:
(1) glass substrate after cleaning is put into thermal evaporation cavity, PbX will be housed
2first crucible of powder and CH is housed
3nH
3second crucible of I crystal is placed on the evaporation electrode in thermal evaporation cavity respectively, first crucible and the second crucible are wound with tungsten filament respectively, it is 5 ~ 8 circles that tungsten filament is wound around the number of turns, and make the vertical range H between the mouth of pot of the first crucible and the second crucible and glass substrate be 10 ~ 14cm, the PbX in the first crucible and the second crucible
2powder and CH
3nH
3the mol ratio of I crystal is: PbX
2powder: CH
3nH
3i crystal=1:(1 ~ 4), wherein X is halogens I or Cl;
(2) to thermal evaporation cavity extracting vacuum, vacuum degree is made to reach 3 × 10
-3below Pa, toasts the substrate of thermal evaporation cavity, and baking temperature is room temperature ~ 50 DEG C, toasts 15 minutes;
(3) to PbX is housed
2the tungsten filament of the first crucible of powder applies 6.4 ~ 7.4A evaporation current, evaporates after 10 minutes, evaporation current is enlarged to 7.4 ~ 8.4A, evaporate 5 minutes, the glass substrate of thermal evaporation cavity obtains PbX
2book film, then to CH is housed
3nH
3the tungsten filament of the second crucible of I crystal applies 5.6A, and evaporation current, evaporates 15 minutes, now in the glass substrate of thermal evaporation cavity, obtain CH
3nH
3pbX
2i film;
(4) make thermal evaporation cavity be down to room temperature, take out with CH from thermal evaporation cavity
3nH
3pbX
2the glass substrate of I book film, places 20 ~ 30 minutes in atmosphere, in atmosphere, by CH
3nH
3pbX
2i book film is heated to 80 ~ 120 DEG C, is incubated 30 minutes;
(5) step (4) is obtained with CH
3nH
3pbX
2the glass substrate of I book film faces up horizontal positioned, and at CH
3nH
3pbX
2a soft gasket is put on I book film surface, and soft gasket arranges one deck flat board, applies the pressure of one 50 ~ 100 Ns, maintain 12 ~ 48 hours on flat board, obtains extruding the perovskite solar cell absorbed layer CH optimized
3nH
3pbX
2i.
2., in preparation method as claimed in claim 1, it is characterized in that wherein said substrate is ITO electro-conductive glass, FTO electro-conductive glass or simple glass.
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CN107119256A (en) * | 2017-04-27 | 2017-09-01 | 南京大学 | A kind of preparation method of tin based perovskites film |
CN107482124A (en) * | 2017-07-14 | 2017-12-15 | 武汉理工大学 | A kind of method that steam auxiliary prepares perovskite solar cell |
CN108847455A (en) * | 2018-06-12 | 2018-11-20 | 北京工业大学 | A method of growth perovskite thin film |
JP2020107912A (en) * | 2020-04-06 | 2020-07-09 | 株式会社東芝 | Method for manufacturing photoelectric conversion film and method for manufacturing photoelectric conversion element |
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CN106887521A (en) * | 2017-04-05 | 2017-06-23 | 陈胜红 | A kind of flexible translucent perovskite solar cell |
CN107119256A (en) * | 2017-04-27 | 2017-09-01 | 南京大学 | A kind of preparation method of tin based perovskites film |
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CN107482124A (en) * | 2017-07-14 | 2017-12-15 | 武汉理工大学 | A kind of method that steam auxiliary prepares perovskite solar cell |
CN108847455A (en) * | 2018-06-12 | 2018-11-20 | 北京工业大学 | A method of growth perovskite thin film |
JP2020107912A (en) * | 2020-04-06 | 2020-07-09 | 株式会社東芝 | Method for manufacturing photoelectric conversion film and method for manufacturing photoelectric conversion element |
JP2022176313A (en) * | 2020-04-06 | 2022-11-25 | 株式会社東芝 | Method for manufacturing photoelectric conversion film and method for manufacturing photoelectric conversion element |
CN112002812A (en) * | 2020-09-15 | 2020-11-27 | 常州大学 | Method for preparing perovskite solar cell absorption layer based on stepwise thermal evaporation and preparation of perovskite solar cell |
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