CN104993060B - A kind of Ca-Ti ore type solar cell without annealing and preparation method thereof - Google Patents
A kind of Ca-Ti ore type solar cell without annealing and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to area of solar cell, disclose a kind of Ca-Ti ore type solar cell without annealing and preparation method thereof, in described preparation method inidum chloride is added in perovskite presoma, film is obtained by spin coating, immersion or czochralski method, the perovskite crystal of crystallization is directly formed at room temperature, then electron transfer layer is obtained using the processing method without annealing.The preparation method of the present invention, with preparation technology is simple, the low advantage of preparation temperature, is conducive to being greatly lowered the cost of organic solar batteries using spin coating, inkjet printing or volume to volume printing process processing Ca-Ti ore type solar cell；Simultaneously to substrate without strict requirements, it is more beneficial for preparing large area, the device of flexible；Avoid calcium titanium ore bed and make crystallization degree in annealing process and differ the present situation of the device efficiency repetitive rate difference brought, no annealing process is simple, easily repeats, improves the uniformity of device efficiency, be easy to industrialized production.
Description
Technical field
The invention belongs to area of solar cell, it is related to a kind of perovskite solar cell and preparation method thereof, particularly
It is related to a kind of Ca-Ti ore type solar cell without annealing and preparation method thereof.
Background technology
Ca-Ti ore type solar cell is one of study hotspot that current photovoltaic device is utilized.Ca-Ti ore type solar cell
The concern of numerous researchers is attracted with its with low cost, advantages of simple structure and simple.Its electricity conversion is in nearly 5 years
More than 15% is brought up to rapidly from 3.8%, is favored by vast scientific researcher.
In 2009, the researcher such as Japanese Miyasaka reported organic-lead halogenation with perovskite structure first
Thing (CH3NH3PbBr3, CH3NH3PbI3) is used for liquid electrolyte DSSC as photoelectric conversion material.
Due to perovskite light-absorption layer in liquid electrolyte less stable, only obtain 3.81% photoelectric transformation efficiency.At present, it is based on
SpiroOMeTAD has been increased to 19.3% as the PCE of the perovskite battery of hole transmission layer, display great potential
Application prospect.
Ca-Ti ore type solar cell moves towards application, it is necessary to solve technologic problem.Generally for mesoporous TiO2
Its annealing of the solar cell of structure needs 500 DEG C of high-temperature process, and high-temperature process has very big limit for the requirement of substrate
System, is also unfavorable for the realization of flexible device, meanwhile, this condition of the high annealing of calcium titanium ore bed film largely governs
The realization of its industrialization.Annealing temperature at present for calcium titanium ore bed film is general at 100 DEG C or so, and which increases device production
The cost that industryization makes, in order to simplify this also process, researcher proposes manufacture craft of the calcium titanium ore bed film without annealing, and it is tied
Structure is similar to traditional structure, by the new material that adulterates in calcium titanium ore bed membrane-film preparation process, reduces perovskite thin film knot
Brilliant activation energy, makes its straight forming in spin coating process, without annealing.
The content of the invention
The technical problem to be solved：Conventional perovskite solar cell needs to carry out annealing process in preparation process,
Its technical process is numerous and diverse, cost is higher, and in order to simplify this also process, the purpose of the present invention is to disclose a kind of calcium titanium without annealing
Ore deposit solar cell and preparation method thereof, preparation method of the invention is new by doping in calcium titanium ore bed membrane-film preparation process
Material, reduces the activation energy of perovskite thin film crystallization, makes its straight forming in spin coating process, without annealing.
Technical scheme：In order to solve the above problems, the invention discloses a kind of Ca-Ti ore type solar cell without annealing
Preparation method, described preparation method comprises the following steps：
（1）By iodate first ammonium (MAI) and lead chloride (PbCl2) and inidum chloride (InCl3) in molar ratio 3:1:0.25-
0.35 is dissolved in N,N-dimethylformamide（DMF）In solution, stir 2-8 hours, obtain 30wt% perovskite DMF solution；
（2）By poly- 3,4- ethylenedioxy thiophenes：Poly styrene sulfonate（PEDOT:PSS）Solution is beaten using spin coating, ink-jet
Print or the processing of volume to volume method form uniform hole transport layer film on base clear electrode；
（3）By hole transport layer film at 95-105 DEG C, anneal 10-40min in air, forms the hole transport of solidification
Layer；
（4）In poly- 3,4- ethylenedioxy thiophenes：Poly styrene sulfonate（PEDOT:PSS）Spin coating, ink-jet are used on film
The method processing calcium titanium ore bed film of printing or volume to volume, unordered annealing is that can obtain uniform curing photosensitive layer；
（5）The method working process using spin coating, inkjet printing or volume to volume can be continued on perovskite thin film
[6,6]-phenyl-C61- methyl butyrates（PCBM）Film, equally can obtain uniform electron transfer layer without annealing；
（6）On the electron transport layer using evaporation or inkjet printing methods processing cathode electrode.
It is preferred that, a kind of preparation method of described Ca-Ti ore type solar cell without annealing, described step（1）In
Iodate first ammonium and lead chloride and inidum chloride mol ratio are 3:1:0.3.
It is preferred that, a kind of preparation method of described Ca-Ti ore type solar cell without annealing, described step（3）In
By film at 100 DEG C, anneal 20min in air.
It is preferred that, a kind of preparation method of described Ca-Ti ore type solar cell without annealing, described step（1）In
Mixing time is 5h.
It is preferred that, a kind of preparation method of described Ca-Ti ore type solar cell without annealing, described preparation method
Middle substrate is flexible substrates, ito glass, AZO glass or FTO glass.
The calcium titanium that a kind of preparation method of Ca-Ti ore type solar cell without annealing described in any of the above is prepared
Ore deposit type solar cell.
Beneficial effect：The present invention compared with prior art, is processed using spin coating, inkjet printing or volume to volume printing process
Ca-Ti ore type solar cell, compared to traditional high annealing preparation technology, with preparation technology is simple, preparation temperature is low excellent
Point, is conducive to being greatly lowered the cost of organic solar batteries；
The Ca-Ti ore type solar cell that prepared by the electron transfer layer without annealing using the perovskite thin film without annealing,
There is cost advantage in large-scale production, while to substrate without strict requirements, being more beneficial for preparing large area, flexible bendable
Bent device；
Calcium titanium ore bed is avoided without annealing process in this patent well make crystallization degree in annealing process and differ and bring
Device efficiency repetitive rate difference present situation, no annealing process is simple, easily repeats, improves the uniformity of device efficiency, be easy to
Industrialized production.
Brief description of the drawings
The structural representation for the Ca-Ti ore type solar cell that Fig. 1 prepares for the preparation method of the present invention, wherein 1 is
Flexible substrates, 2 be anode electrode, and 3 be hole transmission layer, and 4 be perovskite thin film, and 5 be electron transfer layer, and 6 be cathode electrode；
Fig. 2 is the ito glass substrate calcium titanium ore bed film and electric transmission layer film of preparation method of the present invention without annealing
Ca-Ti ore type solar cell device intensity of illumination be AM1.5G under current density voltage curve；
The flexible substrates calcium titanium ore bed film of Fig. 3 preparation methods of the present invention and calcium titanium of the electric transmission layer film without annealing
Current density voltage curve of the ore deposit type solar cell device in the case where intensity of illumination is AM1.5G；
Embodiment
Embodiment 1
（1）One ito glass substrate is provided, and is standardized cleaning；
（2）By iodate first ammonium (MAI) and lead chloride (PbCl2) and inidum chloride (InCl3) in molar ratio 3:1:0.3 is dissolved in
In DMF solution, stir 5 hours, obtain 30wt% perovskite DMF solution；
（3）By PEDOT:PSS solution is processed in substrate transparency electrode using spin coating method, accelerates to turning for 4500rpm
The lower rotation of speed 40 seconds, forms uniform anode modification layer, 100 DEG C are annealed 20 minutes；
（4）In PEDOT:Calcium titanium ore bed film is processed using spin coating method on PSS films, 4000rpm rotating speed is accelerated to
Lower rotation 40 seconds, unordered annealing can obtain the good photosensitive layer of homogeneously crystallized property；
（5）Spin coating method is processed under electron transfer layer PCBM, the rotating speed for accelerating to 2000rpm on perovskite thin film
Rotation 40 seconds, obtains uniform electric transmission layer film；
（6）Cathode electrode Ag is prepared using the method for evaporation, its thickness is 100nm.
Embodiment 2
（1）One ITO flexible substrates is provided, and is standardized cleaning；
（2）By iodate first ammonium (MAI) and lead chloride (PbCl2) and inidum chloride (InCl3) in molar ratio 3:1:0.3 is dissolved in
In DMF solution, stir 5 hours, obtain 30wt% perovskite DMF solution；
（3）By PEDOT:PSS solution is processed in substrate transparency electrode using spin coating method, accelerates to turning for 4500rpm
The lower rotation of speed 40 seconds, forms uniform anode modification layer, 100 DEG C are annealed 20 minutes；
（4）In PEDOT:Calcium titanium ore bed film is processed using spin coating method on PSS films, 4000rpm rotating speed is accelerated to
Lower rotation 40 seconds, unordered annealing can obtain the good photosensitive layer of homogeneously crystallized property；
（5）Spin coating method is processed under electron transfer layer PCBM, the rotating speed for accelerating to 2000rpm on perovskite thin film
Rotation 40 seconds, obtains uniform electric transmission layer film；
（6）Cathode electrode Ag is prepared using the method for evaporation, its thickness is 100nm.
Embodiment 3
（1）One ITO flexible substrates is provided, and is standardized cleaning；
（2）By iodate first ammonium (MAI) and lead chloride (PbCl2) and inidum chloride (InCl3) in molar ratio 3:1:0.25 is dissolved in
In DMF solution, stir 2 hours, obtain 30wt% perovskite DMF solution；
（3）By PEDOT:PSS solution is processed in substrate transparency electrode using spin coating method, accelerates to turning for 4500rpm
The lower rotation of speed 40 seconds, forms uniform anode modification layer, 95 DEG C are annealed 40 minutes；
（4）In PEDOT:Calcium titanium ore bed film is processed using spin coating method on PSS films, 4000rpm rotating speed is accelerated to
Lower rotation 40 seconds, unordered annealing can obtain the good photosensitive layer of homogeneously crystallized property；
（5）Spin coating method is processed under electron transfer layer PCBM, the rotating speed for accelerating to 2000rpm on perovskite thin film
Rotation 40 seconds, obtains uniform electric transmission layer film；
（6）Cathode electrode Ag is prepared using the method for evaporation, its thickness is 100nm.
Embodiment 4
（1）One ITO flexible substrates is provided, and is standardized cleaning；
（2）By iodate first ammonium (MAI) and lead chloride (PbCl2) and inidum chloride (InCl3) in molar ratio 3:1:0.35 is dissolved in
In DMF solution, stir 8 hours, obtain 30wt% perovskite DMF solution；
（3）By PEDOT:PSS solution is processed in substrate transparency electrode using spin coating method, accelerates to turning for 4500rpm
The lower rotation of speed 40 seconds, forms uniform anode modification layer, 105 DEG C are annealed 10 minutes；
（4）In PEDOT:Calcium titanium ore bed film is processed using spin coating method on PSS films, 4000rpm rotating speed is accelerated to
Lower rotation 40 seconds, unordered annealing can obtain the good photosensitive layer of homogeneously crystallized property；
（5）Spin coating method is processed under electron transfer layer PCBM, the rotating speed for accelerating to 2000rpm on perovskite thin film
Rotation 40 seconds, obtains uniform electric transmission layer film；
（6）Cathode electrode Ag is prepared using the method for evaporation, its thickness is 100nm.
Embodiment 5
（1）One ITO flexible substrates is provided, and is standardized cleaning；
（2）By iodate first ammonium (MAI) and lead chloride (PbCl2) and inidum chloride (InCl3) in molar ratio 3:1:0.35 is molten
In DMF solution, stir 8 hours, obtain 30wt% perovskite DMF solution；
（3）By PEDOT:PSS solution is processed in substrate transparency electrode using spin coating method, accelerates to turning for 4500rpm
The lower rotation of speed 40 seconds, forms uniform anode modification layer, 105 DEG C are annealed 10 minutes；
（4）In PEDOT:Calcium titanium ore bed film is processed using spin coating method on PSS films, 4000rpm rotating speed is accelerated to
Lower rotation 40 seconds, unordered annealing can obtain the good photosensitive layer of homogeneously crystallized property；
（5）Spin coating method processing is without fullerene electron transport material indene-C60 on perovskite thin film
Monoadduct (ICMA), accelerates under 2000rpm rotating speed and rotates 40 seconds, obtain uniform electric transmission layer film；
（6）Cathode electrode Ag is prepared using the method for evaporation, its thickness is 100nm.
Comparative example 1
（1）One ITO flexible substrates is provided, and is standardized cleaning；
（2）By iodate first ammonium (MAI) and lead chloride (PbCl2) and ammonium chloride in molar ratio 3:1:0.25 to be dissolved in DMF molten
In liquid, stir 2 hours, obtain 30wt% perovskite DMF solution；
（3）By PEDOT:PSS solution is processed in substrate transparency electrode using spin coating method, accelerates to turning for 4500rpm
The lower rotation of speed 40 seconds, forms uniform anode modification layer, 95 DEG C are annealed 40 minutes；
（4）In PEDOT:Calcium titanium ore bed film is processed using spin coating method on PSS films, 4000rpm rotating speed is accelerated to
Lower rotation 40 seconds, unordered annealing can obtain the good photosensitive layer of homogeneously crystallized property；
（5）Spin coating method is processed under electron transfer layer PCBM, the rotating speed for accelerating to 2000rpm on perovskite thin film
Rotation 40 seconds, obtains uniform electric transmission layer film；
（6）Cathode electrode Ag is prepared using the method for evaporation, its thickness is 100nm.
The performance of above-described embodiment and the solar cell of comparative example is as follows：
Claims (7)
1. a kind of preparation method of the Ca-Ti ore type solar cell without annealing, it is characterised in that calcium in described preparation method
Inidum chloride is added in titanium ore presoma, film is obtained by the method for spin coating, inkjet printing or volume to volume, at room temperature directly
The perovskite crystal of crystallization is formed, then electron transfer layer is obtained using the processing method without annealing.
2. a kind of preparation method of Ca-Ti ore type solar cell without annealing according to claim 1, it is characterised in that
Described preparation method comprises the following steps：
（1）By iodate first ammonium and lead chloride and inidum chloride in molar ratio 3:1:0.25-0.35 is dissolved in N,N-dimethylformamide
In solution, stir 2-8 hours, obtain 30wt% perovskite DMF solution；
（2）By poly- 3,4- ethylenedioxy thiophenes：Poly styrene sulfonate solution uses spin coating, inkjet printing or volume to volume method
Processing forms uniform hole transport layer film on base clear electrode；
（3）By hole transport layer film at 95-105 DEG C, anneal 10-40min in air, forms the hole transmission layer of solidification；
（4）In poly- 3,4- ethylenedioxy thiophenes：Using spin coating, inkjet printing or volume to volume on poly styrene sulfonate film
Method processes calcium titanium ore bed film, and uniform curing photosensitive layer is can obtain without annealing；
（5）Can continue on perovskite thin film using spin coating, inkjet printing or volume to volume method working process [6,
6]-phenyl-C61- methyl butyrates（PCBM）Film, equally can obtain uniform electron transfer layer without annealing；
（6）On the electron transport layer using evaporation or inkjet printing methods processing cathode electrode.
3. a kind of preparation method of Ca-Ti ore type solar cell without annealing according to claim 2, it is characterised in that
Described step（1）Middle iodate first ammonium and lead chloride and inidum chloride mol ratio are 3:1:0.3.
4. a kind of preparation method of Ca-Ti ore type solar cell without annealing according to claim 2, it is characterised in that
Described step（3）It is middle by film at 100 DEG C, anneal 20min in air.
5. a kind of preparation method of Ca-Ti ore type solar cell without annealing according to claim 2, it is characterised in that
Described step（1）Middle mixing time is 5h.
6. a kind of preparation method of Ca-Ti ore type solar cell without annealing according to claim 2, it is characterised in that
Substrate is flexible substrates, ito glass, AZO glass or FTO glass in described preparation method.
7. prepared according to a kind of preparation method of any described Ca-Ti ore type solar cell without annealing of claim 1 to 6
Obtained Ca-Ti ore type solar cell.
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| CN105256374B (en) * | 2015-11-05 | 2017-11-28 | 浙江大学城市学院 | A kind of method that organic perovskite film preparation device prepares CH3NH3PbI3 films |
| CN105789451B (en) * | 2016-04-19 | 2018-05-25 | 中国科学院化学研究所 | A kind of perovskite crystal film and its water vapour annealing preparation method and application |
| CN108550697A (en) * | 2017-10-30 | 2018-09-18 | 上海幂方电子科技有限公司 | Flexible organic solar batteries and its all print preparation method |
| CN109411554B (en) * | 2018-09-10 | 2021-02-05 | 暨南大学 | Anion-cation co-doped inorganic perovskite thin film and preparation method and application thereof |
| CN109473556A (en) * | 2018-09-19 | 2019-03-15 | 南通大学 | In the method for preparing perovskite solar battery under room temperature entirely |
| CN109686989B (en) * | 2018-12-29 | 2021-12-24 | 无锡极电光能科技有限公司 | Preparation method of solid fuel cell cathode material |
| CN110808316A (en) * | 2019-11-14 | 2020-02-18 | 深圳扑浪创新科技有限公司 | Patterning method of perovskite quantum dots |
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