CN104934503B - A kind of preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide - Google Patents

A kind of preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide Download PDF

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CN104934503B
CN104934503B CN201510330755.2A CN201510330755A CN104934503B CN 104934503 B CN104934503 B CN 104934503B CN 201510330755 A CN201510330755 A CN 201510330755A CN 104934503 B CN104934503 B CN 104934503B
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reaction solution
lead
spin coating
bromide
methyl amine
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CN104934503A (en
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唐立丹
梅海林
王冰
彭淑静
齐锦刚
王建中
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Liaoning University of Technology
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L31/00Semiconductor devices sensitive to infra-red radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L31/00Semiconductor devices sensitive to infra-red radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248Semiconductor devices sensitive to infra-red radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256Semiconductor devices sensitive to infra-red radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

A kind of preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide, solid methyl ammonium bromide and solid brominated Asia lead are mixed, it is added to N, in N solvent dimethylformamide, stir, obtain reaction solution, reaction solution is poured in container, after applying pulse electromagnetic field carries out processing reaction solution, Deca is on the electro-conductive glass substrate cleaning up, carry out low speed spin coating and high speed spin coating respectively, form the perovskite thin film that a layer thickness is 500nm~800nm, it is then placed in vacuum drying oven, annealing, obtain methyl amine bromination thin film lead.Advantage is:Preparation process is simple, preparation cost is cheap, processed using pulse electromagnetic field, the degree of crystallinity of product can be improved, and greatly shorten the temperature retention time of annealing, the temperature retention time of annealing is only provided without the 1/6 of pulse electromagnetic field process, thus shortening the production cycle of product, energy saving, is conducive to industrialized production.

Description

A kind of preparation of perovskite solar cell light absorption layer material methyl amine lead bromide Method
Technical field
The invention belongs to solar cell material preparation field, it is related to a kind of high-crystallinity perovskite solaode and absorbs The preparation method of layer material methyl amine lead bromide, more particularly to one kind are prepared highly crystalline using pulse electromagnetic field assisted solution method The method of degree perovskite solar battery obsorbing layer material methyl amine lead bromide.
Background technology
With lack of energy and ecological deterioration, people are badly in need of finding a kind of Novel clean energy of alternative traditional fossil energy Source, solar energy has sustainability and the advantage such as pollution-free, is the important composition portion of countries in the world sustainable development source strategy Point, solaode is the Main Means currently with solar energy.How solaode is with the monocrystal silicon of the second filial generation or many at present Based on crystal silicon solar batteries, there is long the production cycle, high cost in this battery, there is energy consumption relatively in crystal silicon preparation process simultaneously The problems such as height and environmental pollution.Perovskite solaode is a kind of new solaode, and this battery principle is different from biography The crystal silicon based on pn-junction of system and hull cell, have the advantages that high efficiency, low cost, simply prepare, simultaneously its battery efficiency Constantly fast lifting, is promoted to the perovskite sun in 2015 by the battery efficiency of perovskite solaode in 2009 for 3.8% The battery efficiency of energy battery is 20.2%, and perovskite solaode is the extremely potential novel solar battery of one kind.
Organic inorganic hybridization perovskite material is the important component part of perovskite solaode, and the light serving as battery is inhaled Receive layer segment, there is bipolarity (electronics and hole) transfer function.The light absorbing zone of perovskite solaode is generally using tool There is the methyl amine lead iodide (CH of the perovskite structure of ABX33NH3PbI3) or methyl amine lead bromide (CH3NH3PbBr3), its source Extensively, low in raw material price flexible battery can be prepared.At present, the method preparing perovskite material mainly has solwution method and common steaming Send out method, single solwution method be difficult to obtain high-crystallinity perovskite absorbed layer, though coevaporation method be obtained in that highly crystalline The perovskite absorbed layer of degree, but preparation cost valency is higher, and problem above causes perovskite battery cannot large-scale commercial applications metaplasia Produce.Therefore how to obtain the emphasis that inexpensive, highly crystalline quality perovskite absorbed layer is current perovskite solaode research.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of high-crystallinity perovskite solar battery obsorbing layer material first The preparation method of base amine lead bromide, the method preparation process is simple, preparation cost is cheap, can improve the degree of crystallinity of product.
The technical solution of the present invention is:
A kind of preparation method of high-crystallinity perovskite solar battery obsorbing layer material methyl amine lead bromide, it specifically walks Suddenly as follows:
(1) clean substrate
Using FTO electro-conductive glass as substrate, after acetone and washes of absolute alcohol, then deionized water is rinsed well, dries Dry;
(2) prepare reaction solution
By solid methyl ammonium bromide (CH3NH3Br) and solid brominated Asia lead (PbBr2) mixed, it is added to N, N- diformazan In base Methanamide (DMF) solvent, stir, obtain reaction solution, described methyl bromide ammonium with the mol ratio of protobromide lead is 1:2~2:1, the molal volume of described methyl bromide ammonium and DMF is than for 1:1mol/L~1:2mol/L;
(3) pulse electromagnetic field is processed
The reaction solution that step (2) is prepared is poured in container, applies pulse electromagnetic field and carries out processing reaction solution, applies Plus burst length 2min~3min, pulse voltage is 500v~700v, and pulse frequency is 3Hz~5Hz;
(4) spin-coating film
By the reaction solution Deca processing through pulse on electro-conductive glass substrate, carry out low speed spin coating respectively and revolve at a high speed Apply, form the perovskite thin film that a layer thickness is 500nm~800nm, wherein, the revolution of low speed spin coating for 800r/min~ 1200r/min, spin-coating time is 20s~30s;The revolution of high speed spin coating is 2500r/min~3500r/min, and spin-coating time is 30s~40s;
(5) make annealing treatment
Liquid film good for spin coating in step (4) is put in vacuum drying oven, is heated to 70 DEG C~80 DEG C, insulation 20min~30min, obtains methyl amine bromination thin film lead.
The thickness of described FTO electro-conductive glass is 3mm~5mm.
During cleaning FTO electro-conductive glass substrate, first it is cleaned by ultrasonic 10min~20min in acetone, more clear in dehydrated alcohol Wash 10min~20min.
Beneficial effects of the present invention:
(1), degree of crystallinity is had using the methyl amine lead bromide organic-inorganic hybrid material of pulse electromagnetic technology preparation high, pure Degree is high, the advantage of compactness;Show that the methyl amine lead bromide organic-inorganic after processing through extra pulse is miscellaneous by thermogravimetric analysis data Change material decomposition temperature and bring up to 381 DEG C from 375 DEG C, UV-visible spectrometer data display extinction width is from 300nm-674nm Bring up to 300nm-685nm, this material has more preferable stability and absorbing properties, be assembled into perovskite solaode, Be conducive to improving battery efficiency and stability.
(2), pulse electromagnetic field technology energy consumption is low, system operatio is simple, operating cost is low, occupation area of equipment is little, parameter Easily adjust, its handled object and surrounding are not polluted, be a kind of processing method of cleaner environmental protection;Using After pulse electromagnetic field is processed, greatly shorten the temperature retention time of annealing, the temperature retention time of annealing is only provided without The 1/6 of pulse electromagnetic field process, thus shortening the production cycle of product, energy saving, is conducive to industrialized production.
Brief description
Fig. 1 is methyl amine lead bromide (CH prepared by the present invention (corresponding embodiment 1~embodiment 3)3NH3PbBr3) hydridization material The XRD spectrum of material;
Fig. 2 is the methyl amine lead bromide (CH being prepared using common liquid phase method (corresponding comparative example 1)3NH3PbBr3) hydridization The XRD spectrum of material.
Specific embodiment
Embodiment 1
(1) clean substrate
FTO electro-conductive glass using thickness as 3mm, as substrate, is first cleaned by ultrasonic 10min in acetone, then in dehydrated alcohol Middle cleaning 10min, last deionized water is rinsed well, dries;
(2) prepare reaction solution
Take the solid methyl ammonium bromide (CH of 0.01mol3NH3Br) and 0.02mol solid brominated Asia lead (PbBr2), add DMF (DMF) solution of 20mL, stirs and all dissolves to pressed powder, obtain reaction solution;
(3) pulse electromagnetic field is processed
The reaction solution that step (2) is prepared is poured in beaker, and it is 500v that reaction solution is applied pulse voltage, electric arteries and veins Rush the pulse electromagnetic field that frequency is 3Hz and process 3min;
(4) spin-coating film
By the reaction solution Deca processing through pulse on electro-conductive glass substrate, carried out respectively with sol evenning machine low speed spin coating and High speed spin coating, forms the perovskite thin film that a layer thickness is 500nm~600nm, and wherein, the revolution of low speed spin coating is 800r/ Min, spin-coating time is 30s;The revolution of high speed spin coating is 2500r/min, and spin-coating time is 40s;
(5) make annealing treatment
Liquid film good for spin coating in step (4) is put in vacuum drying oven, is heated to 70 DEG C, be incubated 20min, obtain Methyl amine lead bromide (CH3NH3PbBr3) thin film, its XRD spectrum as shown in figure 1, as seen from the figure hence it is evident that find diffraction peak intensity relatively Height, the diffraction maximum relative intensity of wherein main diffraction surfaces (110) and (220) is about 11000~14000;Being calculated by XRD can Know, its crystallite dimension is about 96nm;By thermogravimetric analysiss, its decomposition temperature is 381 DEG C;Through UV-visible spectrometer detection, its Show that extinction width is 300nm-685nm.
Embodiment 2
(1) clean substrate
FTO electro-conductive glass using thickness as 4mm, as substrate, is first cleaned by ultrasonic 15min in acetone, then in dehydrated alcohol Middle cleaning 15min, last deionized water is rinsed well, dries;
(2) prepare reaction solution
Take the solid methyl ammonium bromide (CH of 0.01mol3NH3Br) and 0.01mol solid brominated Asia lead (PbBr2), add DMF (DMF) solution of 15mL, stirs and all dissolves to pressed powder, obtain reaction solution;
(3) pulse electromagnetic field is processed
The reaction solution that step (2) is prepared is poured in beaker, and it is 600v that reaction solution is applied pulse voltage, electric arteries and veins Rush the pulse electromagnetic field that frequency is 4Hz and process 150s;
(4) spin-coating film
By the reaction solution Deca processing through pulse on electro-conductive glass substrate, carried out respectively with sol evenning machine low speed spin coating and High speed spin coating, forms the perovskite thin film that a layer thickness is 600nm~700nm, and wherein, the revolution of low speed spin coating is 1200r/ Min, spin-coating time is 20s;The revolution of high speed spin coating is 3500r/min, and spin-coating time is 30s;
(5) make annealing treatment
Liquid film good for spin coating in step (4) is put in vacuum drying oven, is heated to 75 DEG C, be incubated 25min, obtain Methyl amine bromination thin film lead, its XRD spectrum is as shown in Figure 1;By thermogravimetric analysiss, its decomposition temperature is 381 DEG C;Through UV, visible light Spectrometer, it shows that extinction width is 300nm-685nm.
Embodiment 3
(1) clean substrate
FTO electro-conductive glass using thickness as 5mm, as substrate, is first cleaned by ultrasonic 20min in acetone, then in dehydrated alcohol Middle cleaning 20min, last deionized water is rinsed well, dries;
(2) prepare reaction solution
Take the solid methyl ammonium bromide (CH of 0.02mol3NH3Br) and 0.01mol solid brominated Asia lead (PbBr2), add DMF (DMF) solution of 20mL, stirs and all dissolves to pressed powder, obtain reaction solution;
(3) pulse electromagnetic field is processed
The reaction solution that step (2) is prepared is poured in beaker, and it is 700v that reaction solution is applied pulse voltage, electric arteries and veins Rush the pulse electromagnetic field that frequency is 5Hz and process 2min;
(4) spin-coating film
By the reaction solution Deca processing through pulse on electro-conductive glass substrate, carried out respectively with sol evenning machine low speed spin coating and High speed spin coating, forms the perovskite thin film that a layer thickness is 700nm~800nm, and wherein, the revolution of low speed spin coating is 1000r/ Min, spin-coating time is 25s;The revolution of high speed spin coating is 3000r/min, and spin-coating time is 35s;
(5) make annealing treatment
Liquid film good for spin coating in step (4) is put in vacuum drying oven, is heated to 80 DEG C, be incubated 30min, obtain Methyl amine bromination thin film lead, its XRD spectrum is as shown in Figure 1;By thermogravimetric analysiss, its decomposition temperature is 381 DEG C;Through UV, visible light Spectrometer, it shows that extinction width is 300nm-685nm.
Comparative example 1
(1) clean substrate
FTO electro-conductive glass using thickness as 4mm, as substrate, is first cleaned by ultrasonic 15min in acetone, then in dehydrated alcohol Middle cleaning 15min, last deionized water is rinsed well, dries;
(2) prepare reaction solution
Take the solid methyl ammonium bromide (CH of 0.01mol3NH3Br) and 0.01mol solid brominated Asia lead (PbBr2), add DMF (DMF) solution of 15mL, stirs and all dissolves to pressed powder, obtain reaction solution;
(3) spin-coating film
By reaction solution Deca on electro-conductive glass substrate, carry out low speed spin coating and high speed spin coating, shape respectively with sol evenning machine Become the perovskite thin film that a layer thickness is 700nm~800nm, wherein, the revolution of low speed spin coating is 1000r/min, spin-coating time For 25s;The revolution of high speed spin coating is 3000r/min, and spin-coating time is 35s;
(4) make annealing treatment
Liquid film good for spin coating in step (3) is put in vacuum drying oven, is heated to 70 DEG C, be incubated 2h, obtain first Base amine lead bromide (CH3NH3PbBr3) thin film.As shown in Fig. 2 as seen from the figure, the diffraction peak intensity of this product is relatively for its XRD spectrum Adopt in Fig. 1 pulse process the product obtaining diffraction peak intensity relatively low, the spreading out of wherein main diffraction surfaces (110) and (220) Penetrate peak relative intensity and be about 3800~5000;Calculated by XRD, its crystallite dimension is about 53nm;By thermogravimetric analysiss, its Decomposition temperature is 375 DEG C;Through UV-visible spectrometer detection, it shows that extinction width is 300nm-674nm.
Can be obtained by Fig. 1 and Fig. 2 contrast, the crystallite dimension of the embodiment of the present invention 1~embodiment 3 product is much larger than commonly The crystallite dimension of product prepared by liquid phase method (comparative example 1), thus can know, using pulse electromagnetic field technology preparation product its Degree of crystallinity is greatly improved.
These are only the specific embodiment of the present invention, be not limited to the present invention, for those skilled in the art For member, the present invention can have various modifications and variations.All any modifications within the spirit and principles in the present invention, made, Equivalent, improvement etc., should be included within the scope of the present invention.

Claims (3)

1. a kind of preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide, is characterized in that:
Comprise the following steps that:
(1) clean substrate
Using FTO electro-conductive glass as substrate, after acetone and washes of absolute alcohol, then deionized water is rinsed well, dries;
(2) prepare reaction solution
Solid methyl ammonium bromide and solid brominated Asia lead are mixed, is added in DMF solvent, stirring Uniformly, obtain reaction solution, described methyl bromide ammonium is 1 with the mol ratio of protobromide lead:2~2:1, described methyl bromide ammonium with The molal volume of N,N-dimethylformamide is than for 1:1mol/L~1:2mol/L;
(3) pulse electromagnetic field is processed
The reaction solution that step (2) is prepared is poured in container, applies pulse electromagnetic field and carries out processing reaction solution, applies arteries and veins Rush time 2min~3min, pulse voltage is 500v~700v, pulse frequency is 3Hz~5Hz;
(4) spin-coating film
By the reaction solution Deca processing through pulse on electro-conductive glass substrate, carry out low speed spin coating and high speed spin coating, shape respectively Become the perovskite thin film that a layer thickness is 500nm~800nm, wherein, the revolution of low speed spin coating is 800r/min~1200r/ Min, spin-coating time is 20s~30s;The revolution of high speed spin coating be 2500r/min~3500r/min, spin-coating time be 30s~ 40s;
(5) make annealing treatment
Liquid film good for spin coating in step (4) is put in vacuum drying oven, is heated to 70 DEG C~80 DEG C, insulation 20min~ 30min, obtains methyl amine bromination thin film lead.
2. the preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide according to claim 1, It is characterized in that:The thickness of described FTO electro-conductive glass is 3mm~5mm.
3. the preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide according to claim 1, It is characterized in that:During cleaning FTO electro-conductive glass substrate, first it is cleaned by ultrasonic 10min~20min in acetone, then in dehydrated alcohol Cleaning 10min~20min.
CN201510330755.2A 2015-06-12 2015-06-12 A kind of preparation method of perovskite solar cell light absorption layer material methyl amine lead bromide Expired - Fee Related CN104934503B (en)

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CN107464883B (en) * 2015-12-21 2020-05-19 西安穿越光电科技有限公司 Solar cell
WO2018000294A1 (en) * 2016-06-30 2018-01-04 The University Of Hong Kong An organolead halide perovskite film and the method of making the same
CN107134531B (en) * 2017-05-11 2019-06-28 陕西师范大学 A kind of increase perovskite CH3NH3PbI3Crystal grain is to improve the method for film crystalline quality
CN107482121B (en) * 2017-08-01 2019-09-17 厦门大学 A kind of preparation method of the perovskite thin film based on magnetic field regulation
CN109037459B (en) * 2018-08-03 2022-03-11 辽宁工业大学 Preparation method of high-purity perovskite film

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CN104269452A (en) * 2014-10-11 2015-01-07 中国科学院半导体研究所 Perovskite solar battery made of silicon-based thin-film materials and manufacturing method thereof

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