CN107359252A - A kind of preparation method of crystal isotypy perovskite thin film - Google Patents
A kind of preparation method of crystal isotypy perovskite thin film Download PDFInfo
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- CN107359252A CN107359252A CN201710424348.7A CN201710424348A CN107359252A CN 107359252 A CN107359252 A CN 107359252A CN 201710424348 A CN201710424348 A CN 201710424348A CN 107359252 A CN107359252 A CN 107359252A
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Abstract
The present invention relates to a kind of preparation method of crystal isotypy perovskite thin film, belong to solar energy materials preparing technical field.The present invention is adsorbed with the zeolite of sensitizing dyestuff by preparing doping in electrolyte colloidal sol, due to the high sensitizing dyestuff loaded in zeolite pores, charge recombination speed is high in effectively modified electrolyte, the electrical contact difference problem such as low with electrical conductivity, simultaneously because electrolyte spin coating is as basalis, lead halide is set to penetrate into the inside of mesoporous layer as far as possible, as perovskite film electron transfer layer, make that perovskite film particle size distribution is uniform and surface is smooth, the light absorpting ability of enhanced film, improve charge transport ability, electric charge is set effectively to be transmitted in perovskite thin film, suppress Interface composites, reduce loss of charge, realize effective control to perovskite crystalline and film morphology, improve solar cell service efficiency, with wide prospect of the application.
Description
Technical field
The present invention relates to a kind of preparation method of crystal isotypy perovskite thin film, belongs to solar energy materials technology of preparing neck
Domain.
Background technology
In recent years, thin-film solar cells high speed development, it is divided into amorphous silicon thin-film solar cell, polycrystalline osmanthus film too
Positive energy battery, GaAs thin-film solar cells, CuInSes thin-film solar cells etc., especially Ca-Ti ore type solar cell
With its it is unique the advantages of, attracted the research of numerous scholars.And the development advanced by leaps and bounds is achieved in recent years, its light
Photoelectric transformation efficiency increases to of today more than 20% from 3.8% in 2009.High efficiency, low cost, technique are relatively easy, low stain
The advantages of so that Ca-Ti ore type solar cell obtains broad development, has huge application value.In energy growing tension,
Today that environmental problem increasingly highlights, Development of Novel, perovskite solar cell efficiently, environmentally friendly are particularly important.
In the course of work of perovskite solar cell, as light absorbing layer, i.e. active layer serves point calcium nutrition film
From the effect in electronics and hole, therefore the quality of perovskite film forming affects the performance of device to a certain extent.Evaluate calcium iron
The factor of ore deposit film quality includes distribution hook degree and size, the thickness of film and its coverage rate etc. of the defects of material degree, crystal grain.
If perovskite film will not exclusively produce larger leakage current to substrate covering, so as to cause the open circuit of battery, therefore
The quality for changing titanium ore active layer quality concerns the success or failure of whole battery.But in existing preparation process, but due in film
In forming process, solvent volatilization is fast, rapid, lead halide and the CH of solution concentration3NH3I reactions are very fast to wait the calcium that can all result in
Iron ore crystal size is uneven, and this can make it that calcium nutrition film is bad to the level of coverage of substrate, causes photoelectricity transmission inefficient, shadow
Ring solar cell working performance.
It would therefore be highly desirable to developing a kind of perovskite thin film of photoelectricity transmission excellent in efficiency has necessary meaning.
The content of the invention
The technical problems to be solved by the invention：For calcium nutrition crystal size in existing perovskite thin film preparation process not
It is homogeneous so that calcium nutrition film is bad to the level of coverage of substrate, causes photoelectricity transmission inefficient problem, there is provided a kind of crystal is equal
The preparation method of one type perovskite thin film.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）10~15g titanium dioxide granules are taken, ball milling crosses 200 mesh sieves and obtains titania powder, in mass ratio 1:100, by dioxy
Change titanium powder and simultaneously ultrasonic disperse is mixed with acetonitrile, obtain mixed dispersion liquid, weigh 100~105mL mixed dispersion liquids and 10~20g points
Polyethylene glycol oxide 4~6h of heating water bath that son amount is 4000000, then be to adding 10~20g molecular weight in three-necked flask
534000 Kynoar, 10~12h of insulated and stirred, filter to get filtrate, and rotary evaporation is prepared into modified concentrate；
（3）5~6gN719 ruthenium dyes, 150~200mL tert-butyl alcohols and 180~220mL acetonitriles is weighed respectively to be stirred and add
5~10g zeolites, are stirred and filter and to obtain filter cake, and washing drying is prepared into modified adsorption particle, in mass ratio 1:5, by modification
Adsorption particle is stirred with modified concentrate, and ball milling crosses 500 mesh sieves, obtains electrolyte dye-sensitized slurries；
（3）Dried and clean glass plate is chosen, by the screen process press brushing to dried and clean glass of electrolyte dye-sensitized slurries
Plate surface, stand and solidify and be incubated calcining, obtain mesopore film sensitization modified layer, take 200~250mgPbI2Added to 500~600
μ LN, in dinethylformamide, substrate spin coating liquid is stirred to obtain, takes 65~70 μ L substrate spin coating liquid to be spin-coated to sol evenning machine
The modified layer surface of mesopore film sensitization, dries and stands and be cooled to room temperature, washs and simultaneously dries, you can it is homogeneous to be prepared into a kind of crystal
Type perovskite thin film.
Step（3）Described electrolyte dye-sensitized slurries brushing thickness is 0.25~0.28mm.
Step（3）Described washing step is, after first being rinsed 3~5 times with isopropanol, then with concentration is respectively 8g/L's
CH3NH3I solution and isopropanol rinse 45~60s.
Compared with other method, advantageous effects are the present invention：
（1）The present invention is adsorbed with the zeolite of sensitizing dyestuff by being adulterated in electrolyte colloidal sol, because sized zeolite particles size is homogeneous,
And zeolite crystal is uniformly dispersed, forms it into and stablize complete clad, simultaneously because the high sensitization dye loaded in zeolite pores
Material, the problems such as charge recombination speed is high, electrical contact difference is low with electrical conductivity are effectively modified in electrolyte；
（2）The present invention, as basalis, is made lead halide penetrate into the inside of mesoporous layer as far as possible, turned into using electrolyte spin coating
Perovskite film electron transfer layer, makes that perovskite film particle size distribution is uniform and surface is smooth, the light absorpting ability of enhanced film,
Charge transport ability is improved, electric charge is effectively transmitted in perovskite thin film, suppresses Interface composites, reduces loss of charge, is realized
Effective control to perovskite crystalline and film morphology, greatly improves solar cell service efficiency.
Embodiment
10~15g titanium dioxide granules are weighed first, are placed on 3~5h of ball milling in ball grinder, are crossed 200 mesh sieves and are obtained dioxy
Change titanium powder, in mass ratio 1:100, titania powder is mixed with acetonitrile be placed in ultrasonic disperse 10 under 250~300W~
15min, it is prepared into mixed dispersion liquid；It is 4000000 to weigh 100~105mL mixed dispersion liquids and 10~20g molecular weight respectively
Polyethylene glycol oxide is placed in 1000mL three-necked flasks, 4~6h of heating water bath at 75~85 DEG C, after the completion for the treatment of heating water bath, then
It is 534000 Kynoar to adding 10~20g molecular weight in three-necked flask, insulated and stirred is reacted 10~12h, filtered while hot
Filtrate, filtrate is placed at 45~50 DEG C rotation and is evaporated to the 1/8 of filtrate volume, is prepared into modified concentrate；5 are weighed respectively
~6gN719 ruthenium dyes, 150~200mL tert-butyl alcohols and 180~220mL acetonitriles are placed in 1L conical flasks, are stirred and are incited somebody to action
Three-necked flask is placed in 45~50 DEG C of water-baths, after being incubated 15~20min, to adding 5~10g zeolites in conical flask, again
2~3h of insulated and stirred；After the completion for the treatment of insulated and stirred, filter cake is filtered to obtain, with deionized water rinsing 3~5 times, then at 75~80 DEG C
6~8h is dried, is prepared into modified adsorption particle, in mass ratio 1:5, modified adsorption particle and modified concentrate are stirred simultaneously
It is placed in ball grinder, 3~5h of ball milling under 350~400r/min, crosses 500 mesh sieves, be prepared into electrolyte dye-sensitized slurries；Choosing
Dried and clean glass plate is taken, by the screen process press brushing to dried and clean glass pane surface of electrolyte dye-sensitized slurries, control
Coating thickness processed is 0.25~0.28mm, and after the completion of to be coated, after standing 2~3h of solidification at room temperature, glass plate is placed in into horse
Not in stove, by 5 DEG C/min heating rates from room temperature to 250~300 DEG C, after 25~30min of insulation calcining, standing is cooled to
Room temperature, it is prepared into mesopore film sensitization modified layer；Weigh 200~250mgPbI2Added to 500~600 μ LN, N- dimethyl methyls
In acid amides, 10~12h is stirred at 70~75 DEG C, is prepared into substrate spin coating liquid, weighs the substrate rotation of 65~70 μ L preparations
Masking liquid is spin-coated to the modified layer surface of mesopore film sensitization with sol evenning machine, coat be placed at 75~80 DEG C after 30s dry 25~
30min；After the completion of to be dried, standing is cooled to room temperature, after being rinsed 3~5 times with isopropanol, then with concentration is respectively 8g/L's
CH3NH3I solution and isopropanol rinse 45~60s, after the completion of to be rinsed, then 25~30min are dried under 75~80 DEG C of roasting glue machines,
A kind of crystal isotypy perovskite thin film can be prepared into.
Example 1
10g titanium dioxide granules are weighed first, are placed on ball milling 3h in ball grinder, are crossed 200 mesh sieves and are obtained titania powder, press
Mass ratio 1:100, titania powder is mixed with acetonitrile and is placed in ultrasonic disperse 10min under 250W, it is scattered to be prepared into mixing
Liquid；100mL mixed dispersion liquids and 10g molecular weight are weighed respectively is placed in 1000mL three-necked flasks for 4000000 polyethylene glycol oxide
In, the heating water bath 4h at 75 DEG C, after the completion for the treatment of heating water bath, then it is 534000 poly- to adding 10g molecular weight in three-necked flask
Vinylidene, insulated and stirred reaction 10h, the filtrate filtered while hot, filtrate is placed in rotation at 45 DEG C and is evaporated to filtrate volume
1/8, it is prepared into modified concentrate；5gN719 ruthenium dyes, the 150mL tert-butyl alcohols and 180mL acetonitriles are weighed respectively is placed in 1L triangles burning
In bottle, it is stirred and three-necked flask is placed in 45 DEG C of water-baths, after being incubated 15min, to adding 5g zeolites in conical flask,
Insulated and stirred 2h again；After the completion for the treatment of insulated and stirred, filter cake is filtered to obtain, with deionized water rinsing 3 times, then is dried at 75 DEG C
6h, it is prepared into modified adsorption particle, in mass ratio 1:5, modified adsorption particle is stirred with modified concentrate and is placed in ball
In grinding jar, the ball milling 3h under 350r/min, 500 mesh sieves are crossed, are prepared into electrolyte dye-sensitized slurries；Choose dried and clean glass
Plate, by the screen process press brushing to dried and clean glass pane surface of electrolyte dye-sensitized slurries, the coating thickness is controlled to be
0.25mm, after the completion of to be coated, after standing solidification 2h at room temperature, glass plate is placed in Muffle furnace, heated up by 5 DEG C/min fast
Rate is from room temperature to 250 DEG C, and after insulation calcining 25min, standing is cooled to room temperature, is prepared into mesopore film sensitization modified layer；
Weigh 200mgPbI2Added to 500 μ LN, in dinethylformamide, 10h is stirred at 70 DEG C, is prepared into substrate spin coating
Liquid, the substrate spin coating liquid for weighing 65 μ L preparations are spin-coated to the modified layer surface of mesopore film sensitization with sol evenning machine, coat it after 30s
It is placed at 75 DEG C and dries 25min；After the completion of to be dried, standing is cooled to room temperature, after being rinsed 3 times with isopropanol, then respectively with dense
Spend the CH for 8g/L3NH3I solution and isopropanol rinse 45s, after the completion of to be rinsed, then 25min are dried under 75 DEG C of roasting glue machines, i.e.,
A kind of crystal isotypy perovskite thin film can be prepared into.
By order from bottom to top, the calcium titanium for successively preparing FTO electro-conductive glass, electron transfer layer zinc oxide, the present invention
Ore deposit coating, hole transmission layer p-type spiro-OMeTAD and metal electrode Au are assembled, and are prepared into perovskite solar cell,
The solar cell parameter of crystal isotypy perovskite thin film application prepared by the present invention is Jsc=6.88mA/cm2, Voc=
0.58V, FF=0.38, PCE=1.28%, while electricity conversion are high, up to 12.5%, while after 50 days, photoelectric conversion effect
Rate is 12.1%, and conversion ratio has wide prospect of the application without being decreased obviously.
Example 2
13g titanium dioxide granules are weighed first, are placed on ball milling 4h in ball grinder, are crossed 200 mesh sieves and are obtained titania powder, press
Mass ratio 1:100, titania powder is mixed with acetonitrile and is placed in ultrasonic disperse 13min under 280W, it is scattered to be prepared into mixing
Liquid；103mL mixed dispersion liquids and 15g molecular weight are weighed respectively is placed in 1000mL three-necked flasks for 4000000 polyethylene glycol oxide
In, the heating water bath 5h at 80 DEG C, after the completion for the treatment of heating water bath, then it is 534000 poly- to adding 15g molecular weight in three-necked flask
Vinylidene, insulated and stirred reaction 11h, the filtrate filtered while hot, filtrate is placed in rotation at 48 DEG C and is evaporated to filtrate volume
1/8, it is prepared into modified concentrate；6gN719 ruthenium dyes, the 180mL tert-butyl alcohols and 200mL acetonitriles are weighed respectively is placed in 1L triangles burning
In bottle, it is stirred and three-necked flask is placed in 48 DEG C of water-baths, after being incubated 18min, to adding 8g zeolites in conical flask,
Insulated and stirred 3h again；After the completion for the treatment of insulated and stirred, filter cake is filtered to obtain, with deionized water rinsing 4 times, then is dried at 78 DEG C
7h, it is prepared into modified adsorption particle, in mass ratio 1:5, modified adsorption particle is stirred with modified concentrate and is placed in ball
In grinding jar, the ball milling 4h under 380r/min, 500 mesh sieves are crossed, are prepared into electrolyte dye-sensitized slurries；Choose dried and clean glass
Plate, by the screen process press brushing to dried and clean glass pane surface of electrolyte dye-sensitized slurries, the coating thickness is controlled to be
0.27mm, after the completion of to be coated, after standing solidification 3h at room temperature, glass plate is placed in Muffle furnace, heated up by 5 DEG C/min fast
Rate is from room temperature to 280 DEG C, and after insulation calcining 28min, standing is cooled to room temperature, is prepared into mesopore film sensitization modified layer；
Weigh 230mgPbI2Added to 550 μ LN, in dinethylformamide, 11h is stirred at 73 DEG C, is prepared into substrate spin coating
Liquid, the substrate spin coating liquid for weighing 68 μ L preparations are spin-coated to the modified layer surface of mesopore film sensitization with sol evenning machine, coat it after 30s
It is placed at 78 DEG C and dries 28min；After the completion of to be dried, standing is cooled to room temperature, after being rinsed 4 times with isopropanol, then respectively with dense
Spend the CH for 8g/L3NH3I solution and isopropanol rinse 52s, after the completion of to be rinsed, then 28min are dried under 78 DEG C of roasting glue machines, i.e.,
A kind of crystal isotypy perovskite thin film can be prepared into.
By order from bottom to top, the calcium titanium for successively preparing FTO electro-conductive glass, electron transfer layer zinc oxide, the present invention
Ore deposit coating, hole transmission layer p-type spiro-OMeTAD and metal electrode Au are assembled, and are prepared into perovskite solar cell,
The solar cell parameter of crystal isotypy perovskite thin film application prepared by the present invention is Jsc=6.99mA/cm2, Voc=
0.62V, FF=0.39, PCE=1.29%, while electricity conversion are high, up to 12.7%, while after 50 days, photoelectric conversion effect
Rate is 12.8%, and conversion ratio has wide prospect of the application without being decreased obviously.
Example 3
15g titanium dioxide granules are weighed first, are placed on ball milling 5h in ball grinder, are crossed 200 mesh sieves and are obtained titania powder, press
Mass ratio 1:100, titania powder is mixed with acetonitrile and is placed in ultrasonic disperse 15min under 300W, it is scattered to be prepared into mixing
Liquid；105mL mixed dispersion liquids and 20g molecular weight are weighed respectively is placed in 1000mL three-necked flasks for 4000000 polyethylene glycol oxide
In, the heating water bath 6h at 85 DEG C, after the completion for the treatment of heating water bath, then it is 534000 poly- to adding 20g molecular weight in three-necked flask
Vinylidene, insulated and stirred reaction 12h, the filtrate filtered while hot, filtrate is placed in rotation at 50 DEG C and is evaporated to filtrate volume
1/8, it is prepared into modified concentrate；6gN719 ruthenium dyes, the 200mL tert-butyl alcohols and 220mL acetonitriles are weighed respectively is placed in 1L triangles burning
In bottle, it is stirred and three-necked flask is placed in 50 DEG C of water-baths, after being incubated 20min, to adds 10g boilings in conical flask
Stone, again insulated and stirred 3h；After the completion for the treatment of insulated and stirred, filter cake is filtered to obtain, with deionized water rinsing 5 times, then is done at 80 DEG C
Dry 8h, it is prepared into modified adsorption particle, in mass ratio 1:5, modified adsorption particle is stirred with modified concentrate and is placed in
In ball grinder, the ball milling 5h under 400r/min, 500 mesh sieves are crossed, are prepared into electrolyte dye-sensitized slurries；Choose dried and clean glass
Glass plate, by the screen process press brushing to dried and clean glass pane surface of electrolyte dye-sensitized slurries, the coating thickness is controlled to be
0.28mm, after the completion of to be coated, after standing solidification 3h at room temperature, glass plate is placed in Muffle furnace, heated up by 5 DEG C/min fast
Rate is from room temperature to 300 DEG C, and after insulation calcining 30min, standing is cooled to room temperature, is prepared into mesopore film sensitization modified layer；
Weigh 250mgPbI2Added to 600 μ LN, in dinethylformamide, 12h is stirred at 75 DEG C, is prepared into substrate spin coating
Liquid, the substrate spin coating liquid for weighing 70 μ L preparations are spin-coated to the modified layer surface of mesopore film sensitization with sol evenning machine, coat it after 30s
It is placed at 80 DEG C and dries 30min；After the completion of to be dried, standing is cooled to room temperature, after being rinsed 5 times with isopropanol, then respectively with dense
Spend the CH for 8g/L3NH3I solution and isopropanol rinse 60s, after the completion of to be rinsed, then 30min are dried under 80 DEG C of roasting glue machines, i.e.,
A kind of crystal isotypy perovskite thin film can be prepared into.
By order from bottom to top, the calcium titanium for successively preparing FTO electro-conductive glass, electron transfer layer zinc oxide, the present invention
Ore deposit coating, hole transmission layer p-type spiro-OMeTAD and metal electrode Au are assembled, and are prepared into perovskite solar cell,
The solar cell parameter of crystal isotypy perovskite thin film application prepared by the present invention is Jsc=7.22mA/cm2, Voc=
0.65V, FF=0.42, PCE=1.32%, while electricity conversion are high, up to 13.8%, while after 50 days, photoelectric conversion effect
Rate is 13.5%, and conversion ratio has wide prospect of the application without being decreased obviously.
The solar cell of crystal isotypy perovskite thin film obtained by above-described embodiment will be used with using metal-doped calcium
The solar cell of titanium ore film is detected, and is contrasted, as a result as shown in Table 1.
Table one：
| Example | Jsc（mA/cm2） | Voc（V） | FF | PCE（%） | Electricity conversion（%） | Use the electricity conversion after 50 days（%） |
| Metal-doped perovskite thin film | 6.36~6.82 | 0.49~0.57 | 0.31~0.35 | 1.18~1.26 | 10.9~11.8 | 11.0~11.9 |
| Example 1 | 6.88 | 0.58 | 0.38 | 1.28 | 12.5 | 12.1 |
| Example 2 | 6.99 | 0.62 | 0.39 | 1.29 | 12.7 | 12.8 |
| Example 3 | 7.22 | 0.65 | 0.42 | 1.32 | 13.8 | 13.5 |
As seen from the above table, crystal isotypy perovskite thin film photoelectricity transmission efficiency high of the present invention, obtained solar cell parameter
For Jsc=6.88~7.22mA/cm2, Voc=0.58~0.65V, FF=0.38~0.42, PCE=1.28~1.32%, while photoelectricity
Transformation efficiency is high, and up to 12.5~13.8%, after 50 days, electricity conversion is 12.1~13.5%.
Calcium nutrition crystal size is homogeneous in crystal isotypy perovskite thin film preparation process obtained by the above embodiment of the present invention,
Particle diameter is 60~100nm.
Claims (3)
1. a kind of preparation method of crystal isotypy perovskite thin film, it is characterised in that specifically preparation process is：
（1）10~15g titanium dioxide granules are taken, ball milling crosses 200 mesh sieves and obtains titania powder, in mass ratio 1:100, by dioxy
Change titanium powder and simultaneously ultrasonic disperse is mixed with acetonitrile, obtain mixed dispersion liquid, weigh 100~105mL mixed dispersion liquids and 10~20g points
Polyethylene glycol oxide 4~6h of heating water bath that son amount is 4000000, then be to adding 10~20g molecular weight in three-necked flask
534000 Kynoar, 10~12h of insulated and stirred, filter to get filtrate, and rotary evaporation is prepared into modified concentrate；
（3）5~6gN719 ruthenium dyes, 150~200mL tert-butyl alcohols and 180~220mL acetonitriles is weighed respectively to be stirred and add
5~10g zeolites, are stirred and filter and to obtain filter cake, and washing drying is prepared into modified adsorption particle, in mass ratio 1:5, by modification
Adsorption particle is stirred with modified concentrate, and ball milling crosses 500 mesh sieves, obtains electrolyte dye-sensitized slurries；
（3）Dried and clean glass plate is chosen, by the screen process press brushing to dried and clean glass of electrolyte dye-sensitized slurries
Plate surface, stand and solidify and be incubated calcining, obtain mesopore film sensitization modified layer, take 200~250mgPbI2Added to 500~600
μ LN, in dinethylformamide, substrate spin coating liquid is stirred to obtain, takes 65~70 μ L substrate spin coating liquid to be spin-coated to sol evenning machine
The modified layer surface of mesopore film sensitization, dries and stands and be cooled to room temperature, washs and simultaneously dries, you can it is homogeneous to be prepared into a kind of crystal
Type perovskite thin film.
A kind of 2. preparation method of crystal isotypy perovskite thin film according to claim 1, it is characterised in that：Step
（3）Described electrolyte dye-sensitized slurries brushing thickness is 0.25~0.28mm.
A kind of 3. preparation method of crystal isotypy perovskite thin film according to claim 1, it is characterised in that：Step
（3）Described washing step is, after first being rinsed 3~5 times with isopropanol, then the CH for being respectively 8g/L with concentration3NH3I solution and different
Propyl alcohol rinses 45~60s.
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| CN110311060A (en) * | 2019-08-05 | 2019-10-08 | 广东省半导体产业技术研究院 | A kind of perovskite LED component and its preparation method for inhibiting crystalline size |
| CN111103274A (en) * | 2019-12-23 | 2020-05-05 | 厦门大学 | Method for rapidly detecting lead ions in sample liquid |
| CN111740017A (en) * | 2020-08-06 | 2020-10-02 | 江西省科学院能源研究所 | Method for preparing perovskite solar cell light absorption layer film |
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