CN105870328B - A kind of preparation method of the perovskite solar cell light absorption layer of stabilization - Google Patents
A kind of preparation method of the perovskite solar cell light absorption layer of stabilization Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of the perovskite solar cell light absorption layer of the stabilization using organic silicon nano particle as dispersant and protective film.First by PbI2And CH3NH3I solids are added in dimethylformamide organic solvents, and reaction dissolving obtains CH3NH3PbI3Solution；The ethanol solution of organic silicon nano particle dispersant solution and curing agent is added, secondary filter obtains light absorbing layer coating fluid；It is dropped in glove box in the Conducting Glass of compacted zone, is coated with bar spreader uniform, solvent volatilization repeats to be coated with after drying, and finally uses 90 110 DEG C of heated-air dryings 30 minutes, forms smooth surface and the uniform black perovskite light absorbing layer of crystallization.After perovskite light absorbing layer places 30 days in air, significant change does not occur for surface color, sheet resistance and water contact angle, has good chemical stability.
Description
Technical field
The present invention relates to a kind of preparation methods of the perovskite solar cell light absorption layer of stabilization, are especially received with organosilicon
Preparation method of the rice corpuscles as dispersant and the perovskite solar cell light absorption layer of protective film, belongs to new energy and new material
Field.
Technical background
The solar cell prepared based on organic metal halide perovskite structure light absorbing material is referred to as perovskite too
Positive electricity pond, more than 20%, future is expected to reach 50% its photoelectric conversion efficiency at present, can be made into colorful film battery dress in the future
Decorations are mounted on building surface and promote integrated photovoltaic architectural development.Although perovskite photoelectric conversion efficiency of the solar battery data are just
Constantly refreshing, but it is expanded in research and industrialization there are the problem of non-enough attention.
Halide perovskite light absorbing material CH3NH3PbI3Because having, absorbing properties are good, preparation condition is mild, photoelectricity
The high characteristic of transformation efficiency becomes most promising perovskite battery light absorbing material.But it is in moisture, air, ultraviolet
It is easy to decompose under light, organic solvent or catalyst action, seriously affects perovskite solar cell light absorption layer stability.
Heliotechnics is developed and three big key elements of industrialization are photoelectric conversion efficiency, production cost and cell performance
Stabilizability.Perovskite efficiency of solar cell has been approached commercialized crystal-silicon solar cell, and preparation process is also uncomplicated, it is contemplated that
Manufacturing cost is relatively low, and the long-time stability of perovskite solar cell performance in an outdoor environment will be as its industrialization development
Biggest obstacle, and the stability of perovskite light absorbing layer is crucial.
To improve the stability of perovskite light absorbing layer, ISIS INNOVATION companies of Britain patent of invention US
2015129034（ 2015-05-14）Disclosure is with nanometer Al2O3Casing play replaces nano-TiO2Casing play, it is suppressed that nano-TiO2
To CH3NH3PbI3The photocatalysis Decomposition of perovskite light absorbing layer.University Of Ningbo patent of invention CN104576930（2015-04-29）
The open CH by preparation3NH3PbI3Perovskite light absorbing layer uses the aqueous isopropanol dipping post-processing of long chain silane coupling agent again,
Perovskite light absorbing layer surface hydrophobic is set to enhance, to improve its stability in wet condition.Tsinghua University's patent of invention
Apply for CN104733183（2015-06-24）It is open to use nano-TiO2 / perovskite light absorbing material/nanometer Al2O3The double-deck bone
Frame, nanometer Al therein2O3Layer mainly play protective layer, can prevent with the contact with moisture in air, prevent that performance declines
It moves back.But these patent corrective measures make the preparation process of titanium ore light absorbing layer more complicate.
In addition, existing one step technique prepares CH3NH3PbI3Perovskite light absorbing layer rough surface is uneven, and photoelectricity turns
It changes inefficient；CH is prepared in situ in existing two step method technology3NH3PbI3Perovskite light absorbing layer process control condition is complicated, uncomfortable
It closes and expands research and commercial application.To improve the uniformity of perovskite light absorbing layer, Tianjin Professional College patent application
2016102050822（2016-04-06）In, using silver iodide as CH3NH3PbI3Derivant is crystallized, a step obtains smooth surface
With the uniform perovskite light absorbing layer of crystallization.Nankai University patent of invention CN104218109 (2014-12-17) is disclosed in calcium
A small amount of polyvinylpyrrolidone, which is added, in titanium ore light absorbing layer coating fluid increases CH3NH3PbI3Crystallinity and film layer covering
Rate.
Invention content
It is an object of the present invention to provide a kind of using organic silicon nano particle as the perovskite sun electricity of dispersant and protective film
The preparation method of pond light absorbing layer overcomes perovskite light absorbing layer prepared by existing method unstable in air and rough surface
Non-uniform defect.
The principle of the present invention is in CH3NH3I and PbI2Reaction solution in organic silicon nano particle is added as dispersant,
Perovskite light absorbing layer coating fluid is improved to skeleton nano-TiO2The adhesive force and coverage on surface, and it is adsorbed on PbI2With
CH3NH3PbI3Crystal surface interferes it to generate big crystal grain；When perovskite light absorbing layer coating fluid volatile dry, in coating fluid
CH3NH3I and a large amount of tiny PbI2Crystal seed coordination, hydrogen bond, Van der Waals force it is common driving under, occur self-assembling reaction
It forms smooth surface and crystallizes uniform CH3NH3PbI3Perovskite light absorbing layer；The organosilicon for being adsorbed on light absorbing layer surface is received
The further cross-linked polymeric of rice corpuscles dispersant forms organosilicon nano protective film.Organic silicon nano protects film surface to have centainly
Hydrophobicity, the moisture resistance of perovskite light absorbing layer can be improved in perovskite light absorbing layer adsorption in moisture in blocks air
Energy；Organic silicon nano protective film is coated on skeleton nano-TiO2On, reduce its ultraviolet catalytic to perovskite light absorbing layer
It decomposes, the chemical stability of perovskite light absorbing layer can be improved.
Perovskite solar cell light absorption layer coating fluid of the present invention is by PbI2、CH3NH3I, organosilicone spreading agent, curing agent and
Organic solvent forms, and mass percent is as follows shared by each component：
PbI2 2.9%-14.5%
CH3NH3I 1%-5%
Organosilicone spreading agent 0.3%-1.5%
Curing agent 0-0.5%
Organic solvent surplus.
PbI in perovskite solar cell light absorption layer coating fluid2And CH3NH3I is primary raw material, and molar ratio control is resonable
By metering ratio 1:Near 1-1.05, to cancel the cleaning removal step of excess raw material.
Organosilicone spreading agent is the common organic silicon monomer organic silicon nano particle that acidic hydrolysis generates in alcohol solvent
Solution, to PbI2Crystal seed and CH3NH3PbI3Dispersion and buffer action have been crystallized, crystallization can be blocked and excessively grown up, calcium titanium can be improved
Adhesive force and coverage of the mine light absorbing layer on skeleton surface, select its mass percentage concentration 0.3%-1.5%.It is common organic
Silicon monomer include tetraethoxysilane, methyltriethoxysilane, dimethyl diethoxysilane, organo-silicon coupling agent KH550,
Or mixtures thereof organo-silicon coupling agent KH560, organo-silicon coupling agent KH570.
Common Curing Agents are organic amine, organic metal or coupling agent；Organosilicon containing amino, epoxy group isoreactivity group
Dispersant can be cured with self-crosslinking；PbI2 、CH3NH3I and CH3NH3PbI3It can also be used as organosilicon curing agent.But additional chemistry
Curing agent can promote and adjust the film-forming speed of organosilicone spreading agent.Common curing agent includes methylamine, ethylenediamine, trimerization
Cyanamide, normal-butyl tin, aluminium acetylacetonate, organo-silicon coupling agent KH550, organo-silicon coupling agent KH560 etc..
Organic solvent is can to dissolve PbI2And CH3NH3PbI3Polar solvent dimethylformamide and as diluent
C3-C6 alcohols, C3-C6 ether solvents.
CH in perovskite solar cell light absorption layer coating fluid3NH3PbI3Mass percentage concentration 3%-20% is selected more highly concentrated
Degree can reduce organic solvent consumption and improve the thicknesses of layers that single application is formed, and select low concentration that can repeatedly be applied
Cloth and prevent because crystallization volatilization it is too fast caused by film surface it is coarse and uneven.
Raw material PbI2It is commercially available chemical reagent or is prepared with liquor kalii iodide and lead acetate solution reaction.By iodate when preparation
Potassium is dissolved in hot water, and acetate trihydrate lead water solution is slowly added into the liquor kalii iodide under stirring.Gained precipitation water
After decantation washing, is filtered with Buchner funnel, then precipitation is placed on wet-strong paper and is spread out, it is dry at 80~90 DEG C to form iodine
Change leading crystal.
Raw material CH3NH3I is commercially available chemical reagent or is prepared with methylamine solution and hydroiodic acid solution reaction.It will when preparation
CH3NH2It is added in methanol solution with HI, the reaction generation CH at 0 DEG C3NH3I, the vacuum distillation removing solvent at 50 DEG C,
CH3NH3I crude products recrystallize in ether and alcohol solvent, are dried in vacuo at 60 DEG C and obtain CH3NH3I powder.
Raw material organic silicon monomer tetraethoxysilane, methyltriethoxysilane, dimethyl diethoxysilane, organosilicon
Coupling agent KH550, organo-silicon coupling agent KH560, organo-silicon coupling agent KH570 are commercially available chemical reagent.
Raw material curing agent methylamine, ethylenediamine, melamine, normal-butyl tin, aluminium acetylacetonate, organo-silicon coupling agent KH550,
Organo-silicon coupling agent KH560 etc. is commercially available chemical reagent.
Organic solvent dimethylformamide, C3-C6 alcohol, C3-C6 ethers are commercially available chemical reagent.
The object of the present invention is to provide a kind of preparation method of the perovskite solar cell light absorption layer of stabilization, the skill taken
Art scheme and implementation steps are：
（1）By PbI2And CH3NH3I solids are added in dimethylformamide organic solvents, control PbI2And CH3NH3I's rubs
You are than being 1:1-1.05, reacts 12-24 h at 60 DEG C, and filtering obtains the CH of mass percentage concentration 4%-30%3NH3PbI3It is molten
Liquid；
（2）Organic silicon monomer is mixed with absolute ethyl alcohol, adds deionized water and hydriodic acid aqueous solution, control raw material rubs
You are at ratio：Organic silicon monomer：Absolute ethyl alcohol：Water：HI = 1：50-100：4-10：0.01-0.2 is hydrolyzed at 20-70 DEG C
Reaction 2-12 hours, obtains organic silicon nano particle dispersant solution；
（3）Under stiring to CH3NH3PbI3Organic silicon nano particle dispersant solution is added in clear solution, control is organic
Silicon dispersant mass percentage concentration is 0.3%-1.5%, obtains the CH containing organosilicone spreading agent3NH3PbI3Clear solution；
（4）Under stiring to the CH containing organosilicone spreading agent3NH3PbI3The ethanol solution of curing agent is added in clear solution,
The mass percentage concentration for controlling curing agent is 0-0.5%, adds organic solvent adjustment solution concentration, and secondary filter solution obtains
Light absorbing layer coating fluid；
（5）Light absorbing layer coating fluid is dropped in the Conducting Glass of compacted zone with needle tubing in glove box, uses line
The coating of rod coating device is uniform, and solvent volatilization repeats to be coated with after drying, and so that perovskite light absorbing layer thickness is reached 500-600nm, most
90-110 DEG C of heated-air drying is used afterwards 30 minutes, form smooth surface and crystallize uniform black perovskite light absorbing layer；
（6）The perovskite light absorbing layer sheet resistance 8-15 Ω of preparation, 85-105 ° of water contact angle place 30 in air
After it, surface color, sheet resistance and water contact angle do not change.
Beneficial effects of the present invention are embodied in：
（1）For the present invention using organic silicon nano particle as dispersant, the perovskite light absorbing layer smooth surface of formation is uniform,
The non-uniform defect of light absorbing layer rough surface for overcoming existing one step technique to prepare；
（2）The present invention improves the humidity of perovskite light absorbing layer using organic silicon nano particle as hydrophobic protective film
Performance and UV Aging Resistance, perovskite light absorbing layer have good chemical stability；
（3）The present invention prepares perovskite light absorbing layer and hydrophobic protection film preparation is combined into one, and preparation process is easy, holds
Easy commercial application.
Specific implementation mode
Embodiment 1
By PbI2Reagent 46.1g（100mmol）And CH3NH3I reagents 15.9g（100mmol）200g dimethyl formyls are added
In amine solvent, at 60-70 DEG C at stir 12 h, obtain CH3NH3PbI3Clear solution.
By methyltriethoxysilane 0.89g（5mmol）, absolute ethyl alcohol 16g（350mmol）, deionized water 0.75g
（40mmol）Mixing, adds the hydriodic acid aqueous solution 0.25g of mass percentage concentration 50%（1mmol）, it is 2-3 to make pH value of solution,
Reaction 4 hours is hydrolyzed at 60-70 DEG C, obtains the organic silicon nano particle dispersant solution of mass percentage concentration 5%.It is stirring
It mixes down and is added into CH3NH3PbI3The CH containing organosilicone spreading agent is obtained in solution3NH3PbI3Clear solution.Then matter is added
The normal-butyl tin ethanol solution 1g for measuring percentage concentration 5% adds anhydrous ethanol solvent and adjusts solution quality to 310g, secondary filter
Solution obtains light absorbing layer coating fluid, is transferred in black plastic bottle and preserves.
Light absorbing layer coating fluid is dropped in the 100mm ╳ 100mm fluorine-doped tin dioxide electro-conductive glass of compacted zone with needle tubing
On substrate, with stainless steel wire rod coating device that light absorbing layer coating solution is uniform, being placed in vacuum glove box makes solvent wave
Hair dries, and repeating coating makes light absorbing layer thickness reach 500-600nm 2 times, finally uses 90-110 DEG C of heated-air drying 30 minutes, light
Absorbed layer sheet resistance is reduced rapidly, and color becomes black by rufous rapidly, is formed smooth surface and is covered uniform black
Perovskite light absorbing layer.11 Ω of light absorbing layer sheet resistance is measured, 95 ° of water contact angle places 30 days rear surface face in air
Color, sheet resistance and water contact angle do not change.
Embodiment 2
By PbI2Reagent 46.1g（100mmol）And CH3NH3I reagents 15.9g（100mmol）200g dimethyl formyls are added
In amine solvent, at 60-70 DEG C at stir 12 h, obtain CH3NH3PbI3Clear solution.
By tetraethoxysilane 0.83g（4mmol）, methyltriethoxysilane 0.18g（1mmol）, absolute ethyl alcohol 16g
（350mmol）, deionized water 0.75g（40mmol）Mixing, adds the aqueous solution 0.25g of 50% hydroiodic acid of mass percentage concentration
（1mmol）, it is 2-3 to make pH value of solution, and reaction 4 hours is hydrolyzed at 30-40 DEG C, it is molten to obtain organic silicon nano particle dispersant
Liquid.It is added into CH under stiring3NH3PbI3The CH containing organosilicone spreading agent is obtained in solution3NH3PbI3Clear solution.It adds
Anhydrous ethanol solvent adjusts solution to 310g, and secondary filter solution obtains light absorbing layer coating fluid, is transferred in black plastic bottle and protects
It deposits.
Light absorbing layer coating fluid is dropped in the 100mm ╳ 100mm fluorine-doped tin dioxide electro-conductive glass of compacted zone with needle tubing
On substrate, with stainless steel wire rod coating device that light absorbing layer coating solution is uniform, being placed in vacuum glove box makes solvent wave
Hair dries, and repeating coating makes light absorbing layer thickness reach 500-600nm 2 times, finally uses 90-110 DEG C of heated-air drying 30 minutes, light
Absorbed layer sheet resistance is reduced rapidly, and color becomes black by rufous rapidly, is formed smooth surface and is covered uniform black
Perovskite light absorbing layer.10 Ω of light absorbing layer sheet resistance is measured, 87 ° of water contact angle places 30 days rear surface face in air
Color, sheet resistance and water contact angle do not change.
Embodiment 3
By PbI2Reagent 46.1g（100mmol）And CH3NH3I reagents 15.9g（100mmol）200g dimethyl formyls are added
In amine solvent, at 60-70 DEG C at stir 12 h, obtain CH3NH3PbI3Clear solution.
By tetraethoxysilane 0.83g（4mmol）, organo-silicon coupling agent KH570 0.25g（1mmol）, absolute ethyl alcohol 16g
（350mmol）, deionized water 0.75g（40mmol）Mixing, adds the aqueous solution 0.25g of 50% hydroiodic acid of mass percentage concentration
（1mmol）, it is 2-3 to make pH value of solution, and reaction 4 hours is hydrolyzed at 30-40 DEG C, it is molten to obtain organic silicon nano particle dispersant
Liquid.It is added into CH under stiring3NH3PbI3The CH containing organosilicone spreading agent is obtained in solution3NH3PbI3Clear solution.It adds
Anhydrous ethanol solvent adjusts solution to 310g, and secondary filter solution obtains light absorbing layer coating fluid.
Light absorbing layer coating fluid is dropped in the 100mm ╳ 100mm fluorine-doped tin dioxide electro-conductive glass of compacted zone with needle tubing
On substrate, with stainless steel wire rod coating device that light absorbing layer coating solution is uniform, being placed in vacuum glove box makes solvent wave
Hair dries, and repeating coating makes light absorbing layer thickness reach 500-600nm 2-3 time, finally with 90-110 DEG C of heated-air drying 30 minutes,
Light absorbing layer sheet resistance is reduced rapidly, and color becomes black by rufous rapidly, forms smooth surface and covering is uniform black
Color perovskite light absorbing layer.15 Ω of light absorbing layer sheet resistance is measured, 97 ° of water contact angle, after placing 30 days in air, table
Face color, sheet resistance and water contact angle do not change.
Reference examples
By PbI2Reagent 46.1g（100mmol）And CH3NH3I reagents 15.9g（100mmol）200g dimethyl formyls are added
In amine solvent, at 60-70 DEG C at stir 12 h, obtain CH3NH3PbI3Clear solution.Add anhydrous ethanol solvent adjustment solution
To 310g, secondary filter solution obtains light absorbing layer coating fluid.
Light absorbing layer coating fluid is dropped in the 100mm ╳ 100mm fluorine-doped tin dioxide electro-conductive glass of compacted zone with needle tubing
On substrate, with stainless steel wire rod coating device that light absorbing layer coating solution is uniform, being placed in vacuum glove box makes solvent wave
Hair dries, and repeating coating makes light absorbing layer thickness reach 500-600nm 2 times, finally uses 90-110 DEG C of heated-air drying 30 minutes, light
Absorbed layer sheet resistance is reduced rapidly, and color becomes black by rufous rapidly, but the perovskite light absorbing layer surface formed is thick
Rough uneven, there are substrate is exposed and the unlapped gap of film layer.Measure 8 Ω of light absorbing layer sheet resistance, 57 ° of water contact angle,
Surface color gradually changes in air, and placing 7 days rear surface colors becomes yellow, 870 Ω of sheet resistance, water contact angle
47 °, illustrate that perovskite light absorbing layer almost decomposes.
Claims (3)
1. a kind of preparation method of the perovskite solar cell light absorption layer of stabilization, it is characterised in that made with organic silicon nano particle
For dispersant and protective film, including following preparation process：
（1）By PbI2And CH3NH3I solids are added in dimethylformamide organic solvents, control PbI2And CH3NH3The molar ratio of I
It is 1:1-1.05, reacts 12-24 h at 60 DEG C, and filtering obtains the CH of mass percentage concentration 4%-30%3NH3PbI3Solution；
（2）Organic silicon monomer is mixed with absolute ethyl alcohol, adds deionized water and hydriodic acid aqueous solution, controls material molar ratio
For：Organic silicon monomer：Absolute ethyl alcohol：Water：HI = 1：50-100：4-10：Reaction is hydrolyzed in 0.01-0.2 at 20-70 DEG C
2-12 hours, obtain organic silicon nano particle dispersant solution；
（3）Under stiring to CH3NH3PbI3Organic silicon nano particle dispersant solution, control organosilicon point are added in clear solution
The mass percentage concentration of powder is 0.3%-1.5%, obtains the CH containing organosilicone spreading agent3NH3PbI3Clear solution；
（4）Under stiring to the CH containing organosilicone spreading agent3NH3PbI3The ethanol solution of curing agent, control are added in clear solution
The mass percentage concentration of curing agent is 0-0.5%, adds organic solvent adjustment solution concentration, and secondary filter solution obtains light suction
Receive layer coating fluid；
（5）Light absorbing layer coating fluid is dropped in the Conducting Glass of compacted zone with needle tubing in glove box, is applied with bar
The coating of cloth device is uniform, and solvent volatilization repeats to be coated with after drying, and so that perovskite light absorbing layer thickness is reached 500-600nm, finally uses
90-110 DEG C of heated-air drying 30 minutes forms smooth surface and crystallizes uniform black perovskite light absorbing layer；
（6）The perovskite light absorbing layer sheet resistance 8-15 Ω of preparation, 85-105 ° of water contact angle, after placing 30 days in air,
Surface color, sheet resistance and water contact angle do not change.
2. by the preparation method for the perovskite solar cell light absorption layer stablized described in claim 1, it is characterised in that organosilicon
Monomer is tetraethoxysilane, methyltriethoxysilane, dimethyl diethoxysilane, organo-silicon coupling agent KH550, organic
Or mixtures thereof silicone couplet KH560, organo-silicon coupling agent KH570.
3. by the preparation method for the perovskite solar cell light absorption layer stablized described in claim 1, it is characterised in that curing agent
It is methylamine, ethylenediamine, melamine, normal-butyl tin, aluminium acetylacetonate, organo-silicon coupling agent KH550, organo-silicon coupling agent
KH560 。
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| CN106590629B (en) * | 2016-11-23 | 2018-11-13 | 厦门华厦学院 | A kind of raising MAPbBr3The method of perovskite quantum dot stability |
| CN108970913B (en) * | 2017-06-02 | 2023-09-01 | 杭州纤纳光电科技有限公司 | Perovskite film coating equipment, use method and application |
| CN107221600B (en) * | 2017-06-15 | 2019-05-14 | 绍兴文理学院 | A kind of preparation method of organic and inorganic perovskite composite photo voltaic material |
| CN107634143B (en) * | 2017-09-25 | 2020-04-03 | 中国工程物理研究院材料研究所 | Preparation method of perovskite battery composite material absorption layer |
| CN107768524B (en) * | 2017-12-04 | 2024-02-09 | 湖南师范大学 | Efficient and stable perovskite solar cell and preparation method thereof |
| CN112582543B (en) * | 2019-09-30 | 2023-05-02 | 上海黎元新能源科技有限公司 | Perovskite solar cell |
| CN111312899B (en) * | 2020-01-23 | 2021-10-26 | 浙江大学 | Photoelectric nerve synapse device with zero energy consumption and preparation method thereof |
| WO2024029426A1 (en) * | 2022-08-01 | 2024-02-08 | シャープ株式会社 | Perovskite solar cell and method for producing same |
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